U.S. patent number 3,608,835 [Application Number 04/650,543] was granted by the patent office on 1971-09-28 for ultradisintegration and agglomeration of minerals such as mica, products therefrom and apparatus therefor.
Invention is credited to Josef Ruzicka.
United States Patent |
3,608,835 |
Ruzicka |
September 28, 1971 |
ULTRADISINTEGRATION AND AGGLOMERATION OF MINERALS SUCH AS MICA,
PRODUCTS THEREFROM AND APPARATUS THEREFOR
Abstract
Frangible or cleavable solids, such as mica, are disintegrated
in oriented, high-velocity streams of a fluid medium so as to
produce thin smooth-surfaced particles or flakes having a high
specific surface area and a high ratio of length to thickness. The
resulting particles or flakes are useful as agglomerants, fillers
or pigments or can be agglomerated to form paperlike webs or solid
discs or articles of other predetermined configurations, with or
without added binder, either in self-supporting form or adhered to
a substrate. Various methods and apparatus for such disintegration
and agglomeration are also disclosed.
Inventors: |
Ruzicka; Josef (Rego Park,
NY) |
Family
ID: |
27669889 |
Appl.
No.: |
04/650,543 |
Filed: |
June 30, 1967 |
Current U.S.
Class: |
241/4; 241/39;
241/5; 241/46.06; 241/24.1 |
Current CPC
Class: |
B02C
19/06 (20130101); B28D 1/322 (20130101) |
Current International
Class: |
B02C
19/06 (20060101); B28D 1/00 (20060101); B28D
1/32 (20060101); B02c 019/06 () |
Field of
Search: |
;241/4,46,46.02,46.04,46.06,46.13,79.1,97,266,38,20,27,5,39,24 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Kelly; Donald G.
Claims
I claim:
1. A process for ultradelaminating a crystalline laminar solid into
thin flakes which comprises:
a. forcing a fluid medium through apertures having narrow elongated
cross section in a bottom portion of a conversion zone, said
apertures being oriented substantially parallel to the height of
said zone, and thereby forming in said bottom portion a system of
whirling fluid streams having an orientation approximately parallel
to the apertures,
b. introducing relatively coarse pieces of said solid into said
conversion zone whereby said pieces become suspended in said
whirling streams and disintegrated principally in planes
corresponding to the principal two axes of the solid crystal
lattice,
c. circulating the resulting fluid suspension comprising comminuted
solid from said bottom portion upwardly in the peripheral portion
of said zone into an upper portion thereof,
d. settling insufficiently comminuted solid particles from said
upwardly circulating suspension back into said bottom portion for
further disintegration in said whirling streams,
e. removing solid particles of the required fineness from the upper
portion of said conversion zone.
2. Process for disintegrating mica into thin flat flakes which
comprises suspending relatively coarse pieces of mica in an
essentially inert liquid, in a proportion of 1 part of mica per 5
to 5,000 parts of liquid, in a bottom portion of an upwardly
expanding conversion zone having substantially the shape of a
truncated cone, propelling the mixture near the bottom of said
conversion zone in a centrifugal direction through constricted
substantially vertical channels having a varying width such that
the mixture becomes more constricted as it passes therethrough,
circulating the mixture upwardly along the periphery of the
conversion chamber such that mica particles having the desired
fineness rise to the top and overflow from said conversion zone to
be recovered while insufficiently fine particles settle downward
toward the central portion of the conversion zone for further
passage through said narrow channels for further
disintegration.
3. A process according to claim 2 wherein said channels have
alternating areas of larger and narrower width.
4. A process for ultradelaminating a crystalline laminar solid into
thin flakes which comprises:
a. forcing a liquid medium through apertures in a bottom portion of
a generally circular conversion zone, said apertures being normal
to the height of said zone whereby said liquid forced through said
apertures in said bottom portion forms a system of whirling streams
having an orientation approximating the circular path of said
conversion zone,
b. introducing relatively coarse pieces of said solid into said
system of whirling liquid streams and thereby disintegrating said
pieces principally in planes corresponding to the principal two
axes of the solid crystal lattice,
c. circulating the resulting liquid suspension comprising
comminuted solid from said bottom portion upwardly in the
peripheral portion of said zone into an upper portion thereof,
d. recirculating insufficiently comminuted solid particles from
said upwardly circulating suspension back into said bottom portion
for further disintegration in said whirling streams,
e. removing solid particles of the required fineness from said
conversion zone.
5. A process for disintegrating mica into thin flat flakes which
comprises feeding a suspension of insufficiently fine pieces of
mica in an essentially inert liquid to a bottom portion of an
upwardly extending conversion zone having a substantially circular
cross section, propelling the mixture near the bottom of said
conversion zone in a centrifugal direction through constricted
channels having substantially vertical walls and having a
resiliently varying width such that the mixture becomes more
constricted as it passes therethrough, circulating the mixture
upwardly in the conversion zone such that mica particles having the
desired fineness rise to the top and are recovered from said
conversion zone while insufficiently fine particles settle downward
toward the central portion of the conversion zone for further
passage through said narrow channels for further
disintegration.
6. A process according to claim 5 wherein said channels have
alternating areas of larger and narrower width.
7. A process according to claim 5 wherein said mica particles are
recovered from said conversion zone by electrostatic means.
8. A process according to claim 5 wherein said mica particles are
recovered by flotation.
9. An apparatus for disintegrating solids suspended in a liquid
medium comprising a vessel having a sidewall of generally circular
cross section and providing a disintegration chamber in the lower
portion thereof and an elutriation zone in the upper portion
thereof, disintegration means in said chamber comprising a
plurality of channel-forming members having substantially vertical
walls extending generally radially outward from the central area of
said chamber, said channel-forming members forming channels of
resiliently varying width generally narrowing from said central
area toward the periphery of said chamber and terminating short of
said periphery, means mounting said channel-forming members for
rotation in said chamber and means operatively connected therewith
for rotating said members, said vessel including means for
introducing solids in liquid medium into the central area of said
chamber and means of withdrawing product from said elutriating
zone.
10. An apparatus according to claim 9 wherein said vessel includes
baffle means above said channel-forming means and separating said
disintegration chamber and elutriation zone from one another.
11. An apparatus according to claim 10 wherein said baffle means
includes a wall surface adjacent and parallel to the sidewall of
said vessel for guiding disintegrated particles upwardly along the
periphery of said sidewall as the particles are circulated from
said chamber to said elutriating zone.
Description
SUMMARY OF INVENTION
This invention relates to the disintegration of frangible solids
into ultrafine particles and the reagglomeration of such particles
into desired products, to apparatus for carrying out such
operations, and to various products obtained thereby. More
particularly the invention relates to the oriented disintegration
of a mineral such as mica into a multiplicity of fluidly suspended
ultrathin particles or flakes and the production of new or improved
products such as mica paper therefrom.
This invention generally is concerned with the splitting of easily
splittable or cleavable materials to form fine particles, and
especially the cleavage of minerals such as mica into small, thin
flakes or scales which have active surfaces and which fall
predominantly within a relatively narrow size range. The resulting
products include mica particles characterized by an unusually high
ratio of surface to thickness.
The disintegrating or splitting equipment is intended primarily for
the splitting of mica but is also highly effective in splitting
other materials, especially minerals, which liberate molecularly
bound water or water of crystallization upon heating.
The aforementioned materials can be used in many different ways.
For instance, the free particles or unoriented, easily
redispersible agglomerates of such particles are useful as pigments
and fillers for paints or other coating compositions, for resinous
plastics, for elastomeric compositions; or as adsorbents or
carriers for other materials, etc. In the form of oriented
agglomerates they are useful as insulators or coatings in
electrical equipment, as construction materials, etc.
BACKGROUND OF INVENTION
Mica forms a group of silicates, which are minerals characterized
by their highly pronounced ability of being cleaved along their
basic crystalline plane while being substantially less susceptible
to cleavage along the crystalline plane which is substantially
perpendicular to the first plane, and being still less susceptible
to cleavage along any other plane. Consequently, this type of
mineral has crystalographically a platelike structure which is
highly flexible, resilient and strong and can be divided and
subdivided into very thin flakes or scales.
Mica as a mineral is found in nature in various crystalline sizes,
large sizes being quite rare, and in various chemical compositions
such as muscovite, phlogopite, biotite, etc. Because of its
excellent dielectric and mechanical properties, chemical stability
and resistance to high temperature, mica is used for various
industrial purposes, the highest grades of mica being used
principally in the electrical industry as an insulating material.
Its properties and usefulness, however, differ substantially not
only depending on its basic type but even in a given type the
properties depend on the exact chemical composition. The chemical
composition of natural mica differs substantially, sometimes even
within a single crystal. Yet the exact chemical composition
determines the thermal resistance of individual mica crystals and
when the critical dehydration temperature of a given piece of mica
is exceeded, usually above 500.degree. C., the mica becomes
dehydrated and swells up and disintegrates depending on temperature
and duration of heating. Synthetic mica has similar characteristics
and properties.
PRIOR ART
Natural and synthetic mica crystals are relatively small while
modern industrial requirements point increasingly toward large
surfaces. For this reason the efforts in the art have increasingly
been toward splitting mica into flakes of ever smaller thickness
and reintegrating these thin flakes with or without the aid of
binders into coherent sheets or leaves of large surface area.
However, prior methods for making products of large surface area
from mica particles having a thickness on the order of a few
hundredths of a millimeter, e.g., 0.010 to 0.030 mm., have proved
to be very laborious, the utilization of the mica is relatively low
and the resulting products are quite nonuniform as well as
expensive. Moreover, they lack adhesive surface forces.
Methods of making sheets of large surface area from mica particles
having a thickness on the order of less than 0.01 mm. e.g., about
0.002 to 0.008 mm. have been known for more than 50 years. However,
poor physical and especially mechanical properties of the resulting
products have prevented them from becoming commercially important.
More recent methods such as those described by Heyman in U.S. Pat.
No. 2,405,576 or by Bardet in U.S. Pat. No. 2,549,880 have achieved
a certain degree of commercial significance particularly because
the mechanical properties of the resulting products are better than
those of earlier products. However, though these processes are now
more than 20 years old they have never achieved wide use. They have
only partially succeeded in replacing the older methods which
resulted in particles having a thickness greater than 0.01 mm.,
because their physical and especially their mechanical and
dielectric properties still leave much to be desired, their
processing is difficult, the utilization of the mica raw material
is incomplete, and the operating costs are high.
Even when mica particles are to be used as pigments or fillers the
trend in the art is to require particles of ever smaller thickness,
that is, particles having the greatest possible surface area per
unit weight. However, in requiring this there is also often the
further requirement that the particles should not exceed a
specified maximum dimension and should fall within a rather narrow
particle size range. On the other hand, especially in the case of
particles having a small diameter, such as 1 micron or less, the
art has heretofore been unable to obtain high yields of particles
falling within a predetermined narrow size range. The previously
known mica particles at best had only very weak adhesive surface
forces.
OBJECTS
It is accordingly an object of this invention to prepare fine solid
particles such as mica flakes having a high specific surface area
and other new or improved properties which make such particles
particularly valuable as agglomerants or pigments and also in the
production of aggregated products. Another object is to prepare
improved products by agglomeration of fine particles.
A still further object is to provide new or improved methods and
apparatus for oriented cleavage of mica principally along its main
plane of crystallization and secondly along one further plane of
crystallization while limiting the cleavage or splitting along any
other planes, so as to facilitate the production of particles or
flakes having a large specific surface area and a geometrically
elongated configuration with predominantly submicron thickness, on
the order of a few tenths or even thousandths of one micron or
less, permitting the segregation of flakes having specified
geometric dimensions, wherein the invention permits recycling of
insufficiently disintegrated mica pieces to be split further until
particles or flakes having the specified dimensions are
produced.
A further object is to provide methods and apparatus for preparing
and maintaining a fluid suspension of the fine mica flakes, to be
subsequently converted either into an agglomerate or into free
flowing particles to be used as a pigment or the like.
A still further and particular object is to provide apparatus and
methods for producing improved mica paper or other structures
either solely from the fine mica flakes or from a mixture of such
flakes with other conventionally used auxiliary materials such as
binders, fillers and so forth, particularly mica papers less than
20 microns thick.
THE DRAWINGS
In the drawings
FIG. 1 is a diagram of a process beginning with the preparation of
raw material feed and leading through a splitting step and
production of a fluid particle suspension to a final product
molding step, with or without a separate intervening agglomeration
step.
FIG. 2 illustrates the amount of water which is lost from a typical
sample of mica by heating it to progressively higher temperatures
until a constant anhydrous weight is reached.
FIG. 3 shows the volume increase of mica in relation to the time
employed in heating it from 18.degree. C. to 885.degree. C., i.e.,
the effect of rate of heating on the degree of swelling
achieved.
FIG. 4 is a diagram showing the relationship between the tensile
strength (and also dielectric strength) and the thickness of mica
after it has been bent between two complementary surfaces having a
Z-shaped profile under a load of 10 kg./cm..sup.2.
FIG. 5 is a representation in vertical section of the Z-shaped
device used for bending the mica as referred to in FIG. 4.
FIGS. 6A, 6B and 6C are three views showing a piece of mica being
split along its "x" and "y" axes into thin flakes or plates by the
simultaneous action of heat and a high velocity stream of a fluid
medium.
FIG. 7 is a microscopic illustration of a group of typical mica
particles obtained according to a process such as that of Bardet,
showing both the irregular shape and wide range of prevailing
particle sizes.
FIG. 8 is a greatly enlarged view showing one of the typical
particles from FIG. 7 in vertical section.
FIG. 9 is a microscopic illustration of a group of typical mica
particles made according to the present invention, showing their
predominantly rectangular shape and relatively narrow size
range.
FIG. 9A is a microscopic illustration of a group of mica particles
of ultrafine size useful, for instance, in making pigments or
fillers.
FIG. 10 is a greatly enlarged view in vertical section of a typical
particle or flake of this invention, showing its essential flat
surface free of irregularities.
FIG. 11 is a view in vertical section showing a deposit of
relatively thick, inflexible mica particles of the prior art on a
solid substrate, with cavities between some of the adjacent
particles as well as between the particles and the substrate.
FIG. 12 is a view in vertical section showing a dense deposit of
the thin, flat, flexible particles of this invention on and closely
conforming to the surface of a solid substrate comparable to that
shown in FIG. 11.
FIG. 13 is a view in vertical section of one embodiment of the
apparatus for disintegrating materials such as mica in accordance
with the present invention, preferred for use with a liquid
suspension medium.
FIG. 14 is a plan view of the apparatus shown in FIG. 13, taken
along line 14--14.
FIG. 15 is a partial view in vertical section of a variation of the
apparatus shown in FIG. 13, wherein product particles are removed
from the disintegration chamber via a wide spout by electrostatic
means, liquid overflow is absent or very small, and the particles
are classified into different fractions according to size.
FIG. 16 is a partial view in vertical section of still another
variation of the apparatus shown in FIG. 13, wherein product
particles are removed from the disintegration chamber by
electrophoresis employing a moving belt which serves as an
electrode to which the product particles adhere and from which they
are removed by scraping.
PIGMENTS, FILLERS AND ACTIVE AGGLOMERANTS
The term "pigment" refers here to finely divided solids intended
for addition to paints, other liquid coating compositions, glazes
and the like while the term "filler" refers to finely divided
solids intended for addition to molding resins, powders, pastes,
elastomeric mixtures, graphite compositions, insulating
compositions, papers as well as layers of free flowing solids such
as layers intended for use as thermal or acoustic insulators. The
term "agglomerant" refers here to fine mica particles with active
surfaces or adsorptive capacities which make them suitable as
carriers for active substances such as insecticides or herbicides,
or as components of filtration media, or as carriers for pigments
or other colorants or for materials such as silver or titanium
dioxide powder or the like to make semiconductive products
therefrom. From FIGS. 9 and 10 it is apparent that mica particles
of this invention have the required geometric configuration, that
is, small thickness and a relatively large and flat surface, narrow
particle size range and large specific surface area. Depending on
requirements, the new flakes have a very much higher specific
surface area than similar products made previously, i.e., a surface
area in excess of 7 m..sup.2 /g., e.g., from above 7 to 700 or even
2,500 m..sup.2 /g. with certain kinds of mica. The maximum
dimension of the new thin mica flakes or particles can be
predetermined in accordance with requirements and depending on the
desired specific surface area may be of the order of 1 or more
millimeters, tenths or hundreds of a millimeter and for special
purposes may be of the order of 1 or more microns, tenths, hundreds
or even thousands of microns, especially in preselected narrow size
ranges falling within the overall range between 30 millimeters down
to 2 millimicrons. For instance, the product illustrated in FIGS. 9
and 10 desirably will consist predominantly of particles having a
high ratio of length to thickness, of the order of from 1,000/1 to
as much as 5 million/1.
Pigments, fillers and agglomerants made in accordance with this
invention make possible new applications and new methods of
utilization which were not previously possible, because the
characteristics of the new particles are of a fundamentally new
kind in the physical sense such that, for instance, the finely
divided particles when dispersed in an appropriate fluid behave
like colloids, have a surprising ability to adsorb particles of
other materials on their surfaces, conform tightly to substrates of
various configurations without breaking, etc.
PROCESS OF INVENTION
Step A - Preparation of Raw Material
All available forms of mica, natural or synthetic, may be used in
the present invention. The raw mica is cleaned in any conventional
manner to remove organic matter, dirt and foreign mineral,
preferably to obtain a feed of at least 90 percent purity. One of
the important advantages of the present invention is that it
permits simultaneous processing of mixtures of mica crystals
differing from each other in chemical composition and having a wide
particle size range, i.e., mixtures of large and small pieces.
Step B - Cleavage or Delamination
The method of effecting selectively oriented cleavage of mica in
accordance with the present invention is illustrated in FIGS. 6A,
6B and 6C. Sudden local temperature effects are indicated by arrows
c in FIG. 6B while the effects of the high velocity and high
frequency fluid stream are indicated by arrows a and b in FIGS. 6B
and 6C, and these bring about perfect cleavage of the mica
predominantly in two directions, i.e., primarily along the plane of
lowest cohesion (the basic plane) and further along the plane
having the next lowest cohesion which substantially is
perpendicular to the first plane. The effects in other directions
are not greatly developed and are suppressed by the elasticity of
the mica and are therefore so weak that predominantly they do not
reach values necessary for disrupting the mechanical cohesion of
the mica in any further, less easily splittable directions.
According to this method the continually fed pieces of mica (FIG.
6A) are exposed to the necessary mechanical, delamination forces,
or combination of mechanical and thermal forces, in one or more
splitting chambers which are arranged in series or in parallel. The
forces, at temperatures between as low as about 100.degree. C. and
up to about 1,350.degree. C., act on the large pieces of feed
material for periods which depending on individual particle size
may range from a fraction of a second to a few minutes within a
fluid, and preferably inert, medium. The forces cause splitting of
the mica predominantly in the direction of two planes, by the
pulsating, vibrating and accelerating or decelerating streams of
the medium which whirl in a distinctly oriented manner and which
cause delamination predominantly progressively from the surface of
the mica inward as indicated in FIGS. 6B and 6C until the original
pieces are delaminated to the desired extent. For some kinds of
mica and some kinds of end use the method may be performed in a
single chamber whereas in other cases the splitting may be effected
in a plurality of like or different splitters, e.g., first at
ambient temperature in a liquid medium and then at elevated
temperature in a gaseous medium. This method may of course be
modified in that, for instance, the pieces of mica being fed to the
splitter may be preheated or thermally pretreated prior to
introduction into the splitter chamber, preferably in an inert or
protective fluid such as argon or hydrogen.
The resulting flaked or disintegrated products having active
surfaces (i.e., an adsorptive surface), which they obtain by virtue
of their predetermined geometric dimensions, are immediately and
continuously separated and transferred to the next step. In some
cases one may add binders or other additives such as organic or
inorganic fibers, platelets and the like in order to distribute
them uniformly in the eventual product.
In making pigments, fillers and agglomerants of the kind
illustrated in FIG. 9A, rather than the predominantly
two-dimensional flakes illustrated in FIGS. 9 and 10, it is
necessary to split the mica as much as possible not only along the
first and the second splitting or fissioning planes in order to
obtain the greatest possible specific surface area, but also to
further split the mica to form an ultrafine particle size.
The ultimate size may be specified in terms of the maximum
permissible dimension or diameter or better in terms of the
permissible particle size range, e.g., 10 to 30 microns, or 0.1 to
1 micron, etc. Consequently, the splitting method is oriented for
splitting according to all planes of fission and for producing the
smallest particle size possible it can utilize further effects of
the high velocity of the splitting medium, 100 meters per second or
more, and high frequency waves (20 kilocycles per second or more)
and the acceleration and deceleration of the particles and the
consequent cavitations. The method can be still more effective when
the splitting medium enters into the reaction chamber
intermittently and thus produces pulsations. The apparatus
illustrated in FIGS. 13 to 19 are equipped with devices for the
production of the aforementioned effects, such that pigments,
fillers or agglomerants of various sizes and ratios of length or
particle size to thickness may be produced by adjustment of the
appropriate variable or variables, e.g., by increasing the velocity
of the fluid medium, by increasing the number of operating jets,
etc.
Step C - Preparation of Fluid Suspension
The mica particles having active surfaces are kept in or conducted
to and maintained in a fluid suspension in the previously present
or in a different protective medium. Various combinations of
gaseous or fluid media are possible depending principally on the
requirements of subsequent utilization. It is possible to make
intermediate products in a continuous manner and to concentrate the
suspension and only adjust the consistency or concentration of the
suspension prior to the next processing step and depending on the
requirements of the latter. The maintenance of these particles as a
suspension is advantageously effected with the stream of the
aforesaid medium, and only by mechanical means, but in some cases
it may be useful to employ additionally the effect of an electrical
field.
The suspension of particles of the proper concentration can then be
continuously or intermittently added to an appropriate
agglomerating step or it can be added directly to some other
finishing step.
Product I - Fillers, Pigments and agglomerants,
Fillers, pigments and agglomerants, i.e., mica particles which can
be added to coating compositions, electrical putty, synthetic
resins, rubber compositions, etc. can have two different forms,
that is, either as a loose conglomerate of various shapes such as a
block from which a desired amount of pigment can be easily broken
off for use, or as a free flowing pulverulent mass. An agglomerant
made as outlined above in Step C can be a final product as such. If
it was made from a gaseous suspension it does not require any
finishing operation or it may be classified into fractions of
different size in the dry state in any otherwise known manner. If
it was made from a liquid suspension, finishing operations can
comprise concentration or compacting and drying, or if necessary,
the particles can be classified while wet prior to compacting in
any otherwise known manner. The production of particles in a free
flowing state from a gaseous suspension requires essentially only
contacting them with the ordinary atmosphere while being
circulated, whereby the adhesive surface properties are destroyed,
whereas in the case of a liquid suspension a drying step will
usually be required.
APPARATUS
Splitter
Referring to FIGS. 13 and 14, the apparatus is an axially
symmetrical splitting chamber in the shape of an inverted truncated
cone 50 of circular cross section. However, chambers of other
axially symmetrical configurations, e.g., chambers having a
horizontal cross section which is quadrangular, octagonal, etc. or
which has parallel rather than diverging sidewalls are also usable.
Incompletely split pieces of mica are recirculated back into the
splitting zone in the direction of the main vertical axis. This
device is particularly intended for splitting mica in a liquid
medium such as water or ethyl alcohol though it is possible to
operate it with a gaseous medium. It can be operated either at
ambient temperature, or the operating temperature may be lowered
below the freezing point of water if a suitable nonaqueous fluid
medium is used or it can be increased, e.g., above the temperature
at which mica splits out bound water.
Vessel 50 is provided with a cover 51 which in its central portion
contains a funnel 52 for feeding the pieces of mica which are to be
split. Tubular element 53, which preferably has the shape of a
flared cylinder or cone, is spaced from orienting element 54 which
is attached to and spaced from the sidewall of vessel 50. A
rotating assembly of hinged splitting elements or paddles 55 is
spaced above a rotatable supporting plate 56. The paddles 55 are
hingedly and movably supported on pivots 57 which are attached to
plate 56. The entire splitting assembly is rotated by motor 58.
Vertically arranged baffles or ribs 59 are arranged in the upper
part of chamber 50 and are attached both to the outer wall of
chamber 50 and to tubular element 53. Sonic or ultrasonic vibrators
60 are attached in the outer wall of chamber 50 facing the
orienting element 54. At the bottom of vessel 50 is a drain 61 with
valve 62 which may be used for periodic cleaning of the vessel or
otherwise as needed.
In the upper part of chamber 50 there is a collector and overflow
spout for the finished product. In the bottom circumference of
vessel 50, facing the exterior faces of revolving elements 55,
there is arranged a directional element or ring 64. The pivoted
members 55 are easily removable such that they may be replaced with
members of different configurations, and the total number of the
members can also be varied. The shape and quality of the working
vertical surfaces 65 and 66 are such that they form a resilient
system of channels of outwardly narrowing horizontal cross section.
When rotating the members form a system of essentially vertically
oriented planar streams of the splitting medium flowing radially
outward between adjacent members. It is possible to regulate the
mutual relationship of the lower portion of the walls of filler
tube 53, the directional element 54 and the working surfaces of
members 55 by displacing these elements relative to each other and
thereby vary the flow pattern in the unit. Individual parts of the
equipment are made from appropriate structural materials such as
stainless steel or other metal, synthetic resins, etc. The unit may
be virtually of any size. For instance, it is possible to build
small laboratory type units with splitter chambers having a bottom
diameter of about 35 cm. or less and a height of, for instance, 50
cm.; or large commercial units with splitter chambers having a
bottom diameter as large as 1 or 2 meters or more and a height of 3
to 10 meters or more.
In operation, cleaned chips or pieces of mica of whatever kind and
thickness and size are continuously fed into funnel 52. The
required amount of liquid, for instance 500 parts by weight per
part of mica feed, is also preferably added through funnel 52. The
mica feed and cleavage medium are then aspirated by the rotating
effect of elements 55, partially from supply tube 53 and partially
from the space between the inner wall of directional element 54 and
the lower portion of supply tube 53 where insufficiently
disintegrated particles are recirculated into the splitting zone
until they are comminuted to the desired size.
The intensity of the cleavage action can be controlled by the speed
of rotation of the rotor assembly 56, the width and configuration
of the channels formed between adjacent elements 55 and between the
outer faces of these elements and the outer ring 64, by the
viscosity of the splitting medium, etc. For instance, the assembly
carried on plate 56 may rotate at about 20 to 500 r.p.m. or more
and the contracting width of the channels between individual
elements 55 may range from as much as 50 mm. near the center of the
vessel to 1 mm. or less near the periphery. It will be understood
of course that the width of individual channels varies in operation
and that the narrower the exit of the channel the more effective
will be its splitting action as the vertically oriented mica
particles are carried therethrough in the circulating fluid.
This apparatus has the important advantage that as the mica raw
material is sucked in between the splitting elements 55 it becomes
oriented in accordance with the principal surface of each piece of
feed, essentially parallel to the direction of the fluid flow
through the aforementioned channels and the laminar surfaces of the
resulting fluid streams. Essentially the pieces retain this
orientation throughout the entire splitting process both between
the elements 55 and after tangential discharge from the channels
and passage along directional ring 64, and up into the upper part
of the vessel, and even when vibrators 60 are operating. This
orientation prevails both in the case of freshly added pieces of
mica and in the case of pieces which are recirculated.
The splitting elements 55 form in the course of a process a
resilient assembly with highly effective working surfaces which are
self-cleaning and therefore cannot become obstructed and which can
be easily regulated and simply increased by increasing the diameter
and/or height of the elements, by increasing their surface (as
shown at 65a and 66a) and by increasing their total number.
The total effective working surface can also be increased by
increasing the surface of the directional elements 54 and 64. The
effectiveness of the cleavage operation may be further increased by
placing vibrators 60 in operation.
The cleavage effects are based principally on the effect of the
high velocity laminar plane streams of the fluid medium acting
essentially parallel to the major surfaces of the oriented mica
particles. The velocity of the stream in this process increased in
the centrifugal direction while the thickness of the channels and
hence the laminar fluid streams flowing therethrough decrease in
the radially outward direction. Being resilient, individual
channels become narrower or wider during operation depending on the
thickness of the pieces of mica passing through them.
A shape of the splitting elements such as that illustrated at 65a
and 66a additionally provides a sort of delaying chambers and
increases the number of the narrowest channels or passages through
which the mica is dragged in the process. This produces a pulsating
flow and further enhances the cleavage action.
The velocity of the fluid stream changes according to channel cross
section and is therefore usually lowest in the central part of the
vessel and conversely highest in the peripheral portions. Mica is
thus split by the effects of a fast laminar stream of fluid and the
changes in its velocity, i.e., its acceleration and decelerating,
by the rapid increase in velocity of the fluid stream in the
radially outward direction, the resulting cavitation and vibration
or pulsation along sinusoidal faces 65a and 66a, the slowing down
along the effective surface, etc. When these effects are
insufficient to achieve the desired degree of comminution in any
particular case the cleavage action may be further intensified by
the use of devices 60 which may produce sonic or even ultrasonic
vibrations, etc., vibrations in the range from about 10 kc./sec. up
to about 1 mc./sec.
The split particles having the desired dimensions are continuously
sorted out from the process as soon as they reach the desired size,
being floated up and removed in the overflow of the liquid through
spout 63 and then transferred to whatever further operation may be
desired. The principal variable by which circulation and
recirculation of the particles within the splitting chamber is
controlled, is the speed of rotation of the revolving assembly in
the bottom, but rate of circulation of liquid through the unit can
also be adjusted to cause the desired range of particle sizes to be
floated out of the unit.
Instead of removing the comminuted particles in an overflowing
stream of the liquid medium as shown in FIG. 13, it is possible to
remove them without virtually any liquid by using an arrangement as
shown in FIGS. 15 or 16. As shown in FIG. 15, the liquid medium is
maintained in the splitting chamber 50 with no or virtually no
liquid addition or overflow while two-spaced electrodes are
arranged at the overflow spout 63 such that the particles of mica
product become charged near the liquid surface in the splitting
chamber and then jump out from the liquid by being attracted to the
other electrode whence they are finally removed. An inert gas such
as argon or neon may be maintained in such a system to avoid any
degradation of the product particles by contact with air or oxygen.
By arranging a series of collecting bins beneath the two-spaced
electrodes, the mica particles being ejected from the splitter can
simultaneously be classified into several fractions according to
their weight, the heaviest particles dropping out first and the
progressively finer ones dropping down at more distant points from
the spout.
In an alternative arrangement, illustrated in FIG. 16, a moving
belt may be arranged in the upper portion of the splitter and an
electric field set up such that the product particles become
charged near the top of the liquid medium in chamber 50 and then
are carried by electrophoresis to the oppositely charged moving
belt to which they remain attached until they are scraped off and
recovered. Example 1
A mixture containing about equal proportions of clean pieces of
muscovite and phlogopite about 3 to 100 mm. in diameter is
introduced into the funnel 52 of the apparatus in FIG. 13. 800
parts of clean water per part of mica is simultaneously introduced
and the mixture of mica particles and water is aspired between the
jaws of the rotary elements at the bottom of the splitter and the
mica is thus split into small particles in accordance with its
laminar structure by the action of the water stream and the
auxiliary high frequency means 60 vibrating at 100 kc./sec. The
rotor revolves at 100 r.p.m. When a particle reaches a specific
surface area of 5 m..sup.2 /g. it is immediately sorted out from
the process by floating up in the water whereas coarser particles
settle out from the water stream and return downwardly toward the
rotating elements for further disintegration.
The resulting suspension of mica flakes of proper size overflows
into a storage vessel (not shown in FIG. 13) and then, after
adjustment of proper solids concentration, into the chamber of a
paper making machine.
The new mica products described herein are substantially better in
terms of their mechanical, electrical and other physical
properties, than similar mica products heretofore available,
generally several times better, such that in effect new classes of
mica products having new types of utility are now made available.
The advantages are particularly apparent in fabricated products
made from the new basic material, i.e., the ultrafine mica flakes.
For instance, because of the extremely small thickness of the new
mica flakes, it now becomes possible to make self-supporting
coherent mica webs, coatings and laminates only a few microns
thick.
The key pieces of equipment designed in accordance with this
invention have large capacity and relatively small dimensions, such
that as much as ten times more production can be obtained from a
given plant area than heretofore. Moreover, the disintegration or
cleavage technique of this invention is unusually advantageous in
that it permits the simultaneous utilization of different kinds of
mica such as muscovite and phlogopite, it also permits the use of a
mica feed containing a wide range of particle sizes, and in all of
this it makes possible essentially 100 percent conversion of the
feed material into desired products.
The methods and apparatus of the invention further make it possible
to make combination products from mica and various other materials
such as glass fibers or platelets, fibers of asbestos, silica,
cellulose or synthetic fiber forming resins, glass cloth, binders,
foils of synthetic resins or metals, etc. Because of their high
surface area, the novel mica particles themselves offer unusual
advantages as pigments, fillers and also as carriers for other
pigments and for physiologically active substances and catalytic
substances. Because of the extremely small thickness, coatings or
compositions made from these new mica particles have far superior
barrier effects, novel decorative effects, etc.
As compared with similar products known previously, the
ultradelaminated flakes made in accordance with this invention are
such that they fall into a quite different and new physical field
and are therefore governed by different physical laws than the
earlier products. One of the predominant characteristics of the new
particles is that they behave like colloids in a suitable liquid
medium. Their sedimentation times are extremely long, such that
they can be used in processes where the coarser, previously
available particles were useless or gave poor results.
In addition to the aforementioned product properties, important
advantages are obtained in that certain features of the present
invention permit a very high degree of flexibility of the process,
permitting the economical use of different types of splitters in
parallel or in series depending on types of products required, and
high production capacity per unit area.
It should be understood that the foregoing general description and
specific examples have been given primarily for purposes of
illustration and that numerous variations and modifications thereof
are possible without departing from the scope or spirit of the
disclosed invention. It should also be understood that, in the
absence of indications to the contrary, all percentages and
proportions of materials are expressed in this disclosure on a
weight basis.
The scope of the invention is particularly pointed out in the
appended claims.
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