U.S. patent number 3,879,575 [Application Number 05/444,344] was granted by the patent office on 1975-04-22 for encapsulating compound and closure.
This patent grant is currently assigned to Bell Telephone Laboratories, Incorporated. Invention is credited to Donald Patrick Dobbin, Charles Anthony Fritsch, Raffaele Antonio Sabia.
United States Patent |
3,879,575 |
Dobbin , et al. |
April 22, 1975 |
Encapsulating compound and closure
Abstract
Articles, and particular telephone splices, are protectively
encased in a material consisting of a low viscosity oil gelled by a
block copolymer such as styrene-iosprene-styrene. Addition of
polyethylene to the blend reduces the yield shear stress in the
gelled compound and also advantageously supplies a desirable high
temperature property of nonslump. Component ranges are described.
Stratifying the compound within the closure so that the portion
contacting splices is soft and plastic while the remainder is stiff
and hard, meets a stringent encasement requirement while minimizing
oil separation at high operating temperatures.
Inventors: |
Dobbin; Donald Patrick (Clark,
NJ), Fritsch; Charles Anthony (Mendham, NJ), Sabia;
Raffaele Antonio (Atlanta, GA) |
Assignee: |
Bell Telephone Laboratories,
Incorporated (Murray Hill, NJ)
|
Family
ID: |
23764519 |
Appl.
No.: |
05/444,344 |
Filed: |
February 21, 1974 |
Current U.S.
Class: |
174/92; 174/76;
439/521; 174/23C; 174/87; 524/525 |
Current CPC
Class: |
H02G
15/18 (20130101); H02G 15/117 (20130101); G02B
6/4447 (20130101) |
Current International
Class: |
H02G
15/117 (20060101); H02G 15/18 (20060101); G02B
6/44 (20060101); H02G 15/10 (20060101); H02g
015/08 () |
Field of
Search: |
;174/76,87,88,92,93,23R,23C ;252/316,63 ;117/161 |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
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|
|
|
|
|
|
450,088 |
|
Jul 1936 |
|
GB |
|
1,199,997 |
|
Jul 1970 |
|
GB |
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1,203,138 |
|
Aug 1970 |
|
GB |
|
121,553 |
|
Mar 1971 |
|
NO |
|
Primary Examiner: Clay; Darrell L.
Attorney, Agent or Firm: Graves; C. E.
Claims
What is claimed is:
1. In combination: a plurality of insulated conductor splice points
enveloped in a waterproof encapsulating agent comprising from 84.5
to 92.5 parts by weight of mineral oil, from 0.5 to 3.0 parts by
weight styrene-isoprene-styrene block copolymer, and from 6.0 to
13.0 parts by weight of polyethylene having a weight average
molecular weight above 2000.
2. A closure receiving and encapsulating therein a plurality of
spliced insulated conductors, comprising:
a lower shell and an upper shell mating along extended flat edge
portions and each shell having a recess,
a plurality of spliced electrical conductors disposed between said
shells
the recess of each said shell containing an encapsulating agent
enveloping said splicid electrical conductors, and comprising a
blend of from 84.5 to 92.5 parts by weight of mineral oil, from 0.5
to 3.0 parts by weight of styrene-isoprene-styrene block copolymer,
and from 6.0 to 13.25 parts by weight of a polyolefin.
3. A closure pursuant to claim 2, further comprising elongated clip
means fastening said upper and said lower shells together along
their respective extended edge portions.
4. A closure pursuant to claim 3, wherein the parts by weight of
said mineral oil are in the range of 84.5 to 87.0, the parts by
weight of said styrene-isoprene-styrene block copolymer are in the
range 1.5 to 3.0, and the parts by weight of said polyolefin are in
the range 10.0 to 13.25.
5. A closure pursuant to claim 4 wherein said agent condained in
each said mating shell is stratified into a first layer contacting
said electrical splices, and a second layer filling the remainder
of said shell, said first layer adapted to be rendered relatively
soft by subjecting the some to shearing motion and said second
layer being relatively rigid providing stiff support and protection
for said first layer.
6. An article of manufacture useful as a closure for protecting a
plurality of spliced insulated conductors of a telephone cable
comprising:
a lower shell and an upper shell having flat outer edges formed as
a generally rectilinear extending lip, said lower half being joined
to said upper half along a common hinge formed by a connection of a
lip edge of said first half and a corresponding lip edge of said
second half,
an encapsulating agent substantially filling said lower half and
said upper half and comprising:
a blend of from 84.5 to 92.5 parts by weight of mineral oil, from
0.5 to 3.0 parts by weight of styrene-isoprene-styrene block
copolymer, and from 6.0 to 13.25 parts by weight of a polyolefin,
the said agent being stratified into a first layer located
substantially at the level of said edges for contacting said
splice, and a second layer filling the remainder of said lower half
and said upper half, said first layer adapted to be rendered
relatively soft by subjecting the same to shearing motion, and said
second layer being relatively rigid to supply stiff support and
protection for said first layer, and a sheet of separator material
placed over said first layer.
Description
FIELD OF THE INVENTION
This invention relates in general to protection of articles from
hostile ambients by encasing them in a protective fill. In an
important specific application, this invention relates to
moisture-proofing compounds for protecting electrical conductor
splice points. Still more specifically, the invention relates to a
system for protecting a multiplicity of telephone conductor splices
and includes a class of waterproofing compounds predisposed in a
closure for fast application in the field to splice points. In
another aspect, the invention relates to a class of compounds for
field pumping into closures around splice points.
BACKGROUND OF THE INVENTION
It is well known that one of the largest causes of telephone
service disruption and degradation is the entry of water into or
around the electrical connections at a cable splice point. Many
systems are used to combat the problem, including encapsulating
splicing connectors, elaborate and supposedly waterproof closure
designs to envelop the splice points, and circulating a drying gas
within the splice region.
More recently, systems of waterproof filler for telephone splice
closures are finding use. The purpose of the filling material is to
envelop the entire splice point in a waterproof mass, without in
the process entrapping any liquid water. Certain currently used
materials form nonreenterable plugs. A compound which allows
repeated reentry of the closure and access to the splice point is
more useful, however.
Design of a fully acceptable waterproof filling compound is not
just a matter of assuring its dielectric and physical compatibility
with the metal and plastic of the insulated conductors and splicing
connectors. Account must also be taken of the temperature-dependent
properties and the elasticity of the material. For example, the
flow temperature of the filler predisposed in the closure should be
at least greater than 140.degree.F and should ideally be greater
than 150.degree.F. This high flow temperature is needed to assure
that under extreme field conditions the filler will not slump or
leak out of the closure (since these rarely are reliably
liquid-tight).
In successfully applying the general invention to protecting
telephone splices, another important consideration has been
discerned. Applying the two factory-prefilled halves of the splice
closure to a splice in the field, involves bringing the two halves
together around the splices. In this process it is essential that
the compound "knit" or inelastically flow around each individual
connector splice, without becoming elastically strained. There must
be no elastic force buildup in the compound that would resist a
full enveloping of each splice.
A prime inventive object, therefore, is to realize a soft
encapsulating material that inelastically flows around splices over
a wide temperature range.
A further principal object of the invention is to realize a
waterproofing compound that has substantially the temperature
characteristics defined in the preceding paragraphs.
A general inventive object is to more effectively protect
electrical splice points from the corrosive effects of water,
particularly telephone conductors at splice points where the
corrosion can degrade or eliminate telephone service.
Another general inventive object is to provide an electrically and
chemically inert flowable material that will protect articles from
many adverse ambients.
SUMMARY OF THE INVENTION
In a broad sense the invention involves a protective encasing
material consisting of a low viscosity oil gelled by a block
copolymer.
Advantageously for telephone cable splices, the oil to be gelled is
a mineral oil because of its low viscosity at ambient temperatures
(360 in SUS units), and its low pour point of about 0.degree.F to
-15.degree.F. Also, mineral oil is a paraffinic/naphthenic material
and therefore will not stress crack splicing connectors which
increasingly are made of polycarbonate.
Pursuant to an important aspect of the invention, the filling
material is gelled using a block copolymer composed of
styrene-isoprene-styrene (hereinafter called SIS).
SIS when used alone in mineral oil in the range 0.5 to 5.0 weight
percent of the final product creates a substance ranging from an
elastic fluid to an elastic semirigid gel.
However, pursuant to this invention the undesirable elastic
properties of the foregoing are reduced by a blend of mineral oil,
SIS, and polyolefin wherein the SIS is present in from 0.5 to 5.0
weight percent of the total produce and the polyolefin is present
in from 6.0 to 15.0 weight percent of the total product. The
polyolefin performs the further desirable functions of
substantially reducing the yield shear stress in the final gelled
compound and also supplying high temperature stability or
resistance to slump up to substantially 150.degree.F.
An advantageous encapsulating gel within the above system consists
of mineral oil with from 1.5 to 3.0 weight percent of SIS and from
10.0 to 13.25 weight percent polyolefin stated in weight percent of
the total product. Compositions within these ranges exhibit gel
stability up to temperatures of 140.degree.-160.degree.F., as well
as substantial nonelasticity.
A preferred encapsulating gel consists of mineral oil, SIS and
polyolefin in which the SIS is present in from 2.0 to 2.25 weight
percent of the total product and the polyolefin is present in from
13.0 to 13.25 weight percent of the total product. Compositions
within these ranges are most desirable for nonelastic character and
high temperature slump resistance.
Within the broad invention, an inelastic gel which is sufficiently
fluid to be pumped at temperatures near 0.degree.F is achieved in a
blend of mineral oil, SIS and polyolefin in which the SIS is
present in from 1.5 to 2.0 weight percent of the final product and
the polyolefin is present in from 6 to 8 percent of the final
product.
A specific preferred encapsulant composition pursuant to the
invention, which exhibits both a high degree of inelasticity and
substantial temperature stability, consists of 84.5 weight percent
mineral oil, 2.25 weight percent SIS and 13.25 weight percent
polyethylene.
A specific preferred encapsulant composition useful for field
filling closures at temperatures near 0.degree.F, consists of 92.0
weight percent mineral oil, 2.0 weight percent SIS and 6.0 weight
percent polyethylene.
The preferred polyolefin is polyethylene because of its ready
processability. Either high density or low density polyethylene is
usable to substantially equal advantage in the invention. The most
advantageous number average molecular weight range within which the
polyolefin component of the present invention lies is substantially
from 1,000 to 15,000. A preferred range for ease of blending is
from 1,000 to 5,000. More specifically, a preferred range for
blending high density polyethylene is from 2,000 to 5,000.
The SIS component of the fill desirably is constituted of at least
two styrene blocks per molecule. The molecular weight distribution
advantageously, although not necessarily, falls within the range of
1-2. The weight average molecular weight of the styrene unit
advantageously falls within the range of 5,000 to 10,000. The
weight average molecular weight of the isoprene unit advantageously
falls within the range of 40,000 to 60,000. Desirably, the isoprene
unit weight average molecular weight is substantially 50,000. Also
advantageously, on a weight-percent basis, each isoprene block of
an average SIS molecule is about 60%, and each styrene block is
about 20%.
White mineral oils are a complex mixture of paraffin and naphthene
hydrocarbons which, for use in the present invention, prefereably
include approximately 18 to 36 carbon atoms with the hydrocarbons
substantially saturated. Importantly these oils undergo no phase
changes in the 0.degree.F through 160.degree.F temperature range of
present interest.
Pursuant to a further aspect of the invention the yield shear
stress of the gels is further reduced by preshearing the materials.
The original properties may be recovered, if desired, by reheating
the presheared material above about 194.degree.F.
Pursuant to another aspect of the invention, the requirement of
storability without leakage at 140.degree.-160.degree.F is met
concurrently with the requirement of "knit-around" when the
compound is applied to splices, by stratifying the compound within
the closure. With stratifying, the portion of the compound
contacting the splice is made relatively soft and plastic, while
the remainder is stiff and hard. The softening of the material is
achieved by subjecting it to shear forces, which break down some of
the bonds creating the gel.
The invention and its further objects, features, and advantages
will be made more readily apparent by the descriptions to follow of
illustrative embodiments.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic perspective diagram of a closure suitable for
receiving filling material of the invention;
FIG. 2 is a side schematic view showing the closure of FIG. 1
installed on a cable or cables;
FIG. 3 is a sectional front view of a closure similar to that of
FIG. 1; and
FIG. 4 is a further variety of closure suitable for use with the
filling material of the invention.
DETAILED DESCRIPTION OF ILLUSTRATIVE EMBODIMENTS
The invention will first be described by way of several
illustrations of materials systems consisting of various amounts of
mineral oil, SIS, and polyolefin (principally low density
polyethylene, and their preparation).
Example 1
A blend of 85 parts by weight mineral oil, 2 parts by weight SIS
and 13 parts by weight low density polyethylene with appropriate
stabilizer was produced. The polyethylene had a number average
molecular weight of substantially 2,000. Because the isoprene units
will oxidatively degrade by chain scission, the blending
temperature was kept between 316.degree.F and 364.degree.F. Due to
the compatibility of the materials, simple stirring with magnetic
bars was sufficient to bring all materials into solution. On
cooling substantially below the glass transition of polyethylene, a
gel was formed. The ability of the blend to remain cohesively
together under its own weight was tested. A 300 gram sample of the
blend was poured hot into a 400 ml circular beaker. The sample was
allowed to cool for a period of 17 hours after which its
temperature was about 70.degree. F. The sample was then turned
upside down and exposed to a temperature of about 140.degree.F for
48 hours. During this period mineral oil separation totaling less
than 1 percent of that originally present was measured, thus
establishing the ability of the blend to resist slumping.
Example 2
A composition consisting of 84.5 parts by weight mineral oil, 2.25
parts by weight SIS, and 13.25 parts by weight polyethylene was
made by the procedure of Example 1. A gel having substantially the
same characteristics of Example 1 was obtained.
Example 3
A blend of 85 parts by weight mineral oil, 3 parts by weight SIS
and 12 parts by weight polyethylene was made by the method of
Example 1. A sample was applied to a test splice connector and
visually found to exhibit only slight--and for most purposes
insignificant--drawback, signifying acceptable inelasticity. Slump
temperature properties were observed to be substantially as found
in the Example 1 composition.
Example 4
A blend of 85 parts by weight mineral oil, 5 parts by weight SIS
and 10 parts by weight polyethylene was prepared by the method of
Example 1. The blend exhibited no significant temperature slump
dissociation until the 140.degree.-160.degree.F range. Its
inelasticity was marginally acceptable at 70.degree.F. By hot-melt
encapsulation--that is, heating the blend to about 390.degree.F and
pouring the blend over the article to be encapsulated, and then
allowing the blend to gel on cooling--drawback resulting from the
relative elasticity is greatly minimized or eliminated.
Example 5
A blend of 87-3-10 parts by weight mineral oil, SIS, and
polyethylene respectively was prepared by the method of Example 1,
cooled to about 70.degree.F and applied to a test connector. Its
inelasticity was observed to be acceptable. On heating, no
significant temperature slump was encountered until the range of
140.degree.-160.degree.F. Use of this mix as a hot-melt encapsulant
is preferred.
Example 6
A blend of 86.5-3.5-10 parts by weight mineral oil, SIS, and
polyethylene respectively was prepared as in Example 1 and found to
exhibit substantially the same characteristics as did the Example 5
blend. Use as a hot-melt encapsulant is preferred.
Example 7
A blend of 85.5-1.5-13 parts by weight mineral oil, SIS, and
polyethylene respectively was prepared pursuant to the method of
Example 1. The blend exhibited the desirable high temperature
properties of the Example 1 blend.
Example 8
A blend of 84.5-0.5 -15 respective parts by weight of mineral oil,
SIS, and polyethylene was produced by the method of Example 1. The
resulting composition exhibited highly desirable temperature
stability to about 160.degree.F. The observed elasticity was
considered acceptable for certain encapsulation jobs. Hot-melt
encapsulation renders the blend acceptable for a wider range of
applications.
Example 9
A blend consisting of 92.0-2.0-6.0 parts by weight respectively of
mineral oil, SIS, and polyethylene was produced as in Example 1.
The resulting composition on cooling to 70.degree.F was acceptably
inelastic. A sample of the blend was placed in a syringe and
brought down to a temperature of 0.degree.F. The material was
easily extruded. from the syringe, without undergoing oil
separation or gel breakdown due to shearing. This material is
preferred as a fill to be applied to splice closured by crewman
working in the field during colder weather.
Example 10
A blend consisting of 92.5-1.5-6.0 parts by weight respectively of
mineral oil, SIS, and polyethylene was produced as in Example 1.
The resulting composition exhibited somewhat more softness than
that of Example 9, connoting a reduced but still acceptable
gel-producing pseudo-network. The product was easily pumped at
0.degree.F. Temperature stability up to substantially 140.degree.F
is obtainable.
Example 11
A blend consisting of 90.0-2.0-8.0 parts by weight respectively of
mineral oil, SIS, and polyethylene was produced as in Example 1.
The resulting composition exhibited a more desirable degree of
inelasticity than the products of Examples 9 and 10. Its
pumpability at 0.degree.F was demonstrated. Its temperature
stability was acceptable up to substantially
150.degree.-160.degree.F.
Experiments were made with blends of mineral oil and polyethylene
respectively without SIS. The resulting compositions significantly
lacked gel stability. Moreover, the compositions exhibited drastic
shear thinning (as, for example, when pumped or molded around a
splice), with insignificant recovery following termination of the
shear.
Experiments were also made with blends of mineral oil and 0.5-5.0
weight percent SIS, without polyethylene. The resulting gel at all
points exhibited at least an undesirable degree of elasticity, and
an undesirably narrow temperature stability range. The relative
acceptability of gel-type encapsulants as a function in part of gel
elasticity, is a factor not heretofore considered in any depth by
designers of encapsulants for electrical splices. The factor is
assessible in a number of ways, including: microscopic measurement
of "drawback" of a given encapsulant from a given splice
configuration; visual inspection of drawback in a given case, and
measurements on the materials themselves from which an
extrapolation as to elasticity factor may be made.
Experiments involving the last-noted method were made by
hot-casting of samples of the following blends in a syringe, and
then noting the volume percent swell when each is extruded from the
syringe.
______________________________________ Volume Percent Material
Swell ______________________________________ Mineral Poly- Oil SIS
ethylene 85.0 5.0 10.0 64 86.5 3.5 10.0 57 87.0 3.0 10.0 43 85.0
3.0 12.0 35 ______________________________________
The data suggests the variability of elasticity with differing
blends. It should be recognized, however, that overall
acceptability of a given gel is also a function of its temperature
stability properties.
Mineral oils suitable in the above formulations include Drakeol 35
from Pennsylvania Refining Co. and Pentol from Witco Chemical. In
general, mineral oils are all similar in composition; but some
contain impurities and unsaturated hydrocarbons, and vary in odor
and color. Many of the unsaturated hydrocarbons are aromatic and
these may cause stress cracking of polycarbonate, for example. For
this reason the use of an unsaturated mineral oil is some
applications of the invention would depend on its stress-cracking
activity. White mineral oil is a preferred material, however, for
its freedom from stress cracking.
An antioxidant stabilizer such as Irganoz 1010 available from
Ciba-Geigy, or Ionol from Shell Chemical of the hindered phenol
type has been found desirable. The addition of about 0.1 weight
percent of stabilizer to the compounds of Examples 1-11 is
desirable.
Closure Structure
A closure which is generally suitable to receive the preferred
compounds described above, is depicted in FIG. 1 as consisting of
an upper half 10 and a lower half 11, advantageously sharing a
common hinge 12. The fill material designated 13 is placed either
in the factory, or where appropriate in the field, within each of
the halves. The outer edges of the halves 10, 11 are formed as an
extending lip designated 10a for the upper half and 11a for the
lower half. To accommodate telephone cables to be spliced, the lips
10a, 11a are provided with a throat section formed by
semicylindrical portions denoted 15.
A variation of the closure shown in FIG. 1 is depicted in FIG. 2 as
having a dual diameter neck portion denoted 16, to accommodate, for
example, cables 17, 18 and wires 19, 20.
The assembling of either of the closures shown in FIG. 1 and FIG. 2
is facilitated by use of the spring clips such as 21, 22, 23, and
24 which grasp and secure the outwardly extending edges of the
upper and lower halves.
In order to meet the requirement of storage at temperatures at
least up to 140.degree.F without leakage for those closures filled
in the factory, the compound must have substantially strong bonds
which in turn may cause it to be harder or more solidified at
normal working temperatures than is desired. To the extent the
compound is elastic, it will not flow as readily into all the
interstices about the splices when the closure is sealed about the
splice joint. A method has been discovered of solving the foregoing
problem, by stratifying the compound within the closure. The
portion of the compound in intimate contact with the splices is
made relatively soft and flexible and thus can be easily
redistributed to fill all interstices thereabout. The remainder of
the compound in the closure is made stiff and thus provides added
strength to prevent leakage at the high storage temperatures.
One way of softening or deelasticizing the gels is to release the
yield shear stress by preshearing of the material. This can be
achived by any mechanical working of the material. Experiments have
also revealed that the original properties are recovered by a
reheating of the sheared material in the region of approximately
190.degree.F.
FIG. 3 is a cross-sectional view through the midsection of a
closure 110 in an open configuration showing a stratified formation
of the compound therein. A first layer or stratum 30a of compound
30 having a relatively rigid structure to provide stiff support at
the high storage temperatures and to inhibit the movement of the
conductor splices out to the walls of the cover, is formed in the
bottom of cavities 118 and 120 of cover halves 112 and 114,
respectively. A second relatively soft layer or stratum 30b of
compound 30 is formed over layer 30a. The splices lie in the
compound 30 so that when closure 110 is sealed about the splice
joint, the relatively soft layer 30b is easily redistributed about
the splices filling all interstices at the parting line of the
closure 110. A sheet of separator material 140 lies over layer 30b
and temporary separator blocks 142 or a separator frame can be
placed thereon for shipping and to allow slight overfilling of the
closure if desired. The separator is removed at installation.
The relative thicknesses of layers 30a and 30b depend upon such
factors as the size of the specific closure being utilized and the
number of splices to be placed therein and hence the quantity of
relatively soft flexible compound required to fill all interstices.
The maximum thickness of layer 30b is set by the mechanical
properties of the sheared material. The thickness of 30a simply
fills the rest of the cavity. When the thickness of the layer 30b
is near the maximum allowable thickness, the throat section of the
closure, such as designated 15 in FIG. 1, advantageously can be
filled with the relatively stiffer material comprising layer 30a in
order to help support the softer less viscous material in layer 30b
when the closure is stored on end, i.e., in an upright
position.
The formation of strata or layers in a compound having a uniform
composition throughout, but having different yield shear stresses
for the various strata, is accomplished by forming the strata by
different mechanical processes. For example, if the composition is
subjected to the previously described shearing pressures or forces
such as those encountered when the material is extruded through a
nozzle, the yield shear stress thereof is decreased because some of
the bonds creating the gelled condition are ruptured. This
phenomena is utilized in forming the strata, such as 30a and 30b.
For example, stratum or layer 30a comprises a layer of compound 30
which is hot-poured into the closure while the compound 30 is in a
liquid state. When layer 30a cools, it gels or solidifies to form
an extensive internal bonding network which results in a relatively
stiff strong layer. Layer 30b comprises a layer of compound 30
which is extruded through a nozzle at room temperature thereby
shearing and rupturing a portion of the bonds and resulting in a
relatively soft, that is, low yield shear stress layer which can be
easily forced into interstices. The shearing pressure applied to
the compound of layer 30b is determined by the nozzle size, rate of
extrusion, etc., and will depend upon such factors as the
composition being utilized and the relative degree of low yield
shear stress required in layer 30b.
FIG. 4 illustrates a further variety of spliced closure constructed
pursuant to this aspect of the invention. The closure denoted 60
consists of two halves 61, 62, advantageously joined by a common
hinge 63, and including extended edge portions 64 on each half
which abut when the closure is sealed. The edge portions 64 of the
closure 60 are provided with semicylindrical throat portions 75,
76, 77, 78 to accommodate incoming and outgoing cables 80, 81, 82,
and 83. The numerous splice mechanisms, denoted generally as 90 in
FIG. 4 are merely symbolic of the type of splice connector that can
be used in this closure. The splices 90 are shown as completed and
ready to be embedded and encased in the fill 30.
The spirit of the invention is embraced in the scope of the claims
to follow.
* * * * *