U.S. patent application number 13/514835 was filed with the patent office on 2013-07-25 for improved, low viscosity, shelf stable, energy-actiivated compositions, equipment, sytems and methods for producing same.
This patent application is currently assigned to H.B. Fuller Company. The applicant listed for this patent is Michael W. Jorgenson, Danielle E. Koeth, Jeffrey C. Krotine, JR.. Invention is credited to Michael W. Jorgenson, Danielle E. Koeth, Jeffrey C. Krotine, JR..
Application Number | 20130186913 13/514835 |
Document ID | / |
Family ID | 44145937 |
Filed Date | 2013-07-25 |
United States Patent
Application |
20130186913 |
Kind Code |
A1 |
Jorgenson; Michael W. ; et
al. |
July 25, 2013 |
IMPROVED, LOW VISCOSITY, SHELF STABLE, ENERGY-ACTIIVATED
COMPOSITIONS, EQUIPMENT, SYTEMS AND METHODS FOR PRODUCING SAME
Abstract
The present invention provides low viscosity energy-activated
room temperature polymer compositions, equipment, systems and
methods for handling, activating and dispensing the
thermodynamically unstable, high solids, activatable liquid
compositions.
Inventors: |
Jorgenson; Michael W.;
(Quincey, IL) ; Koeth; Danielle E.; (Cleveland,
OH) ; Krotine, JR.; Jeffrey C.; (Strongsville,
OH) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
Jorgenson; Michael W.
Koeth; Danielle E.
Krotine, JR.; Jeffrey C. |
Quincey
Cleveland
Strongsville |
IL
OH
OH |
US
US
US |
|
|
Assignee: |
H.B. Fuller Company
St. Paul
MN
|
Family ID: |
44145937 |
Appl. No.: |
13/514835 |
Filed: |
December 10, 2010 |
PCT Filed: |
December 10, 2010 |
PCT NO: |
PCT/US10/59913 |
371 Date: |
January 16, 2013 |
Related U.S. Patent Documents
|
|
|
|
|
|
Application
Number |
Filing Date |
Patent Number |
|
|
61285816 |
Dec 11, 2009 |
|
|
|
61294679 |
Jan 13, 2010 |
|
|
|
61309181 |
Mar 1, 2010 |
|
|
|
Current U.S.
Class: |
222/146.1 |
Current CPC
Class: |
C08L 51/06 20130101;
C08L 2205/03 20130101; B65D 83/14 20130101; C08L 91/00 20130101;
C08L 23/06 20130101; C08L 2205/03 20130101; C09J 123/10 20130101;
C08L 91/00 20130101; C08L 51/06 20130101; C09J 123/10 20130101;
C08L 23/06 20130101 |
Class at
Publication: |
222/146.1 |
International
Class: |
B65D 83/14 20060101
B65D083/14 |
Claims
1-22. (canceled)
22. A delivery system for a thermally activatable composition, the
delivery system having: a low pressure side comprising a reservoir
for receiving the thermally activatable composition; and a high
pressure side comprising a pump having an input side for receiving
a flow of the thermally activatable composition from the reservoir,
wherein the high pressure side further comprises a heat break
between the input side and the heat exchanger/dispenser, said heat
break comprising: a first insulator, with a first end connected to
the heat exchanger/dispenser and; a tubular heat dissipator made of
a conductive material, the first end of said heat dissipator being
connected to the second end of the first insulator.
23. (canceled)
24. The delivery system according to claim 22 wherein the heat
break further comprises: a second insulator connected to the second
end of the tubular heat dissipater.
25. The delivery system according to claim 24 wherein the heat
break further comprises an internal heat dissipater having a pin
portion extending into the inner channel of the tubular heat
dissipater and grooves that allow the thermally activatable
composition to pass through the heat break to the heat
exchanger/dispenser.
26. The delivery system according to claim 25 wherein when the
pressure is rapidly reduced on the high pressure side, thermally
activatable material that has been heated cools to form a chemical
plug between the pin portion of the internal heat dissipater and
inner walls of the tubular heat dissipater defining the inner
channel therethrough, the chemical plug being dislodgeable when
pressure is reapplied to the high pressure side of the delivery
system.
27. A heat break for use in a high pressure side of delivery system
for a thermally activatable composition that includes a heat
exchanger/dispenser, the heat break comprising a first insulator
connected to the heat exchanger/dispenser; and a tubular heat
dissipater including an inner channel, said tubular heat dissipater
being connected to the first insulator.
28. The heat break according to claim 27 wherein the heat break
further comprises a second insulator connected to the tubular heat
dissipater.
29. The heat break according to claim 28 wherein the heat break
further comprises an internal heat dissipater having a pin portion
extending into the inner channel of the tubular heat dissipater and
grooves that allow the thermally activatable composition to pass
through the heat break to the heat exchanger/dispenser.
30. The heat break according to claim 29 wherein when the pressure
is rapidly reduced on the high pressure side of the delivery
system, the heat break is adapted to cause thermally activatable
material that has been heated to cool to form a chemical plug
between the pin portion of the internal heat dissipater and inner
walls of the tubular heat dissipater defining the inner channel
therethrough, the chemical plug being dislodgeable when pressure is
reapplied to the high pressure side of the delivery system.
31. The heat break according to claim 27 wherein the outer surface
of the tubular heat dissipator comprises a plurality of heat sink
fins.
32. The heat break according to claim 27 wherein the heat
dissipator is made of a conductive material.
33. The heat break according to claim 32 wherein the conductive
material is aluminum.
34. The delivery system of claim 22 further comprising a friction
loss coil.
Description
PRIORITY CLAIM
[0001] This application claims priority to U.S. App. Ser. No.
61/285,816, filed Dec. 11, 2009, U.S. App. Ser No. 61/294,679,
filed Jan. 13, 2010, and U.S. App. Ser. No. 61/309,181, filed Mar.
1, 2010, each of which is hereby incorporated by reference in its
entirety.
BACKGROUND OF INVENTION
[0002] 1. Field of Invention
[0003] The present invention provides low viscosity
energy-activated room temperature polymer compositions, equipment,
systems and methods for handling, activating and dispensing the
thermodynamically unstable, high solids, activatable liquid
compositions.
[0004] 2. Description of Related Art
[0005] Hot melt adhesives are routinely used in various
applications where a stable surface-to-surface bond must be formed.
Further, hot melt adhesives are used in securing a variety of both
similar and dissimilar materials (e.g., cellulosic substrates such
as wood, corrugated paper, cardboard, paper, carton stock, and
other substrate materials such as plastics, metals, fabric and
other textiles, leather etc.) together in a mating relationship.
These adhesives are especially useful in applications where it is
desirable to have the adhesive solidify rapidly after being
dispensed. There are several drawbacks with the use of conventional
hot melt dispensing systems including handling solids, high energy
consumption, polymer decomposition, expensive equipment, safety
concerns and the like.
[0006] Stumphauzer, WO/2001/53389 A1, describes a heat-activated
thermoplastic material for forming an adhesive formed from an
admixture of a thermoplastic resin (typically polyvinyl chloride)
in a liquid carrier (typically a phthalate-based plasticizer). The
admixture is a liquid slurry at room temperature that undergoes a
change in which the slurry becomes pasty upon heating to a fusion
temperature and liquefies upon further heating to form a pumpable
molten liquid. The molten liquid hardens as it cools to form an
adhesive.
[0007] Stumphauzer et al., U.S. Pat. Nos. 7,221,859, 7,285,583,
7,501,468, and 7,772,312, each of which is hereby incorporated by
reference in its entirety, disclose a multiple component polymer
compositions that are pumpable at room temperature and form a
molten hot melt material when heated above about 300.degree. F. and
mixed and equipment for activating and dispensing such composition.
The molten hot melt material can be dispensed to form a solid
adhesive material upon cooling.
[0008] Jorgenson et. al., WO/2009/108685 A1, which is hereby
incorporated by reference in its entirety, discloses methods and
compositions including a foamed adhesive that utilizes relatively
small amounts of blowing agents such as water at temperatures
heated above about 140.degree. F. and equipment capable of
processing these compositions. Upon dispensing of the heated
polymeric adhesive, the vapor from the heated water aids in the
performance of the foamed solid adhesive. Subsequent research has
shown that optimization of this foam to create uniformly dispersed,
stable, fine cells sometimes requires the use of various complex
processing additives.
[0009] The compositions and equipment described by Stumphauzer et.
al. and Jorgenson et. al. overcame many of the problems facing
conventional adhesives, sealant and gasket systems by eliminating
the unpleasant odors and smoke associated with remote kettles, the
high energy costs, the safety hazards and the thermal degradation
of the adhesive compositions. Such compositions need only to be
energy-activated at the point of dispensing, which thus confers
many of the advantages of cold glue applications, but has the
advantage over cold glue systems of much more rapid speed due to
the high solids, the ability to use materials that would normally
degrade under extended and repeated exposure to high temperatures
and cleaner, faster applications at the elevated temperatures of
the point of dispensing.
[0010] Jorgenson et. al. further teach that a combination of the
micro-structure and the resultant macro-structure can affect the
stability, viscosity, rheological properties, and the like, of the
liquid emulsions, dispersion and/or suspensions below 140.degree.
F. Jorgenson et al. teach that lower viscosity materials can be
obtained using a relatively complex emulsion polymerized ethyl
vinyl acetate product and ground poly-alkylene polymers mixed at
room temperature.
[0011] Although the technology described by Stumphauzer et al. and
Jorgenson et al. provides significant advances over the prior art,
improvements can still be made to address practical process and
equipment limitations in the industrial setting associated with
waste and product separation in the low pressure delivery systems,
separation in the high pressure delivery systems, frequent problems
with shut-down and start-ups. Compositions such as disclosed by
Stumphauzer et al. and Jorgenson et al. tend to be
thermodynamically unstable, meaning that pressure, shear forces or
polymer hysteresis, chemical induced differentials on the
composition tend to cause the various components of the composition
to separate (e.g., the liquid carrier can separate from the polymer
solids). While the prior art gives pumpable, liquid, polymer
compositions that are reasonably stable to separation, they suffer
from being high viscosity requiring complicated equipment solutions
to satisfactorily transfer and dispense the compositions.
Alternatively, pumpable, liquid polymer compositions that are low
viscosities can be prepared but have limited resistance to
separation of the polymer and the liquid phases which creates
consistency problems in storage, separation in hoses and/or in a
heat break and inconsistent processing of the pumpable, liquid
polymer compositions.
BRIEF SUMMARY OF THE INVENTION
[0012] In view of the foregoing, the present invention provides
compositions, processes, equipment and methods that provide
substantial advantages over the prior art in the form of less
waste, improved shelf life stability, improved system stability,
consistent start-up processing, no pack outs and ultimate
performance advantages.
[0013] The compositions according to the invention are low
viscosity, shelf life stable products at room temperature that can
be activated to form substantially homogeneous molten material
capable of bonding two components when dispensed and cooled as a
cellular or solid non-cellular polymeric substantially non-exuding
material. The compositions according to the invention comprise:
[0014] solid particles comprising one or more polymers (sometimes
hereinafter referred to as the "first component"), which are
emulsified, dispersed and/or suspended at temperatures
substantially below the melting point or below the temperature
where the solid particles are soluble with a second liquid
component; [0015] a second liquid component comprising one or more
polymers processed in a liquid carrier at temperatures exceeding
100.degree. F. and substantially below the melting point or below
the temperature where the liquid plasticizes the bulk (about 75% or
greater by weight) of the polymers creating a high viscosity
intermediate component, which can be used to form a lower solids,
lower viscosity liquid emulsion, dispersion and/or suspension; and
[0016] a liquid carrier that is selected based upon the ability of
the first and/or second component to substantially resist
absorption of the liquid carrier at the storage and pre-processing
temperatures and is absorbed when the material is activated to form
a substantially homogeneous molten material capable of bonding two
components when dispensed and cooled as a cellular or solid
non-cellular polymeric substantially non-exuding solid.
[0017] Unless otherwise expressly stated, the term "room
temperature" is hereby defined as being 72.+-.5.degree. F. and at
other ambient temperatures from about 32.degree. F. to 140.degree.
F., preferably 50.degree. F. to 120.degree. F., most preferably
60.degree. F. to 110.degree. F.
[0018] The present invention is also directed towards a delivery
system for handling and delivering low viscosity, shelf life
stable, room temperature compositions that can be activated to form
substantially homogeneous molten material capable of bonding two
components when dispensed and cooled as a cellular or solid
non-cellular polymeric substantially non-exuding material in a
stable, homogeneous room temperature emulsion, dispersion and/or
suspension from a low pressure side to a high pressure side. The
low pressure side comprises a shipping container, which is capable
of being evacuated via gravity feed or with vacuum created by a
hydraulic pump, and a reservoir capable of: [0019] delivering
greater than 10 pounds per hour, preferably greater than 20 pounds
per hour and most preferably greater than 40 pounds per hour via
gravity feed or vacuum assist, and [0020] delivering first in-first
out with minimal polymer separation from the liquid carrier.
[0021] The high pressure side of the delivery system comprises a
pump capable of delivering low viscosity, shelf life stable, room
temperature compositions that can be activated to form
substantially homogeneous molten material capable of bonding two
components when dispensed and cooled as a cellular or solid
non-cellular polymeric substantially non-exuding material that is
connected to: [0022] a heat break device designed to insure
maintenance free start ups after temporary interruptions; and/or
[0023] a heat break in combination with a "friction loss" component
and timed shut down protocol, which continuously and gradually
reduces the pressure on the composition inducing back-flowing
heat-activatable material to solidify at a point in the system
where it can be easily reheated, thereby preventing irreversible
plugging of the unheated portion of the system as pressure
differentials are relieved; and/or [0024] a three component
"chemical heat break check" which induces back-flowing
heat-activatable material to solidify at a point in the system
where it can be easily reheated, thereby preventing irreversible
plugging of the unheated portion of the system as pressure
differentials are relieved.
[0025] The foregoing and other features of the invention are
hereinafter more fully described and particularly pointed out in
the claims, the following description setting forth in detail
certain illustrative embodiments of the invention, these being
indicative, however, of but a few of the various ways in which the
principles of the present invention may be employed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] FIG. 1 is a schematic representation of a delivery system
according to an embodiment of the invention.
[0027] FIG. 2a is a perspective view of an embodiment of a
reservoir and associated conduits for a delivery system according
to the invention.
[0028] FIG. 2b is a cross-sectional view taken through the middle
of a reservoir design that did not perform as desired.
[0029] FIG. 2c is a cross-sectional view taken through the middle
of a reservoir design that did perform as desired.
[0030] FIG. 3 is an assembled view of a heat break according to an
embodiment of the invention.
[0031] FIG. 4 is an exploded view of the heat break shown in FIG.
3.
[0032] FIG. 5 is a section view taken longitudinally through the
center of the heat break shown in FIG. 4.
[0033] FIG. 6 schematically illustrates a controlled plug in the
section view of FIG. 5.
DETAILED DESCRIPTION OF THE INVENTION
[0034] As noted above, compositions according to the invention are
low viscosity, shelf life stable products at room temperature that
can be activated to form substantially homogeneous molten material
capable of bonding two components when dispensed and cooled as a
cellular or solid non-cellular polymeric substantially non-exuding
material. The compositions according to the invention comprise:
[0035] solid particles comprising one or more polymers (sometimes
hereinafter referred to as the "first component"), which are
emulsified, dispersed and/or suspended at temperatures
substantially below the melting point or below the temperature
where the solid particles are soluble with a second liquid
component; [0036] a second liquid component comprising one or more
polymers processed in a liquid carrier at temperatures exceeding
100.degree. F. and substantially below the melting point or below
the temperature where the bulk of the polymers in the liquid
carrier become soluble creating a high viscosity, homogeneous
liquid component; thereby creating a lower solids, lower viscosity
liquid emulsion, dispersion and/or suspension; and [0037] a liquid
carrier that is selected based upon the ability of the first and/or
second component to substantially resist absorption of the liquid
carrier at the storage and pre-processing temperatures and is
absorbed when the material is activated to form a substantially
homogeneous molten material capable of bonding two components when
dispensed and cooled as a cellular or solid non-cellular polymeric
substantially non-exuding solid.
A. The First Component
Monomers/Starters
[0038] The first component of the compositions according to the
invention comprises solid particles of one or more polymers that
can be derived from polymerizing any combination of ethylene,
propylene, butylene, higher .alpha.-olefins or isomers thereof,
styrene and its isomers, isoprene, butadiene, higher .alpha.-dienes
or isomers thereof, norbornene, dicyclopentadiene, acrylic acid and
its derivatives thereof, methacrylic acid and its derivatives
thereof, olefinically unsaturated dicarboxylic acid and its
derivatives thereof, acrylonitrile, vinyl chloride, vinylidene
chloride, vinyl ester, vinyl ethers, vinyl silanes and the like.
Additional polymers can be constructed with combinations of starter
molecules with reactive hydrogen such as water, sorbitol, glycerol,
sucrose, multifunctional amines, and the like, together with or,
optionally the monomers by themselves or in combination with
themselves such as oxides, for example, ethylene oxide, propylene
oxide, tetrahydrofuran, and the like, various multifunctional acids
or anhydrides, for example terephthalic acid, phthalic anhydride,
adipic acid, succinic anhydride and the like, glycols such as
ethylene glycol, propylene glycols, butlyene glycol, and the like,
and/or various multi-function amines, for example, urea, ethylene
diamine, hexamethylene diamine, and the like. These chemicals in
various combinations result in polyethers, polyesters, polyamides,
polyether amines which can result in high performance finished
products. Highly specialized polymers could include silicones
formulated for adhesion similar to those used in room temperature
vulcanization (RTV's) processes where the silanols condense at high
temperatures. Natural polymers such as proteins and their
derivatives, starches and their derivatives, cellulosics and their
derivatives, fats and oils their derivatives, for example natural
and synthetic rubbers, lignins, terpene resins, rosin esters,
derivatives of wood, gum, and tall oil rosin can be used in any
combination with the above fossil fuel polymers that permits them
to be emulsified, dispersed or suspended as solids in the second
liquid component at room temperature up to temperatures
substantially below the melting point or below the temperature
where the solid particles are soluble with the second liquid
component.
Polymerization Conditions
[0039] The first component may include combinations of polymers
that can range from homo-polymers to multi-feedstock polymers,
copolymerized, step-polymerized, or any combination of the above in
the gas or liquid phase. The processes can include addition,
condensation, free radical, anion or cation, gas, liquid or solid
state, and the like, catalyzed polymerizations. The choice of
polymer process and compositions can lead to polymers with random,
block, branched, tipped or any combination of these leading to
various distributions along the chain or chains. In addition,
polymers that have grafted monomers on the polymer chain can lead
to further enhancements. Judicious choice of these parameters
ultimately lead to various macrostructures that could include
standard structure polymeric materials capable of being ground,
higher or lower crystallinity polymers, spherical or jagged
particles, core and shell particles, and the like.
Particle Size
[0040] The polymers used in the first component may be obtained as
virgin, recycled or scrap material in the form of pellets, sheets,
tubes, rods, films, formed materials, bottles, or the like.
However, in order to achieve the proper plastisol viscosity,
stability, pumpability and over-all delivery characteristics, such
materials should be reduced to an average particle size (diameter)
of less than about 5000 microns, preferably less than about 1,500
microns and most preferably below about 1000 microns. Thus, it may
be advantageous to purchase the material in the form of a powder or
other granular forms.
[0041] The first component in the invention is selected based upon
the ability of the first and second component to: [0042]
substantially resist absorption of the liquid carrier at the
storage and pre-processing temperatures; [0043] the ability of the
first and second component to irreversibly absorb substantially a
majority of the liquid carrier when the composition is subjected to
elevated processing temperatures where the materials are fused,
and; [0044] the ability of the first component to prevent exudation
of the liquid carrier from the fused solid material that is formed
when the composition is dispensed and cooled from the elevated
processing and activation temperature.
[0045] The levels of the actual polymer or combination of polymers
used as the first component is a function of the beginning
viscosity of the second component which is dependent on the actual
polymer or combination of polymers used as part of the second
liquid component and any other ancillary additives. Depending on
the composition and characteristics of the first component and the
viscosity of the second component, the first component ranges from
2.5% to 45%, preferably 5% to 40%, most preferably 10% to 35%.
[0046] The ultimate choice of polymer(s) for the first component
will be a function of many criteria discussed above in addition to
the stability to oxidation and radiation such as light,
micro-waves, costs, degree of transparency to radiation, the tack
time which is that time when the energized polymer is no longer
sticky, process hygiene, set time which is the time the application
is workable, bond time described below, open time which is the time
the application can me moved without damaging the finished product
characteristics, stiffness, hardness, density which is a function
of both the polymer and blowing agent, volume, flexibility,
conformability, resilience, creep, elongation, strength modulus
elongation, chemical resistance, temperature resistance,
environmental resistance and compressibility and the like.
B. The Second Component
[0047] Key factors influencing the selection of polymers and liquid
carriers include the impact on the viscosity and shelf life
stability of the composition in its pumpable, pre-activated state.
Lowering the viscosity of the composition while maintaining the
shelf life stability in its pre-activated room temperature state is
highly desirable as it allows the material to be transferred by
gravity, pneumatics, peristaltic pumps, gear pumps, piston pumps
and the like and stored in a variety of containers for extended
periods of time. It has surprisingly been found that high levels of
polymers can be emulsified, dispersed and/or suspended in the
liquid carrier at elevated temperatures below the melting point of
the polymers or below the temperature where the liquid is
substantially soluble in the polymer to produce a second liquid
component with relatively high solids and when combined with the
first component simultaneously creates a low viscosity and shelf
life stabile composition in the pre-activated state.
[0048] The actual polymer or combination of polymers used as part
of the second liquid component is selected from the first component
based upon the majority of the polymers ability to substantially
resist absorption of the liquid carrier at the storage and
pre-processing temperatures. Advantageously, the performance of the
final composition is enhanced if the majority of the polymers in
the second liquid, [0049] preferably absorbs substantially a
majority of the liquid carrier when the composition is subjected to
elevated processing temperatures where the materials are fused,
and; [0050] most preferably, prevents exudation of the liquid
carrier from the fused solid material that is formed when the
composition is dispensed and cooled from the elevated processing
and activation temperatures.
[0051] Mixing the polymer in the liquid carrier at temperatures
above or nearing the melting point or temperatures where the
polymer is highly plasticized creates higher viscosity liquids,
paste or solid when cooled to room temperature; thereby, creating a
stable, pumpable, material with unacceptably high viscosity. As
anticipated, this behavior is highly dependent on the solids used
in the process, i.e., higher solids give higher viscosity second
component liquids.
[0052] Unexpectedly, it was discovered that a low viscosity, high
solids second component could be produced adding and mixing a high
level of the solids to a carrier heated greater than 100.degree. F.
and more than 25.degree. F. below, preferably more than 50.degree.
F. below, most preferably more than 75.degree. F. below the melting
point or temperatures where substantial plasticization for a
majority of the polymer added to the heated carrier occurs, where a
majority is greater than 60%, preferably greater than 80%, and most
preferably greater than 90% of the polymer composition.
[0053] Generally speaking, higher concentrations of the polymers
can be used in the second component if the melting point,
solubility and plasticization characteristics of the polymers are
balanced against the conditions and temperatures at which the
second component is processed. The percentage of solids in the
second component ranges up to 60%, preferably up to 50%, most
preferably up to 40%. The percentage of the second component of the
final composition can be up to 95%, preferably up to 80%, most
preferably up to 70%.
[0054] While not being bound to any particular theory, the
compositions created are thought to be liquid carrier stabilized
particles. This is not expected since the carrier would not be
classified as a classical stabilizer such as a surfactant, reactive
grafted polymer, compatibilizer, or the like. In addition, the low
viscosities should actually increase since it is well know that any
absorption or loss of the liquid phase creates higher viscosity end
products. In another aspect of the theory, it is speculated that
the liquid carrier stabilized particles must have other qualities
of smoother, more pliable surfaces that have a slip agent qualities
in the liquid phase resulting in the low viscosity and shelf life
stable products.
C. The Liquid Carrier
[0055] The liquid carrier must be a flowable material at room
temperature. The liquid carrier enables the composition to be
pumpable at room temperatures up to 110.degree. F., preferably up
to 120.degree. F. and most preferably up to about 140.degree. F.
and contributes to the quality and unique properties of the fused
matrix on cooling. The liquid carrier may be chosen by optimizing
several factors including cost, reactivity at storage conditions
and dispensing temperatures, compatibility with the first component
and second component at various temperatures, volatility, safety
considerations, regulatory approvals, and the like. Suitable
materials for use as the liquid carrier include low volatility
solvents, tall oils, liquid plasticizers, aliphatic hydrocarbons,
hydrocarbon esters, vegetable oils and their derivatives, glycerol
and its derivatives, glycols and their derivatives, polyols and
alkoxylates. Such liquids must be substantially stable with the
first and second components, processing aids and optional liquid or
solid components at temperatures less than about 85.degree. F.,
preferably less than about 100.degree. F. and most preferably less
than about 140.degree. F.
[0056] The choice and level of liquid carrier and any material that
is liquid or soluble at room temperature is a key determinant in
obtaining a low viscosity finished product. The levels in the end
use product range up to 65%, preferably up to 55%, most preferably
up to 45%.
[0057] Liquid natural products such as vegetable oils and their
derivatives and by products, fats, carbohydrates and their
derivatives or other natural materials derived from renewable
sources are preferred for the second component. The most preferred
choices for the second component are soybean oil and its
derivatives (e.g., epoxidized soybean oil), biodiesel, glycerol and
the like.
D. End Use Products
[0058] The compositions according to the invention are low
viscosity, shelf life stable products at room temperature that can
be activated to form substantially homogeneous molten material
capable of bonding two components when dispensed and cooled as a
cellular or solid non-cellular polymeric substantially non-exuding
material.
[0059] The compositions according to the invention comprise: [0060]
solid particles comprising one or more polymers (sometimes
hereinafter referred to as the "first component"), which are
emulsified, dispersed and/or suspended at temperatures
substantially below the melting point or below the temperature
where the solid particles are soluble with a second liquid
component; [0061] a second liquid component comprising one or more
polymers processed in a liquid carrier at temperatures exceeding
100.degree. F. and substantially below the melting point or below
the temperature where the liquid plasticizes the bulk (about 75% or
greater by weight) of the polymers creating a high viscosity
intermediate component, which can be used to form a lower solids,
lower viscosity liquid emulsion, dispersion and/or suspension; and
[0062] a liquid carrier that is selected based upon the ability of
the first and/or second component to substantially resist
absorption of the liquid carrier at the storage and pre-processing
temperatures and is absorbed when the material is activated to form
a substantially homogeneous molten material capable of bonding two
components when dispensed and cooled as a cellular or solid
non-cellular polymeric substantially non-exuding solid.
[0063] The compositions according to the invention, before being
energy-activated, can be characterized as liquid emulsions,
dispersions and/or suspensions in which the first component and any
other optional additional solids or liquids, are emulsified,
dispersed or suspended as distinct or composite particles in the
second component. Alternatively, the optional liquid or solid
components can be soluble in the second component. For example,
solid tackifiers and soybean oil can be combined in various ratios
to create a higher proportion of liquid carrier and lower viscosity
liquid polymer compositions.
[0064] These optional components can also include thermoset
polymers, natural by-products such as lignin derivatives,
intractable animal and plant proteins, initiators, curing agents,
cure accelerators, catalysts, crosslinking agents, tackifiers,
plasticizers, dyes, flame retardants, coupling agents, pigments,
impact modifiers, flow control agents, foaming agents, fillers,
glass treated and untreated microspheres, inorganic and organic
polymer microparticles, other particles including electrically
conductive particles, thermally conductive particles, synthetic,
plant and animal fibers, antistatic agents, antioxidants, and UV
absorbers, biocides, rheology modifiers, film formers, tackifying
resin dispersions, soluble tackfiers and their derivatives.
[0065] Thus, the low viscosity intermediate composition is an
emulsion, dispersion or suspension or combination of the above that
can be used advantageously to produce a low viscosity, pumpable,
pre-activated polymer composition.
[0066] Ethylvinyl acetate polymers are advantageously used as the
first component to absorb the second component during processing. A
fused homogenous blend comprising such polymers exhibits excellent
bonding to a broad range of substrates upon cooling to a
temperature below about 140.degree. F.
[0067] In another embodiment of the invention, combinations of high
levels of low surface energy, unreactive homopolymers that are not
normally considered adhesives by themselves, such as polypropylene
or polyethylene homopolymers, are used in combination with
ethylvinylacetate polymers to create room temperature-pumpable
compositions that do not need activators such as sebacic acid. The
amount of polypropylene preferably comprises up to about 40% by
weight of the total composition, and more preferably less than
about 30% by weight and most preferably less than about 20% by
weight of the total composition. The amount of polyethylene
preferably comprises up to about 20% by weight of the total
composition, and more preferably less than about 15% by weight and
most preferably less than about 10% by weight of the total
composition. It is possible to produce room temperature-pumpable
compositions according to the invention that have viscosities less
than about 15,000 cps, preferably less than about 10,000 cps and
most preferably less than 8,000 cps.
[0068] Thus, compositions according to the invention can exist in
four different states, depending upon conditions: [0069] (i) a
liquid emulsion, dispersion or suspension when stored at
temperatures from about 32.degree. F. up to about 140.degree. F.;
[0070] (ii) a substantially homogeneous, fused molten blend when
first heated above about 140.degree. F. (and more preferably above
about 212.degree. F.) and mixed; [0071] (iii) a substantially
homogeneous, fused molten blend capable of being applied directly
or expanded with the aid of a blowing agent when dispensed above
about 140.degree. F. (and more preferably above about 212.degree.
F.); and [0072] (iv) a thermoplastic cellular or solid non-cellular
polymeric solid material, which may be capable of bonding one or
more substrates when the dispensed substantially homogeneous, fused
molten blend cools to a temperature below about 140.degree. F.
E. Method of Bonding Two Substrates Together
[0073] In yet another embodiment of the invention, the composition
is activated in a reactor and dispensed between two substrates.
Upon cooling, the material forms an adhesive bond between the two
substrates.
F. Products
[0074] The invention includes cases or cartons comprising one or
more flaps that have been sealed using the compositions and methods
of the invention, and adhesives, sealants, coatings and gaskets
formed using the compositions and methods of the invention.
G. Delivery System
[0075] It is well known that chemical and/or physical means can be
used to influence the stability of emulsions, dispersions or
suspension. As noted above and in the examples, the present
invention provides a product that has greatly improved static
stability as exemplified by the viscosity and centrifuge tests. In
spite of this improved stability, it has been found that shear and
pressure differentials can still lead to minor inconsistencies in
the composition of the low viscosity, shelf life stable products as
they transition through the various components of the system. The
present invention thus also provides a delivery system for
dispensing such a product that ensures that the: [0076] material
can be continuously and reliably delivered to the dispensing
apparatus with minimal waste, [0077] destabilizing differentials
are avoided on the material that could lead to the separation of
the components thereby requiring unwanted maintenance, and [0078]
activated material does not flow backwards in the delivery system,
thereby solidifying within the portions unactivated material in the
intended cool portions of the system creating the need for unwanted
maintenance.
[0079] A delivery system 10 according to the invention is
schematically illustrated in FIG. 1. The system 10 includes a low
pressure side 20, which comprises a shipping container 30 and a
reservoir 40, and a high pressure side 50, which comprises a pump
60, an insulator 80, a heat exchanger 90 and a dispenser 100. In
the preferred embodiment, the insulator 80 is part of a heat break
110. The system 10 also preferably comprises a "T" 70 and a
friction loss coil 120, which is in fluid communication between the
high pressure side 50 and the low pressure side 20.
1. Low Pressure Side
[0080] The reservoir 40 is disposed between the shipping container
30 and the components of high pressure side 50 of the system 10.
The shipping container can be a small container (e.g., a
bag-in-box, a drum, a tote or other container) or a larger bulk
container. The reservoir 40 is adapted to receive, store and supply
unheated material to the pump 60 with minimal waste and product
deterioration. The reservoir 40 can be formed of any material that
does not react with or degrade the product to be dispensed. In one
embodiment, the reservoir 40 is formed of polyvinyl chloride (PVC).
In a more preferred embodiment, the reservoir 40 is made of
polyalkylene materials. Preferably, the reservoir 40 comprises a
vessel to which a vacuum or gas, which could be air or an inert
material, could be alternately applied to substantially empty the
shipping container 30 while simultaneously delivering an
uninterrupted flow of pumpable composition through a conduit to the
pump 60. The volume of the reservoir and its associated conduits is
sufficient to allow an operator to replace an emptied shipping
container with a shipping container containing a new supply of
material without introducing debris, entraining gas in the material
or destabilizing the material.
[0081] This reservoir insures consistent delivery and allows the
user to easily manage the replacement of the shipping container
without disruption. It was unexpectedly discovered that this low
pressure reservoir system could not be constructed in the simple,
cost effective manner such as is conventional for other liquid
handling systems.
[0082] It was desirable to have a gravity feed and/or vacuum assist
provided by the high pressure pump delivering material to the
activation portion of the delivery system. A five gallon bag-in-box
system with a one inch port was selected as the preferred shipping
vessel to evaluate low pressure reservoir configurations. To insure
consistent performance over time for pumpable materials with
viscosities ranging from 5,000 to 60,000 cps, preferably 6,000 to
30,000 cps, and most preferably from 7.500 to 20,000 cps the
reservoir must be able to: [0083] deliver greater than 10 pounds
per hour, preferably greater than 20 pounds per hour and most
preferably greater than 40 pounds per hour via gravity feed or
vacuum assist, and [0084] be capable of delivering first in-first
out with minimal polymer separation from the liquid carrier.
[0085] It was discovered that any barrier or dead spot in the
reservoir system would lead to areas where "dry" material would
lodge at the barrier or dead spot creating an inhomogeneous
material to continuously build up eventually leading to failure of
the system reservoir capability. The term "dry" as used herein
describes a material in which the liquid has separated sufficiently
from the solid particles to become an unflowable, inhomogeneous
mass. A barrier leading to the formation of a "dry" material could
be a ledge or a sharp bend representing a corner.
[0086] FIG. 2a is a perspective view of an embodiment of a
reservoir 40 and associated conduits for a delivery system 10
according to the invention. The shipping container 30 (not shown)
is adapted to couple to a conduit 410 via a coupling 420. Product
flows from the shipping container through the conduit 410 and into
the reservoir 40. Intermediate the coupling 420 and the reservoir
40, the conduit 410 includes a port 430, which as described in
greater detail below, receives material flowing from the high
pressure side 50 to the low pressure side 20 through a friction
loss coil 120. Product from the shipping container flows into the
reservoir 40 and exits the reservoir 40 through a conduit 440,
which supplies the material to the pump 60 (not shown).
[0087] In order to monitor the amount of product in the reservoir
40, product exiting the reservoir can optionally also be directed
to flow through a conduit 450, which includes a portion that rises
vertically substantially parallel to the reservoir and includes a
sight glass portion 460 that allows for visual determination of the
amount of product in the reservoir 40. An electronically controlled
vent valve 470 can be provided at the end of the conduit 450 and
above the reservoir 40 to permit air to escape and relieve pressure
within the low pressure side. A low level sensor 480 can be
installed in conduit 450. And, an empty cutoff sensor 490 can be
installed in conduit 440. It will be appreciated that the
configuration of the reservoir 40 and its associated conduits can
be varied, as required, to meet the needs of the particular
application.
[0088] FIG. 2b shows a cross-sectional view of a reservoir 40',
which includes sharp corners 500 and horizontal flat areas 510. A
reservoir 40' having this configuration did not function as
desired. It was found that a one inch right angle PVC joint
resulted in the formation of a "dry" mass, which restricted the
flow to the point that the desired delivery rate could not be
met.
[0089] FIG. 2c shows a cross-sectional view of a reservoir 40 that
does function as desired. The reservoir 40 shown in FIG. 2c does
not include any sharp (e.g., 90.degree.) angles. Surprisingly, the
elimination of sharp angles and flat (horizontal) areas appears to
be very important. Instead, the reservoir 40 shown in FIG. 2c
includes non-horizontal ramp portions 520 and angles 530 greater
than 90.degree..
[0090] A reservoir 40 according to the present invention thus
preferably comprises: [0091] a container having greater than 1
liter, preferably greater than 3 liters and most preferably greater
than 5 liter capacity, [0092] no restriction in the primary flow
path of greater than 0.75 inch, preferably less than 1.0 inch, most
preferably less than 1.5 inch, [0093] no barriers greater than
0.5'' in depth, preferably greater than 0.25'', most preferably
greater than 0.1'', [0094] no turns in the primary flow pattern
where the obtuse angle measured on the outside of the respective
turn formed by two tangential lines on the outside of the turn has
a combined measurement of one inch and the measured obtuse angle is
not less than 120 degrees, [0095] the ability to hold vacuum or
accept pressures up to 120 PSIG, and [0096] a mechanical or
automated vent capable of sufficiently releasing trapped gas as the
material flows into the reservoir.
[0097] Optionally, the reservoir component further comprises:
[0098] a sight glass or tubing capable of allowing for a
measurement device that has greater than 1.00 times the diameter of
the diameter of the connector to the shipping container, and [0099]
other connections capable of returning material from the high
pressure side of system such as an inlet from a friction loss coil
and the like.
[0100] Variations can be made in the arrangement of the parts in
the storage container and reservoir without departing from the
scope of the invention so long as the low pressure side of the
system performs the following functions: substantially empties the
shipping container of a material; substantially maintains the
thermodynamically unstable, high solids, activatable liquid
compositions in the same condition and performance as the material
in the shipping container; and allows for continuous, uninterrupted
operation of the system for supplying the material to the high
pressure side.
2. High Pressure Side
[0101] Developing a high pressure delivery system that is stable
during routine running, shut down and start up poses unexpected
challenges associated with the movement of the liquid in the pump
60, connecting hoses or lines and in the heat break 110 as the
pressure is applied or released and/or as temperature is applied or
released. It has been surprisingly discovered that obstacles faced
in the low pressure system are also present in the high pressure
system as pressure differentials, restrictions, barriers and turns
can induce the liquid carrier to separate from the polymer. Failure
of the equipment to properly manage this flow results in the system
slowly starting up or not starting up at all, can lead to weak
and/or inconsistent bead dispensing, and/or production
disruptions.
a. Hydraulic Pump System
[0102] A key element of the high pressure delivery system is a
hydraulic pumping system 60 that does not lead to discontinuous
pressure differentials as the system experiences planned or
unplanned disruptions or is shut down over an extended period of
time. With reference to FIG. 1, it has been found that separation
of the polymer from the liquid carrier can be eliminated in the
hydraulic pump 60 by connecting the high pressure output of the
hydraulic pump to a "T" 70 having two parallel channels: [0103] a
primary channel 130 designed to deliver the liquid to the
components required to activate the composition and dispense the
composition when the dispenser is opened for dispensing, and [0104]
a secondary channel 140, which includes the "friction loss
component" 120 that constantly returns a small quantity of liquid
back to the low pressure reservoir 40 or the input side of the pump
60.
[0105] The system according to the invention preferably comprises a
tubular friction loss coil 120, which is in fluid communication
between a friction loss outlet (i.e., the port in the "T" 70 to
which the secondary channel 140 is connected) on the high pressure
side of the system and an inlet in the reservoir on the low
pressure side of the system. The term "coil" is used only to
describe a preferred embodiment of the invention. It will be
appreciated that the tubular friction loss conduit need not
actually be coiled in order to perform its desired function, which
is to gradually reduce pressure on the material as it passes from
the high pressure side of the system to the low pressure side of
the system.
[0106] The term "friction loss" refers to that portion of pressure
lost by fluids while moving through a pipe, hose or other limited
space. The friction loss coil according to the invention ensures
that the pump can remain on and can cycle when material is not
being dispensed or it slowly diminishes the pressure when the pump
is stopped. In both instances, material will flow through the
friction loss coil and back into the reservoir 40. The pressure at
the pump will remain high, but due to "friction loss" the pressure
at the reservoir will be low. Friction loss causes a gradual
diminishment of pressure on the material, rather than an abrupt
pressure differential in the pumping system. This prevents the
material from separating in the system.
[0107] The length and diameter of friction loss coil is sufficient
to gradually reduce the pressure on the material from the high
pressure side which is >300 psi hydraulic pressure to the low
pressure side which is equal to or less than atmospheric pressure.
The length, diameter and pressure differentials of the friction
loss coil will be selected in view of the viscosity, flow
characteristics, thermodynamic stability, inherent particle sizes,
and the like of the material to insure that the pumps and flow
patterns do not stop flowing or seize up creating unwanted pressure
differentials.
[0108] The "friction loss" component must: [0109] continuously
deliver less than 5%, preferably less than 2.5% and most preferably
less than 1% of the weight capacity of the hydraulic pump, and
[0110] gradually reduce the pressure from the hydraulic head
pressure to less than 50 psig, preferably less than 25 psig and
most preferably less than 10 psig at the return to reservoir or
input of the pump b. Heat Break System
[0111] The heat break prevents thermal energy from migrating from a
heat exchanger 90, which heats and activates the product to be
dispensed through the dispenser 100, into unheated portions of the
system. This is critical to insure that the material is not
prematurely activated. Normal dispensing conditions allow for an
equilibrium to be established where the cold incoming liquid
material meets the heated material from the heat exchanger 90 and
no deleterious plugs or "dry" material are formed causing the
dispensing unit 100 to stop or lose pressure. However, relief of
the pressure used to pump the material to the heat break and
through the heat exchanger and dispenser generally leads to the
heated material reversing direction towards the pump, where it can
cool thereby creating a plug or form "dry" material in the heat
break 110, hose or both. This can lead to an irreversible situation
as the heat exchanger 90 can no longer provide enough energy to
cause the plug to be substantially liquefied to flow or the
pressure in the system is not powerful enough to push the plug
through the hose, heat break or both.
[0112] Complex systems involving check valves, dump valves, timing
sequences and the like have been used to overcome this key
deficiency. However, separation can occur when conventional check
valves are used, because the liquid phase, for example oils, will
leak through to the low pressure side of small openings such as a
check valves, constrictions, or poor O-ring seals, fittings, and
the like. Due to this phenomenon associated with thermodynamically
unstable, high solids liquids, separation of the material can occur
leaving dry material on one side of the pressure differential and
liquid on the other side. This creates undesirable consequences
which include plugs, creates poor performance, causes disruption in
production, and the like.
[0113] The heat break systems described by Stumphauzer et. al. and
Jorgenson et. al. function according to their intended purpose of
suppressing heat from activating the glue in the hydraulic hose as
long as the adhesive is dispensed on substantially uninterrupted
basis in the high pressure system. However, the present invention
provides improvements, which are particularly advantageous in
manufacturing environments where frequent disruptions and shut
downs occur. In order to provide the most efficient dispensing
system the heat break design must be optimized bringing the
following benefits: [0114] it should be able to re-activate cured
material after short term interruptions, short and long term shut
downs, and unplanned disruptions in the dispensing process, [0115]
it should prevent thermal energy from traveling from the heat
exchanger/dispenser to other areas in the system where thermal
energy inappropriately activates the liquid, and [0116] it should
be designed to insure that the carrier and polymer do not separate
in the device to form a dry plug, which would will prevent flow of
material to the dispenser 100.
[0117] With reference to FIG. 3, it was discovered that a heat
break 110 comprising the following components and/or features
overcomes these problems, and performs well during short term
disruptions: [0118] a first insulator 80 made of a non-conductive
material, most preferably constructed from PEEK, and [0119] a heat
dissipater 150 made of a conductive material, most preferably
aluminum, wherein [0120] a channel is provided between the first
insulator 80 and the heat dissipater 150 greater than 0.100 inch,
preferably greater than 0.125 inch and most preferably greater than
0.200 inch, and optionally [0121] a second insulator 160,
preferably made of PEEK,
[0122] The first insulator 80 is coupled between the heat exchanger
90 and the heat dissipater 150. The first insulator 80 prevents
heat from migrating from the heat exchanger 90 toward the unheated
portion of the delivery system connection 130 and beyond. The heat
dissipater 150, in this particular embodiment includes a channel
through which material supplied from the cold end 170 can be
supplied. The outer surface of the heat dissipater 150 preferably
includes a plurality of heat sink fins 210 shown in FIGS. 5 and 6,
which allow heat to escape to the atmosphere. Heat can reach the
first heat dissipater 150 when heated material flows back into the
heat break 110 after it has been heated in the heat exchanger 90.
Material flowing back from the heat exchanger 90 enters the hot end
180 of the insulator 80 and then makes contact with the heat
dissipater 150. The second insulator 160 helps isolate the heat
break 110 from the remaining cold portions of the delivery system
10.
[0123] While not wishing to be held to any particular theory, the
heat dissipater 150 functions to cool the activated material in a
region adjacent to the heat exchanger/dispenser 90/100 (these units
can be combined) to form a short "chemical plug" that is capable of
being reversibly pushed back into the heat exchanger/dispenser
90/100 via pressure supplied by the pump 60. This chemical plug
serves as pseudo check valve stopping the pressurized, activated
material in the heat exchanger/dispenser 90/100 from pushing back
into regions of the delivery system that are designed to be at or
near room temperature. Eliminating irreversible plugs enables the
dispensing process to be temporarily disrupted and have the
dispensing process restarted with no manual maintenance of the
system. The chemical plug forms between the heat dissipater which
has a mix of activated and heated material and the heat break,
which has cool unactivated material in a substantial portion of the
heat break. The design of the region where it is desirable to form
this chemical plug in the heat dissipater 150 and heat break
consists of: [0124] no barriers greater than 0.100'' in depth,
preferably greater than 0.050'', most preferably greater than
0.025'', and [0125] no constrictions in the forward flow pattern
before the glue is subjected to melting temperatures in the heat
dissipater.
[0126] The subject of this invention solved the problems associated
with short term disruption as long as the pressure was maintained.
However, a complete disruption of the temperature and a pressure
caused other unanticipated pressure differentials associated with
activated glue cooling down, creating a vacuum in the heat
exchanger/dispenser unit. This unanticipated pressure differential
led to the liquid carrier being separated from the polymer which
then required maintenance to satisfactorily dispense the activated
liquid on restarting the system.
c. Friction Loss/Thermal Break Process
[0127] Thus, to avoid this problem, in a preferred embodiment of
the invention, it is desirable to combine the hydraulic pump system
disclosed above, or a comparable hydraulic pumping system capable
releasing the pressure in a controlled manner, with the heat break
in a process where the temperature is first shut down followed by
shutting down of the pressure of greater than 5 minutes later,
preferably greater than 15 minutes later and most preferably
greater than 30 minutes later.
d. Chemical Heat Break Check
[0128] It is sometimes desirable to be able to simultaneously shut
down the temperature and pressure on the system without any time
delays. In order to achieve this desire, a heat break system was
developed that could allow for: [0129] separation of heated and
cold material via a heat break, [0130] temporary disruptions in
dispensing activated material, [0131] long term shut down and start
up scenarios, and [0132] immediate disruption in temperate and/or
pressure.
[0133] The present invention thus provides an alternative
embodiment of a chemical heat break check 110 and methods utilizing
the same for preventing the activatable material from flowing back
into the non-heated portions of the system when the pressure is
relieved. The heat break check 110 prevents irreversible plugs from
forming and eliminates the need for complex systems. The heat break
check 110 according to the invention is suitable for systems that
have both heated and room temperature components. It keeps hot and
cool material separate in the system when pressure is relieved on
the system.
[0134] The heat break check 110 has the same external attributes
and features as previously described. However, with reference to
FIG. 4, which shows an exploded perspective view of this embodiment
of the heat break 110, the heat break 110 further comprises an
internal dissipater 190, which as described below, improves the
performance of the heat break 110 when pressure on the system is
relieved. FIGS. 4 and 5 show cross-sectional views of the fully
assembled heat break 110 shown in FIG. 4.
[0135] A cold end 170 of the heat break 110 is in fluid
communication with an unheated a supply conduit and a hot end 180
of the heat break 110 is in fluid communication with the heated
material in the heat exchanger/dispenser. The second heat
dissipater 190 in the heat break check 110 induces solidification
of heated material within the heat break check when the pressure is
relieved and the system is cooled down by allowing the heated
material to flow back through a high surface area fitting that is
adapted to rapidly heat and/or cool, depending upon whether the
system is operating or not. Upon start-up, the novel design of heat
break check allows the plug 200 (see FIG. 6) that was formed in the
heat break check upon shutdown to be reheated, plastified and/or
liquefied sufficiently to allow the pressure of the system to
reversibly push it in the heat exchanger thereby eliminating
unwanted irreversible drops in pressure or stoppage of the
dispensing system. The subject of this invention contained an
external heat dissipater 150 and an internal heat dissipater 190.
The external heat dissipater served the conventional purpose
described above. The internal heat dissipater 190 includes a high
surface area pin 220 and a groove portion 230, which is cooled by
the incoming glue during normal operation. When the pressure is
disrupted or rapidly turned off, the activated material pushes back
toward the pin 220, where it undergoes rapid cooling and thereby
creates a solid plug 200, which acts a chemical check allowing the
system to begin normal dispensing even after an abnormal disruption
in dispensing. This plug 200 can be dislodged via pressure supplied
by the pump 60, when normal operations resume.
[0136] Thus, a heat break 110 according to this embodiment of the
invention comprises: [0137] a first insulator 80 made of a
non-conductive material, most preferably constructed from PEEK, and
[0138] a heat dissipater 150 made of a conductive material, most
preferably aluminum, [0139] an internal heat dissipater 190 made of
conductive material, most preferably constructed of aluminum, and
optionally [0140] a second insulator 160, preferably made of
PEEK,
[0141] Most preferably, the combination of the friction loss coil
and heat break check allows for a system that experience gradual
pressure loss on shutdown and cooling that result in a system that
is substantially pressure equalized from the reservoir to the heat
break check. This unique combination avoids unwanted pressure
differentials thereby eliminating areas of separated dry and liquid
components, cooled activatable material in undesirable locations in
the cool areas, and results in clean start-ups and production
sequences.
[0142] The following examples are intended only to illustrate the
invention and should not be construed as imposing limitations upon
the claims.
Test Procedures
Standard Test Procedure 1: Viscosity
[0143] The viscosities were measured with a Brookfield viscometer
after the spindle had equilibrated for 10 minutes.
Standard Test Procedure 2: Centrifuge Stability
[0144] Centrifuge tubes were loaded with the pumpable liquids and
centrifuged for greater than 30 minutes. The tubes were compared
for separation into the various components and rated on a scale of
good to poor.
Standard Test Procedure 3: Bond Time
[0145] Bond time testing was carried out by pumping the liquid
emulsion, dispersion or suspension at a specified pressure on a
hydraulic pump with a 15:1 pumping ratio to a reactor set at a
variable temperature generally described in the '859 patent. The
heating and any resultant chemical reactions occurred in the period
of time defined as being the moment the Liquid Polymer Composition
sample entered the heated reaction zone in the reactor to the
moment that the dispensed material solidified on as a foamed solid
material on a substrate.
[0146] To determine the weight of adhesive composition applied, a
1.5 inch strip of adhesive was dispensed onto a piece of masking
tape. After the adhesive cooled, the 1.5 inch adhesive strip was
removed from the masking tape and weighed. This was done three
times and the average of the weights was registered as the Average
Weight of Bead to normalize the data taken on the adhesive
performance.
[0147] To determine adhesive performance, a corrugated cardboard
substrate was first attached to a 656 g base plate and then a 1.5
inch strip of the adhesive composition was dispensed on the
substrate while the substrate (attached to said plate) was passed
under a liquid hot melt dispenser (specifically a Hydromatic.TM.
from Liquid Polymer Corporation, Lorain, Ohio) at a conveying speed
of 75' per minute. After dispensing the adhesive, and after waiting
for a variable period of pre-lamination time (t1), a second
corrugated substrate of equal dimensions was laminated to the top
of the first substrate under constant pressure for a variable
period of time under pressure (t2). Next, the second substrate was
vertically lifted to test the laminated structure's ability to
support the weight of the base plate without delaminating. The
shortest period of time under pressure (t2) that can be tolerated
without leading to delamination was defined as the Bond Time (three
consecutive passing tests of separate laminates are required before
a process condition was deemed to yield a Bond Time). The
Normalized Bond Time was then derived at by taking the (Bond Time
t2)*Average Weight of Bead)/0.10 grams. A shorter Bond Time
correlates with faster and more effective adhesives.
Standard Test Procedure 4: Hand Gun Test
[0148] Processability was measured by pumping the liquid emulsion,
dispersion or suspension at a specified pressure on a hydraulic
pump with a 15:1 pumping ratio to a reactor set at a variable
temperature generally described in the '859 patent. The heating and
any resultant chemical reactions occurred in the period of time
defined as being the moment the liquid sample entered the heated
reaction zone in the reactor to the moment that the dispensed
material solidified on as a foamed solid material on a substrate.
The test was run at 50 psi using a TurboActivator (equipment
available from Liquamelt Corp.) at 350.degree. F. and hand gun at
350.degree. F. A simple protocol for pass/fail was developed. If
the equipment was able to dispense for 20 seconds it was considered
a pass. Anything less than this was considered a failure.
Standard Test Procedure 4: Plastic Bond Test
[0149] Plastic Bonding was measured by pumping the liquid emulsion,
dispersion or suspension at a specified pressure on a hydraulic
pump with a 15:1 pumping ratio to a reactor set at a variable
temperature generally described in the '859 patent. The heating and
any resultant chemical reactions occurred in the period of time
defined as being the moment the liquid sample entered the heated
reaction zone in the reactor to the moment that the dispensed
material solidified on as a foamed solid material on a substrate.
The test was run a 60 psig, TurboActivator at 350.degree. F. and
hand gun at 350.degree. F. A simple protocol for pass/fail was
developed. A bead was applied to a polyester plastic film, followed
by the application of urethane foam and fiber strap. If the foam
the foam tore, it was considered a pass-if it did not tear, it was
a failure. If the fiber strap held upon pulling by hand, it was
considered a pass-if it did not hold, it was a failure. To pass the
test, both the foam and strap evaluations had to pass.
Standard Test Procedure 5: Equipment Configuration Test
Protocol:
[0150] A reservoir or container containing the unactivated liquid
material is fluidly connected to the high pressure hydraulic system
consisted of a Graco Fireball Pneumatic Piston Pump 15:1 which
pumps the unheated material from the low pressure side to the high
pressure side of the system. The standard material used in this
test is LM1250, available from Liquamelt Corp. Upon exiting the
pump, it is connected to a brass 1/2'' inside diameter check valve
which hooked up a manifold. A 10 foot hydraulic hose is fluidly
connected to the manifold. The standard pressure for testing the
performance of the heat break system was 60 psig which translates
to approximately 900 psi hydraulic pressure on the hydraulic
hose.
[0151] Optionally, a friction loss outlet is also fluidly connected
to the manifold depending on the particular testing to be carried
out.
[0152] The outlet of the hydraulic hose was fluidly connected with
various heat break configurations for testing.
[0153] Pressurized unheated material flows sequentially through the
heat break or heat break check and then a heat exchanger. The heat
exchanger heat-activates and mixes and activates the material,
which can be selectively dispensed through a dispenser nozzle.
Pressurized unheated material flows sequentially into the heat
break configuration to a TurboActivator as described in Jorgenson,
et. al. The outlet of the TurboActivator was connected to a
standard automatic dispensing device consisting of a standard
manifold and gun module with 0.016 inch opening. Both the
TurboActivator and manifold temperature were controlled to
350.degree. F.
Raw Material Identification
Raw Material Chemicals
[0154] The materials and abbreviations listed below are referenced
in the following examples: [0155] MICROTHENE.RTM. FE532 EVA
[24937-78-8], 9% vinyl acetate, melt index=9, from Equistar;
average particle size=20 microns with a particle size distribution
5-50 microns [0156] ATEVA.RTM. 1820; poly(ethylene-co-vinyl
acetate), 18% vinyl acetate, melt index=3 g/10 min., from Celanese
[0157] ATEVA.RTM. 1941; poly(ethylene-co-vinyl acetate), 19% vinyl
acetate, melt index=30 g/10 min., from Celanese [0158] ATEVA.RTM.
2830; poly(ethylene-co-vinyl acetate), 28% vinyl acetate, melt
index=150 g/10 min., from Celanese [0159] MAPP-1, Licocene 6252
maleated polypropylene, from Clariant [0160] MAPP-2, E-43 maleated
polypropylene, from Westlake Chemical Corporation [0161] MAPP-3,
A-C925 maleated polypropylene, A-C Performance Products, a division
of Honeywell Corporation [0162] Polypropylene 1, Licocene 6102
polypropylene, from Clariant [0163] Polypropylene 2, A-C1660
polypropylene, A-C Performance Products, a division of Honeywell
Corporation [0164] Polyethylene 1, AC-8 polyethylene, from A-C
Performance Products, a division of Honeywell Corporation [0165]
Polyethylene 2, Licocene 5301 polyethylene, from Clariant [0166]
Soy Bean Oil RBD (Refined, Bleached, Deodorized), from Archer
Daniels Midland Company [0167] Water [0168] HI-SIL.TM. T-700
Silica, Silica Thickener, synthetic amorphous silicon dioxide, PPG
Industries, Inc. [0169] LoVel.TM. 29 Non-Treated Silica Flatting
Agent, synthetic amorphous precipitated silicas, PPG Industries,
Inc. [0170] Pluronic F-127, surfactant, from BASF [0171] Sodium
bicarbonate, Industrial grade, from Solvay Chemicals [0172] Irganox
B225;
Tetrakis(methylene(3,5-di-tertbutyl-4-hydroxyhydrocinnamate))methane
and Tris(2,4-ditert-butylphenyl) phosphate, Antioxidant, from
BASF
Draw Material Chemical Sample Preparation
Standard Preparation Procedure 1: Ground Ethylvinyl Acetate
Polymers.
[0173] While the precise values for the particle size distribution
are not critical to the invention, the ethylene vinyl acetate
polymers used in the examples were mechanically ground to the size
distribution set forth in Table 1 below:
TABLE-US-00001 TABLE 1 Rotap Information (U.S. Standard Sieves) %
of polymer on screen 35 Mesh Screen (500 microns) <0.5% 40 Mesh
Screen (425 microns) <35% 60 Mesh Screen (250 microns) <45%
80 Mesh Screen (180 microns) <45% 100 Mesh Screen (150 microns)
<15% 140 Mesh Screen (106 microns) <15% Pan (<140 Mesh
Screen) <15%
Standard Preparation Procedure 2: Ground Polypropylene.
[0174] While the precise values for the particle size distribution
are not critical to the invention, the polypropylene polymers used
in the examples were mechanically ground to the size distribution
set forth in Table 2 below:
TABLE-US-00002 TABLE 2 Rotap Information (U.S. Standard Sieves) %
of polymer on screen 40 Mesh Screen (425 microns) <0.5% 60 Mesh
Screen (250 microns) <15-35% 80 Mesh Screen (180 microns)
<15-25% 100 Mesh Screen (150 microns) <5-10% 140 Mesh Screen
(106 microns) <10-15% Pan (<140 Mesh Screen) <20-75%
Standard Preparation Procedure 3: Ground Maleated
Polypropylene.
[0175] While the precise values for the particle size distribution
are not critical to the invention, the polypropylene polymers used
in the examples were mechanically ground to the size distribution
set forth in Table 2 below:
TABLE-US-00003 TABLE 3 Rotap Information (U.S. Standard Sieves) %
of polymer on screen 40 Mesh Screen (425 microns) <0.5-10% 60
Mesh Screen (250 microns) <15-35% 80 Mesh Screen (180 microns)
<15-25% 100 Mesh Screen (150 microns) <5-10% 140 Mesh Screen
(106 microns) <10-15% Pan (<140 Mesh Screen) <20-75%
PREPARATION OF COMPONENT TWO EXAMPLES
Comparative Intermediate Examples 1A-1E
[0176] In preparing the comparative examples for intermediates, the
polypropylene, polyethylene, oil and/or silica and/or surfactant
were heated to >250.degree. F. to create a molten homogeneous
liquid. The molten material was allowed to cool to create the first
set of comparative Intermediate Examples 1A-1E. This set of
examples represents one extreme where the polymers are above the
melting point and/or solubility point in the carrier component.
TABLE-US-00004 TABLE 4 Comparative Comparative Comparative
Comparative Comparative Intermediate Intermediate Intermediate
Intermediate Intermediate Ingredient ID 1A 1B 1C 1D 1E Soybean Oil
41.5 41.5 14 13.5 13.5 Polypropylene-1 16.5 0 8 2 2 Polyethylene-1
0 3 0 1.9 1.9 Silica 0.5 0.5 0.5 0 0 Pluronic F-127 0 0 0 0.2 0
Exemplary Intermediate Examples 2A-2B
[0177] In preparing the exemplary examples for intermediates, the
polypropylene, polyethylene and silica were heated to approximately
260.degree. F. to create a molten homogeneous liquid. The molten
material was dispensed using a standard hot melt unit with a module
fitted with a spray pattern nozzle to dispense the molten liquid
into the room temperature soybean oil to create the first set of
exemplary Intermediate Examples 2A-2B. In this example, the
intermediate was dispersed in oil that created domains where the
oil was well below the melting or solubility temperatures but above
the room temperature in the regions where the molten homogeneous
liquid enters the carrier.
TABLE-US-00005 TABLE 5 Exemplary Intermediate Exemplary
Intermediate Ingredient ID 2A 2B Soybean Oil 41.5 41.5
Polypropylene-1 16.5 16.5 Polyethylene-1 0 0.25 Silica 0.5 0.5
Exemplary Intermediate Examples 3A-3C
[0178] In another embodiment of the invention the oil and silica
were heated to approximately 200 to 230.degree. F. and the highest
melting polymers which had melting points of about 300.degree. F.,
polypropylene and maleated polypropylene, were added, stirred and
allowed to bring the temperature down to less than 190.degree. F.
where the polymer having lower melting points of about 200.degree.
F., polyethylene, was added stirred and allowed to cool.
TABLE-US-00006 TABLE 6 Comparative Comparative Comparative
Intermediate Intermediate Intermediate Ingredient ID 3A 3B 3C
Soybean Oil 41.5 41.5 40.5 Polypropylene-1 16.5 16.5 16.5 Maleated
PP-1 0 0 4 Polyethylene-1 0 3 3 Silica 0.5 0.5 0.5 % Premix Total
58.5 61.5 64.5
Exemplary Intermediate Examples 4A-4E
[0179] In another embodiment of the invention the oil and silica
was heated to approximately 130.degree. F. and the highest melting
polymers which had melting points of about 300.degree. F.,
polypropylene and maleated polypropylene, were added, at which time
the polymer having lower melting points of about 200.degree. F.,
polyethylene, was added stirred and then the entire mixture was
heat to 145.degree. F. and the temperature is maintained for 20
minutes and then allowed to cool. Examples 4A and 4C.
[0180] Example 4B follows the same process as described for example
4A except for that at 100.degree. F., the EVA is added to the
formulation and mixed for 5 minutes. The mixture is then allowed to
cool.
[0181] Example 4D follows the same process as described for example
4A except that instead of Silica, Pluronic F-127 surfactant is
added to the oil at the start of the process.
[0182] Example 4E follows the same process as described for example
4A except that Irganox B225 is added to the oil silica mixture at
the start of the process.
TABLE-US-00007 TABLE 7 Exemplary Exemplary Exemplary Exemplary
Exemplary Intermediate Intermediate Intermediate Intermediate
Intermediate Ingredient ID 4A 4B 4C 4D 4E Soybean Oil 41.5 41.5
41.5 41.5 41.5 Polypropylene-1 16.5 16.5 -- 2 16.5 Polypropylene-2
-- -- 16.5 14.8 -- Maleated PP-1 4.1 4.1 4.1 4 4.1 Polyethylene-1 3
3 3 3 3 Silica 0.5 0.5 0.5 0 0.5 Pluronic F-127 0 0 0 0.2 0 Ateva
1820 0 24.3 0 0 0 Irganox B225 0 0.1 0 0 0.1 % Premix Total 65.6 90
65.6 65.5 65.7
Exemplary Intermediate Examples 5A-5B
[0183] In another embodiment of the invention the oil was heated to
approximately 100.degree. F. at which point the Ateva 2830 EVA is
added to the mixing, heated oil. Once the Ateva 2830 EVA is
dispersed into the oil, Pluronic F-127 (surfactant) is added
followed immediately by the Irganox B225 (antioxidant) and the
Sodium Bicarbonate. As the temperature reached 110.degree. F., the
mixture is charged with polypropylene. As the temperature reached
115.degree. F., the mixture is charged with maleated polypropylene.
The temperature is then increased to 130.degree. F., at which point
the heat is turned off and the mixture was then allowed to cool.
Example 5A.
[0184] Example 5B follows the same process except for the fact that
once all the dry raw materials were charge to the heated oil, the
formulation was heated to a maximum temperature of 125.degree. F.
for a period of 15 minutes prior to removing the heat and allowing
the mixture to cool.
[0185] Example 5C follows the same process as 5A except for the
fact that once all the dry raw materials were charge to the heated
oil, the formulation was heated to a maximum temperature of
125.degree. F. at which point the heat was removed allowing the
mixture to cool.
[0186] Example 5D follows the same process as 5C except for the
fact that it does not contain Sodium Bicarbonate.
[0187] Example 5E follows the same process as 5C except for the
fact that it does not contain either Sodium Bicarbonate or Pluronic
F-127 surfactant.
TABLE-US-00008 TABLE 8 Comparative Comparative Comparative
Comparative Comparative Intermediate Intermediate Intermediate
Intermediate Intermediate Ingredient ID 5A 5B 5C 5D 5E Soybean Oil
30 43 43 41.92 42.56 Polypropylene-1 3 3 2.92 2 Polypropylene-2
7.85 7.85 7.85 7.65 10.02 Maleated PP-1 2.5 2.5 2.44 4.5 Maleated
PP-2 4 4 4 3.9 -- Polyethylene-2 -- -- 2.25 2.19 2.26 Pluronic
F-127 0.2 0.2 0.2 0.2 -- Ateva 2830 EVA 2.5 2.5 2.5 2.44 2.51
Irganox B225 0.15 0.15 0.15 0.15 0.15 Sodium Bicarbonate 0.1 0.1
0.1 -- -- % Premix Total 44.8 63.3 65.55 63.81 64
COMPARATIVE EXAMPLES
Low Viscosity
Shelf Stable Materials
Viscosity/Stability Results
[0188] In each case the Intermediate was cooled close to room
temperature and the additional ingredients were blended up to make
the final room temperature pumpable emulsion, dispersion or
suspension. 1A shows the expected results of a solid as with the
liquid carrier no longer being effective in providing a pumpable
liquid. The products provided utilizing 2A and 3A show remarkably
low viscosity and stability when compared to 1A. In the preferable
process, 3A and 3B demonstrates that very high solids content, low
viscosity and shelf life stability can be simultaneously obtained.
In the even more preferable process, 4A demonstrates that even
higher solids content, low viscosity and shelf life stability can
be simultaneously obtained.
TABLE-US-00009 TABLE 9 Intermediate ID 1A 2A 3A 1B 2B 3B 4A % % % %
% % % Intermediate 58.5 58.5 58.5 45 58.75 61.5 65.6 Soybean Oil --
-- -- -- -- -- -- Water 1 1 1 1 1 1 1 Polypropylene-1 0 0 0 16.5 0
0 -- Polypropylene-2 -- -- -- -- -- -- -- Polyethylene-1 3 3 3 0
2.75 0 -- MAPP-1 4.2 4.2 4.2 4.2 4.2 4.2 -- FE 532 (EVA) 9 9 9 9 9
9 9 ATEVA 1820 24.3 24.3 24.3 24.3 24.3 24.3 24.3 Pluronic F-127 --
-- -- -- -- -- -- Irganox B225 -- -- -- -- -- -- 0.1 Viscosity
(cps) Solid 14,675 8,225 13,600 16,075 7,050 11,300 Stability NA
Good Good Good Good Good Good
Bond Time Testing
[0189] Bond time testing was carried according to the test
procedures. Results are reported in Table 10 below:
TABLE-US-00010 TABLE 10 Ingredient ID 2A 2C 3C 4A FE532 9 9 9 9
1820 EVA 24.3 24.3 24.3 24.3 Soy 41.5 41.5 41.5 41.5 (MAPP) 4.2 4
4.2 4.1 (PP) 16.5 16.5 16.5 16.5 Water 1 1 1 1 AC 8 (PE) 3 3 3 3
Pluronic F-127 0 0 0 0 LoVel 29 0.5 0.5 0.5 0.5 Irganox B 225 -- --
-- 0.1 Viscosity (cP) 14675 15750 7000 11300 Stability Good Good
Good Good 320.degree. F./50 PSI (sec) 0.7 0.7 0.6 0.5 Bead Weight
(g) 0.07 0.06 0.08 0.07 320.degree. F./90 PSI (sec) 0.6 0.4 0.6 0.4
Bead Weight (g) 0.24 0.25 0.19 0.22 350.degree. F./70 PSI (sec) 0.5
0.5 0.5 0.5 Bead Weight (g) 0.21 0.20 0.18 0.18 380.degree. F./90
PSI (sec) 0.7 0.6 0.6 0.5 Bead Weight (g) 0.1 0.12 0.11 0.13
380.degree. F./90 PSI (sec) 0.7 0.8 0.5 NA Bead Weight (g) 0.35
0.39 0.31 0.33 NA = Material too low, viscosity causing bounce
off.
[0190] The foregoing examples demonstrate the criticality of oil
temperature relative to the temperature of the polymers in the
formation of a low-viscosity intermediate. When the temperature of
the oil is near, but below, the melting point of the polymers used
in the composition, intermediates (Examples 3A-3C, 4A) can be
obtained that have lower viscosity as compared to intermediates
obtained when the oil is at a temperature above the melting point
of the polymers (Examples 1A-1C). The methods of the invention can
be utilized to prepare compositions that exhibit long-term
stability and low viscosity.
Unique Bonding and Application in Plastic Assembly Example
TABLE-US-00011 [0191] TABLE 11 Hand Gun Test Results Intermediate
ID None 4C 4E 1D 1E 4D 5A 5B % % % % % % % % Intermediate % 0 65.6
65.7 17.6 17.4 65.5 44.8 63.3 Soybean Oil 41.5 -- -- 28 28 -- 13 --
Water 1 1 1 1 1 1 1.25 1.25 Polypropylene- 16.5 0 0 -- -- -- 3 -- 1
Polypropylene- -- -- -- 14.8 14.8 -- -- -- 2 Polyethylene-1 3 3 3
1.1 1.1 -- -- -- Polyethylene-2 -- -- -- -- -- -- 2.25 2.25 MAPP-1
4.1 4.2 4.2 4 4 -- 2.5 -- FE 532 (EVA) 9 9 9 8.95 8.95 8.95 9.2 9.2
ATEVA 1820 24.3 24.3 24.3 24.3 24.3 24.3 12 12 (EVA) Ateva 1941 --
-- -- -- -- -- 12 12 (EVA) Pluronic F-127 -- -- -- -- -- -- -- --
Irganox B225 0.1 -- -- 0.15 0.15 0.15 -- -- Silica 0.5 -- -- -- --
-- -- -- Sodium -- -- -- 0.1 0.1 0.1 -- -- Bicarbonate Hand Gun
Test Fail Pass Pass Fail Fail Pass Fail Fail Plastic Bond -- --
Pass Fail -- -- -- Fail Test
[0192] The foregoing examples demonstrate the inherent benefit of
improved processing in the Turbo Activator.RTM. as it relates to
the processing of the intermediate. Utilizing the Hand Gun Test
protocol, a distinctive relationship between the intermediate
process and the ability to pass the test is demonstrated.
Intermediates 4C, 4D and 4E all demonstrate the enhanced
processability of their final formulation as it relates to the
passage of the Hand Gun Test protocol. While the remaining examples
in table 11 further support the evidence of the unique benefits of
Intermediate Process group 4.
[0193] Surprisingly, it was discovered that these compositions not
only had the unexpected advantage of being low viscosity and shelf
stablility in the preactivation stage; but it performed
advantageously on low surface energy plastic substrates. When
compositions were prepared according to the invention the resulting
product successfully bonded foam to plastic shields and fiber
straps to the same shields. The material prepared by conventionally
mixing the same raw materials at room temperature failed.
Equipment Stabilization Compositions
TABLE-US-00012 [0194] TABLE 12 Equipment Stabilizing Compositions
Comparative Exemplary Exemplary Exemplary Exemplary Example 6A
Example 6B Example 6C Example 6D Example 6E Stabilizer Ingredient
Soda Ash Stabilizer Zn(Stearate) ZnO ZnO Package 2 Stabilizer
Concentration 0.15 1.24 1 0.1 0.075 Intermediate ID 5C 5C 5C 5D 5E
Intermediate % 65.45 64.72 62.98 63.8 64 Soybean Oil -- -- 0.98
0.99 -- Water 1.25 1.24 0.98 0.99 0.99 FF 532 (EVA) 9.19 9.09 8.98
9.11 9.10 ATEVA 1820 (EVA) 23.96 23.72 -- -- 9.68 Ateva 1941 (EVA)
-- -- 24.65 25.00 16.14 Silica -- 0.49 -- -- -- Sodium Bicarbonate
-- -- 0.40 -- -- Soda Ash 0.15 -- -- -- -- Calcium Carbonate --
0.20 -- -- -- Zinc Stearate -- 0.20 1.00 -- -- Zinc Oxide -- -- --
0.10 0.08 Zinc (Dust) -- 0.1 -- -- -- Chemstat HTSA #22-20M -- 0.25
-- -- -- Time without Failure (min) -- 15500 9,260 20,220 2,640
Time to Failure (min) 3,043 Did not fail Did not fail Did not fail
Did not fail Gun Cycles 73,032 372,000 222,240 485,280 63,360 Total
module test time 3,043 15,500 9,260 38,210 40,850
[0195] The activated material composition in Example 6A failed with
a stainless steel needle and seat in a very short period of time
which was unexpected. Surprisingly, we found that zinc related
materials extended the life of the seat and needle. It was
theorized that adding a slip agent, a sacrificial metal ion, or
metal stabilizer could interact with the material and equipment to
create a stable interface for materials made and used according to
the subject invention.
Friction Loss/Process Comparative Examples
TABLE-US-00013 [0196] TABLE 13 Friction Loss/Process Experiment 7A
7B 7C 7D 7E Resistor NA 30' aluminum 30' Aluminum 30' Aluminum 30'
Aluminum Dispense Time 90 min 50-270 min 10 min 15 min 10 min
Variable Changed -- Added resistor -- Added resistor Left Pressure
to 6A in after the check on for 15 between the valve so it can
minutes after pump and relieve shutting off check valve pressure
temperature Pump Result Fail Pass Pass Pass Pass Product separated
in pump Hose Result -- NA Fail Pass Pass Dry material plug Heat
Break Result -- NA Fail Fail Pass Dry material Plug with cured
material Start Up Evaluation Fail NA Weak then Fail Fail Pass
Temperature Off 0 min 0 min 0 min 0 min 0 min Pressure Off 0 min 0
min 0 min 0 min 15 min Time to Cool NA NA 45 min 45 Min 45 min
Turbo
[0197] Standard Test Procedure 6 for equipment testing was used in
Examples 7A-7E. The heat break configuration is the subject of this
invention; peek-aluminum-peek. Test Comparative Example 7A and
exemplary Example 7B clearly demonstrate the advantage of a
friction loss component (resistor) in ensuring the pressure
differentials found in the pump do not lead to unwanted separation
of the polymer and carrier which ultimately create unwanted
packouts. Examples 7C-7E demonstrate that the location of the
friction loss component (resistor) not only insures the smooth
operation of the hydraulic pump during interruptions and slow
dispensing; but allows for a reversible plug to be formed and
allows for the system pressure to be gradually released thereby
minimizing pressure differentials which lead to separation which
can result in poor start ups to total failure of the system
starting.
Chemical Heat Break Examples
TABLE-US-00014 [0198] TABLE 14 Friction Loss/Process Heat break
Experiment # description 8A 8B 8C 8D 8E 8F First Component NA Peek
Aluminum Peek Peek Peek Second Component NA NA Peek Aluminum
Aluminum Aluminum Third Component NA NA NA NA Peek Peek Chemical
Check NA NA NA NA NA Yes Heat break ID NA 1/8'' 1/4'' 1/4'' 1/4''
1/4'' Plug Location 6'' into 2'' into 0.2'' into 0.2'' into Plug
stops Plug stops hydraulic hydraulic hydraulic hydraulic half way
half way hose hose hose hose through through third second component
component Start Up Evaluation Fail Fail Fail Fail Weak Pass
[0199] Standard Test Procedure 6 for equipment testing was used in
Examples 8A-8F. Test Comparative Example 8A-8C clearly demonstrate
the necessity of a heat break in the system and show the advantage
of a larger diameter for the activated material move forward and
backward as the system experiences different conditions. Examples
8D-8F demonstrate the importance of the chemical check component of
the heat break design. The chemical check forces the plug to stop
mid way through the aluminum, this allows the plug to be
reactivated on a startup and pushed through the system. By
reactivating the plug, material can be moved through the system
efficiently, providing a clean startup. If the plug is located past
the aluminum component, the plug cannot be reactivated and startup
will be considered weak or a failure, as demonstrated in examples
8D-8E.
[0200] Additional advantages and modifications will readily occur
to those skilled in the art. Therefore, the invention in its
broader aspects is not limited to the specific details and
illustrative examples shown and described herein. Accordingly,
various modifications may be made without departing from the spirit
or scope of the general inventive concept as defined by the
appended claims and their equivalents.
* * * * *