Europaisches Patentamt

3
European Patent Office tt) Publication number: 0 079 5 9 6
Office europeen des brevets B1

EUROPEAN PATENT SPECIFICATION

(45) Date of publication of patent specification : 17.02.88 Intel.4: B 29 B 1 5 / 0 2

Application number: 82110467.6

Date of filing: 12.11.82

(54) Pneumatic polymer eductor conveyor dryer.

() Priority: 12.11.81 US 320820 @ Proprietor: LABOFINA S.A.

52, rue de I'lndustrie
B-1040Bruxelles(BE)
(43) Date of publication of application:
25.05.83 Bulletin 83/21
Inventor: Terhune, Robert David
105Pfeiffer
(45) Publication of the grant of the patent: Borger Texas 79007 (US)
17.02.88 Bulletin 88/07 Inventor: Bazin II, George Leo
327 S. E. Boston
Bartlesville Oklahoma 74003 (US)
(84) Designated Contracting States: Inventor: Long, James Henry
AT BE CH DE FR GB IT LI LU NL SE 222 Inverness
Borger Texas 79007 (US)
Inventor: Nguyen, Linh Van
(58) References cited: 2527 Planters Row
DE-B-1 232 340 Sugarland Texas 77478 (US)
DE-B-1 273 804
DE-B-2 028 742
US-A-1 869 703 (74) Representative: Altenburg, Udo, Dipl.-Phys.
0Q US-A-3 370 358 etal
Patent- und Rechtsanwalte Bardehle-
CO Pagenberg-Dost-Altenburg & Partner Postfach
O) 86 06 20
If) D-8000 Munchen 86 (DE)

o
o Note: Within nine months from the publication of the mention of the grant of the European patent, any person may
give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall
Q. be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been
LU paid. (Art. 99(1) European patent convention).
Courier Press, Leamington Spa, England.
 0 079 596
Description
The invention relates to the drying of polymeric materials. In one aspect, the invention pertains to an
apparatus effective for drying water-moist polymeric particles.
5 USA3 370 358 describes a process and apparatus for working up rubber in which partially
dehydrated material is fed from a screw extruder into a first air stream guided by a cooled medium to
further dehydrate the material. DE B12 32 340 describes an apparatus for post-drying of rubber crumbs.
In this apparatus an extruder extrudes rubber via a die plate through a ring nozzle surrounding the die
plate. The DEB 12 73 804 finally describes an apparatus for post-drying rubber crumbs which is similar
w to the apparatus mentioned. In this apparatus, too, a gas stream is coaxially introduced through a ring
nozzle surrounding the extruder die plate the air in this reference is referred to as the transport air.
In the production of rubbery materials by polymerization of one or more polymerizable monomers in a
non-aqueous solvent with organometal initiators, the resulting product is obtained as a solution or
suspension of rubber in the non-aqueous solvent, usually a rubber-in-hydrocarbon solvent solution termed
is a cement. Subsequently, the polymeric material must be recovered (separated) from the non-aqueous
solvent. For this purpose, treatment of the cement with water has been convenient, usually by steam- -
stripping which has been most widely used on a commercial basis. Steam-stripping, usually assisted by k
one or more crumb-forming additives, removes the nonaqueous solvent or solvents and leaves a
polymeric product in the form of a crumb as a slurry in water.
20 A similar net effect is involved in emulsion polymerizations, in that the product is a finely divided slurry
of polymeric product in water.
Much of the water can be removed by filtration, pressing, or the like.
The product at this stage contains considerable percentages of water. If derived from a non-aqueous
solvent polymerization system, a few percent of volatile and off times potentially flammable solvent still
25 may remain associated with the polymeric/rubbery particles.
Various methods have been utilized in efforts to remove the final few percent of water, and, where
present, the final few percent of remaining non-aqueous solvent.
One of the most common commercial methods employed is the so-called expansion process. In this
process, the moist material is compressed in an extruder, such as a worm extruder which heats the
30 material by the work and friction, optionally with a supplementary supply of heat if desired, and is extruded
through nozzles of relatively small diameter. The reduction in pressure which occurs on the discharge side
of the die plate assists in evaporation of the moisture/solvent present.
Unfortunately, the normal collection method on the discharge side of the die plate has been to
discharge the particles or strands into a relatively large receiving chamber or "hot box" which usually has a
35 conveyor to remove the dry material. While various configurations have been tried, none have been
particularly effective. The reason for this is that as the rubber or polymeric particles, crumbs, or strands, are
sprayed out, impinging on the top and sides of the hot box, a buildup of polymer occurs on the surfaces of
the chamber or hot box, usually on the upper portions of the sides and on the top of the hot box or .
expansion chamber. Being cooler, these surfaces, tend also to accumulate various proportions of moisture.
40 The build-up of material lags in the chamber and tends to "age", resulting in degradative effects, or
formation of gel from age, heat, and moisture. Periodically, various chunks of such materials fall back into
the box and become associated with the fresh rubber or polymeric particles. These chunks of material,
more or less moist, and of differing physical properties from the fresh product, may fall down onto the
conveyor in the bottom of the 'hot box", and ultimately be included in the pressed bales of products. As
45 much as 5 to 10 percent by weight of the bale may be such undesirable product. This frequently requires
either physical separation, or product rejection, resulting in increased costs to produce products without
said undesirables in it.
Further, the accumulation on the surfaces of the "hot box" require periodic shutdown of the entire
production train, and frequent manual cleaning. This in itself not only is a chore, but results in "track-in" of
so undesirable materials, grit, sand, and the like, from the outside of the consequence of the cleaning
operation, and further contamination of the ultimate baled product.
Another problem has been with spontaneous fires due to flaming of the hydrocarbon solvent traces,
Cesulting in overheating and fire hazards.
In spite of many difficulties, expansion drying has had advantages over other methods of drying,
55 primarily being low cost of plant and operating costs. Nevertheless, distinct improvements are and have
been needed.
The above indicated problems are solved in accordance with this invention by a process and an
apparatus as defined in the claims.
In our pneumatic polymer eductor conveyor dryer, a water-wet polymer from a product recovery
60 operation is extruded through a die plate. Free water removed by the extruding action of the die plate is
atomized and/or evaporated into a flowing air stream. The flow rate is controlled to preferably avoid
explosive expulsion. The die plate assembly discharges the rubber/moisture into a receiver which is a
closely adjacent funnel receiver spaced away from but openly surrounding the die plate, and connecting to
and discharging into a lesser diameter conveying tube. The latter in turn can dump into a conventional hot
65 box, or preferably conveying to a cyclone accumulator. The die plate and surrounding funnel are totally

2
 0 079 596
enclosed by a chamber, so that air, which can be heated and/or cooled and/or humidified or dehumidified
as needed, is input thereto tangentially. The tangential input of the airflow is preferably behind the funnel
receiver, away from the die plate, toward the rear of the enclosure. The tangentially input resulting airflow
creates a vortex action at the die plate, and provides a relatively high velocity flow in the narrow spacing
5 between the edge of the plate and the closely adjacent edge of the receiver funnel, thus assisting in a
pulling and stripping action of rubber particles from the die plate, effectively a swirling shearing action,
maintaining a clean die plate, and in turn conveying the dry rubbery particles into the conveying tube and
through the conveying tube into the recovery unit.
The net result is effective recovery, virtually no degradation of rubber; no accumulation of product on
w the die plate or in the cone or conveying tube; a dry product; and no fire hazards. By our invention, the old
"hot box" can still be used but is much improved, substantially being eliminated from accumulation of
rubber mats or pads on the surfaces and ceiling thereof. Alternatively, and preferably, our inventive
receiver apparatus permits elimination of the hot box, and recovery of the well-dried product in a cyclone.

15 Brief Description of the Drawings

Figure 1 shows the basic heart of our invention by a longitudinal section view through the enclosed
receiver. The die plate 1 receives wet rubber from an extruder (not shown) and extrudes the wet rubber
through various orifices 2 of the die plate 1. These orifices discharge the rubber particles into a funnel
receiver 3 which is spaced away from the discharge end of the die plate 4 (exterior end of the orifices), but
20 openly surrounds them 5. The funnel 3 collects the particles by means of an air flow, and the particles then
are conveyed on down the conveying tube 6. It is seen that the orifice discharge and funnel are completely
enclosed by a box 7 so as to make a closed chamber, closed except for die holes 4, the discharge 8 for the
air/rubber particles, and of course for the air inlet 9. The air inlet 9 is shown 11, entering in a tangential
fashion into the surrounding chamber 7, which creates then a swirling or shearing vortex action at the die
25 plate face 12, as the air pours in around and through the funnel receiver 3, tearing the rubber particles and
conveying them at the same time through the receiver and down through the conveying tube.
Figure 2 shows our novel chamber coupled with a hot box. The same indicator numbers as in Fig. 1 are
employed for similar components. Shown in Figure 2 is an option that can be employed in any of the
configurations on our apparatus: The extruder 21 brings rubber to the die plate 1. The die plate 1 extrudes
30 rubber through orifices 2, 4 into the funnel collector 3, shown with our complete enclosure 7, air input 9.
Rubber particles in the air stream discharging in this configuration into the hot box fall onto the conveyor
23 for ultimate removal 26 and recovery such as baling (not shown). Shown is an option 27 by which an
additive, such as a talcum powder, can be fed by an aspirator arrangement 28, and admixed with forced air
29, for flow into the air inlet 9. Optionally, a portion of the primary air 31 provided by air pump 36 can be
35 heated 32, or cooled 33, or both together, with a tempering device 34, or humidified.
Figure 3 shows essentials as described with Figure 1, except conveying 8 the dry rubber particles by
means of the air stream into a receiving cyclone 41 which accumulates the dried rubber in the bottom
hopper 42 for removal 43, and the air then is discharged 44 and removed 45, optionally with auxiliary
exhaust blower 46.
40 Figure 4 shows a typical die plate itself. Orifices 2, 4 can be of variable diameter and configuration,
need not be of the reduced diameter shown, can be a nozzle or cone configuration as may be desired.
Figure 5 shows an overall arrangement including a hopper feed 51 , an extruder 52 discharging into the
apparatus of our invention, supplied with air, optionally heated 32, as described above. Here the process
sequence conveys the dried rubber to the described cyclone 41. The cyclone 41 accumulates the dried
45 particles 42 which are then discharged periodically 43 into a bale hopper 53, box, or other packaging
device.
In Figure 6 an alternate, but presently preferred sequence, is shown. Interveningly, an intervening first
cyclone 61 is employed to collect the rubber particles, which are then removed periodically or continuously
62 and reground 63, and conveyed 64 by air flow into the collector cyclone 41, which accumulates the
so rubber particles 42 for periodic discharge 43 to a bale hopper 53 or packaging device. This method provides
more uniform control of particle size.
Detailed Description of the Invention
Rubber/water admixtures received from such as an emulsion polymerization process, or steam
55 stripping of a non-aqueous polymerization process, may contain varying quantities of water. Usually, the
water content is mechanically reduced by squeezing, filtration, pressing, and the like, to such as between 6
and 15 weight percent. The remaining water then is evaporated in an expansion process.
In the expansion process, the moist material is raised to a pressure of such as 3,4.1 06 to 8,3-1 06 Pa (34
to 82 atmospheres gauge), preferably 5,0-7,0-106Pa (50 70 atm)., and a temperature of such as 120 to
60 230C, preferably 148 to 204C, and extruded through narrow nozzles with simultaneous releases of
pressure. As the pressure is released, due to the change in pressure and change in temperature induced by
the heating caused by the extrusion process, the moisture tends to evaporate. Preferred is control so that a
non-explosive evaporation is involved but with sufficient expansion to avoid formation of strands. This
extrusion/heating/discharge process not only removes moisture, but also removes any remaining non-
65 aqueous volatiles.

3
 0 079 596
The resulting rubber is thus broken down into small, open-celled spongy lumps, and tends to be cooled
to such as 100C by the evaporating water. Depending on the rubber, of course, particles may be produced,
or sometimes long strings.
In our invention, a pneumatic polymer eductor conveyor dryer is provided. A water-wet polymer from
5 a polymer recovery operation is received. The water-wet polymer is put through an extruder and extruded
through a die plate. The die plate as to the size of orifices, configuration thereof, number thereof, can be
varied by one skilled in the art depending on the type of rubber, amount of moisture, and the like. Usually,
in the extruder, the effect of working and compression increases the temperature of the rubber. This can be
controlled by the usual means of cooling the extruder, controlling the flow of rubber, to avoid overheating.
w Upon discharge of the rubber from the orifices, free water is removed by the extruding action at the die
plate, is atomized and/or evaporated into an air stream. Discharge from the orifices is into a closed
chamber. The closed chamber is equipped with an air input which normally is to the rear of the chamber
and is in a tangential position relative to the chamber and orifice. Immediately adjacent to, spaced away
from, but openly surrounding the die plate, is a funnel of cone or conoid type and of preferably truncated
15 construction such that the vertex of the cone or conoid has been removed. The vertex usually is removed at
a flat perpendicular plane to the cone, but could be removed, if desired, on a slanted intersecting plane
forming an elipsoid. At the resulting plane is connected a conveying tube of somewhat lesser diameter
than the base or open end of the cone or conoid. The open end of the funnel, the large end, openly but
closely surrounds the die plate, receives the rubber particles and air, and conveys them then by closed
20 connection into the discharge tube. It is important to note that the closed chamber with tangential air input
provides an effective swirling shearing action at the die plate assembly, effectively shearing and clearing
the rubber particles as they are extruded, either as particles or spaghetti strands, keeping the die plate
clean, the receiving funnel clean, and the conveying tube clean.
The tube then can discharge into a conventional hot box as shown in Figure 2, or preferably convey
25 into a receiving cyclone as shown in Figures 3, 5, and 6.
The die plate and surrounding cone are totally enclosed by a chamber into which air is input, preferably
at low pressure of such as about 13,8-103 to 27,6-103 Pa (2 to 4 psig), and importantly is input tangentially
into the chamber in an area spaced away from the die plate and cone.
The tangential air flow rate depends on the characteristics of the rubber, its water content, the
30 temperature of the extruded rubber, the temperature and humidity of the air, desired final water (moisture)
content of the rubber and relative size of extruder and chamber, and can be readily determined. Airflows of
0,047 to 47 m3/sec (100 to 100,000 cu. ft./min.) may be involved, more usually 0,47 4,7 m3/sec
(1,00010,000 cu. ft. per minute), at ambient or less to 93,3C (200F.) more usually ambient to 79,4C
(175F.).
35 The tangential air inlet into the enclosed chamber provides a vortex action at the extruder nozzle,
producing a spiral flow as the air passes into the narrow space formed by the open end of the cone
surrounding the die plate assembly, a spiral flow as the air passes across the die plate, into the cone and
into the conveying tube. In our observation, the swirling or vortex action of the air flow at the die plate
assists in pulling or stripping rubber crumbs or strands from the die plate face, as well as providing the
40 necessary air to evaporate the moisture, and to convey the "dry rubber" either into a conventional but now
useful hot box, or preferably and desirably into a cyclone receiver. It is to be noted that the orifices, the
surrounding but spaced open end of the truncated funnel, and the receiving tube sealably connected to the
plane of the truncated cone, all are axially aligned. Once past the enclosure or enclosed chamber in
accordance with our invention, the conveying tube can be handled as may be desired or convenient for
45 various plant configurations, such as shown in Figures 2, 3, 5, and 6. Discharge can be into a conventional
hot box, in which the rubbery particles are blown into and fall onto a conveyor as shown by the dotted line.
Discharge can be shown schematically into a cyclone as shown in Figure 3, or, into a cyclone as shown in
Figure 5, or into a series of cyclones, preferably with intervening grinder, as shown in Fiaure 6.

50 Polymers
The polymers to be treated usually are rubbery polymers prepared by polymerizing one or more
conjugated diene monomers alone, or in admixture with, or sequentially with one or more active CH2=C<
group which are copolymerisable therewith. Suitable comonomers containing this group CH2=C< include
the monovinylarenes as described hereinafter, as well as acrylonitrile, methyl acrylate, methyl
55 methacrylate, vinyl chloride, methyl vinyl ether, ethylene, propylene, 1-butene, 1-propene, 1-octene, and
the like. Generally at least 50 weight percent conjugated diene is used in the monomer mixture when
copolymers are prepared in order to prepare the preferred rubbery copolymers to which our invention is
most applicable.
The polymers to which the steam stripping process of our invention can be applied also include the
60 hydroxyl, carboxyl, mercapto, and amino-containing derivatives of the conjugated diene polymers
described.
The polymer cements are prepared by polymerizing the monomers in an organic solvent selected from
paraffins, cycloparaffins, and aromatic hydrocarbons, which is relatively inert, non-deleterious, and liquid
under the conditions of the polymerization process. Examples include the lower molecular weight alkanes
65 such as propane, butane, pentane, hexane, heptane, and isooctane; cycloparaffins such as cyclohexane;

4
 ) 079 596

and methylcyclohexane; and aromatic compounds such as benzene and toluene.

A variety of initiator systems are suitable for the solution polymerization process production of the
polymers.
One useful type of initiator system is a two or more component system wherein one component is an
5 organometal compound of the metals of Groups I, II, and III, including those where one or more but not all
of the organo is replaced by a halogen, a metal hydride, or a metal of Group I, II or III and the second
component is a Group IV to VI compound, e.g., salt or alcoholate. This type of initiator system is fully
described with examples in columns 5 and 8 of Patent No. 2,886,561, dated May 12, 1959.
Another type of suitable initiator system are the organolithium compounds R2(Li)x as described
70 hereinafter for preparing the lactone copolymers. The amount of organolithium initiator used to prepare
the conjugated dienes polymers can vary over a broad range, but in general is in the range of about 0.1 to
100, preferably about 0.25 to 2, gram milliequivalents of lithium per 100 parts by weight of total monomers
charged. Of course, organoalkali metal compounds of other Group la metals can be used as is known in the
art.
is Another initiator system utilizes a cobalt compound and a metal alkyl of the Group III metals as
exemplified by aluminum wherein one but not ail of the alkyl groups can be replaced by halogen. Examples
of these organometal compounds include trialkyl aluminums such as triethylaluminum and
triisobutylaluminum, and alkyl aluminum halides such as ethylaluminum dichloride and diethylaluminum
chloride. For the cobalt compound, the cobaltous form is preferred, including such as cobaltous chloride,
20 cobaltous sulfate, and cobaltous nitrate, and the salts of organic acids such as cobaltous acetate.
Conjugated dienes containing such as 4 to 12 carbon atoms per molecule, optionally with the
monovinylarenes containing such as 8 to 12 carbon atoms per molecule, can be used.
Suitable conjugated dienes include 1,3-butadiene, isoprene, piperylene, 1,3-hexadiene, 1,3-octadiene,
6-phenyl-1,3-hexadiene, and mixtures. Suitable monovinylarenes include styrene, a-methylstyrene, 4-
25 methylstyrene, 4-isopropylstyrene, 2,4-dimethylstyrene, 1-vinylnaphthalene, 2-vinylnaphthalene, and
mixtures.
Polymerization temperatures, times, and the like, do not form a part of our invention, since these are
known and are within the skill of one skilled in the art. The polymers can be linear, branched, random or
block, coupled or uncoupled, and of mixed type; and can be terminated by groups such as carboxy, all as
30 known in the art.
In emulsion polymerizations, the usual conditions can be employed, using various types of free radical
polymerization initiators, all as well known in the art.
Those products produced as a slurry, can then be recovered as discussed hereinbefore by-filtration,
pressing, and the like. Those produced as a solvent or slurry in hydrocarbon or other non-aqueous solvent
35 can be recovered by such as steam stripping, and the resulting particles then recovered by pressing,
filtration, or the like. The resulting material is a water-wet material, which may contain various amounts of
potentially hazardous hydrocarbon, and is the subject for recovery then in a dry condition free of moisture
and/or hydrocarbon solvent in accordance with the apparatus of our invention.

40. Examples
The following examples record runs/data from our development of the pneumatic polymer eductor
conveyor dryer in accordance with our invention. Particular materials employed, amounts, relationships,
and the like, are intended to be exemplary.

45 Example 1
A carboxy terminated linear block 85/15 butadiene/styrene copolymer, was first dried with the PEC
system illustrated in Figure 5. Conditions required to produce dry polymer were readily attained. Various
dies were tested in the expander die plate in an attempt to produce a polymer suitable for marketing as
crumb without success. The product form was suitable for baling, but the strands were too long and
so irregular for marketing as crumb. The product from the collecting cyclone was too hot for baling indicating
the need for an additional cooling step. The run was continued for 12 hours to demonstrate system
reliability without any significant build-up of rubber in the conveying equipment. Data for Test 1 is shown in
Table I:

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The above runs were made with equipment arrangement as snown in rigure o, wmui uuu&i&ieu
basically of a positive displacement blower, air preheater, our PEC, a cyclone, and a cyclone balancing
blower. The system is satisfactory for polymers that fragmented easily at the die plate, but tended to leave
some polymers in strands of varying length. The system satisfactorily conveyed all forms of material: fines,
indicated that the
5 crumb, and long strands. These results obtained in the above runs, as well as other runs,
air preheater was not necessary.
Example 2
A linear block 70/30 butadiene/styrene copolymer of about 160,000 Mw (wt. avg. mol. wt.) (Solprene
to 308 from Phillips Petroleum Co.) was successfully dried with the PEC system illustrated in Figure 5. The
expander die plate was fitted with one 7-hole die (0,36 cm (9/64-inch) holes). The PEC device produced a
fragile rice-like material with some fines. The PEC system handled the fines without the problems
associated with the conventional hot box system. The system was operated for about 7 hours with no
serious build-up of polymer in the conveying system.
'5
Example 3
A linear block 75/25 butadiene/styrene copolymer with about 83,000 Mw (wt. avg. mol. wt.) (Solprene
1205 from Phillips Petroleum Co.) was first dried with the PEC system illustrated in Figure 5. Several die
configurations were tested in an attempt to yield product that would be satisfactory to package as crumb.
io Two 37-hole dies (0,16 cm (1/16-inch) holes) produced strands up to 30,5 cm (12 inches) long and appeared
to have too much open area for Solprene 1205. Product moisture was about 1.0 percent. Four 1-hole dies
(0,48 cm (3/16 inch) holes) also produced long strands at 0.5 to 1.0 per cent moisture. Use of two 1-hole dies
(0,24 cm (3/32-inch) holes) over-dried the polymer and produced a mixture of fine, crumb, and strands.
Three 1-hole dies (0,24 cm (3/32-inch) holes) gave dry polymer and 5,07,6 cm (23 inch) strands. The PEC
>5 satisfactorily conveyed all of these polymer forms. The failure of Solprene 1205 to fragment into crumb at
the die plate is probably due to the characteristics of the Pilot Plant expeller-expander system. Moisture in
the expeller discharge is not high enough to give much blasting at the expander die plate. A total of 906 kg
(2000 pounds) of polymer was dried during this test with no appreciable build-up of polymer in the
conveying system. Data for the first Solprene 1205 test is shown in Table II:
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Example 4
The PEC system was revised to eliminate the air preheater and incorporate a Wedco UT-18 mill and an
additinal cyclone as illustrated in Figure 6. The Wedco screen, cutting blocks and speed can be varied to
give the desired polymer size reduction. This system alalowed for a complete change of air between the
s PEC device and the final product discharge, thus aiding in drying and cooling the polymer.
A second test using the same type of copolymer as described in Example I was made after the Wedco.
mill and the second cyclone were added to the PEC system as shown in Figure 6. The expander die plate
contained two 37-hole (0,16 cm (1/16-inch) holes) dies. The Wedco mill contained a screen with 0,64 cm
(1/14-inch) holes, 0,95 cm (3/8-inch) cutting blocks with 0,64 cm (1/4-inch) clearance, and was operated at
w 53,3 Hz (3200 RPM). Strands of varying lengths 1,3 to 13 cm (1/2 to 5 inches) were produced at the die plate.
The strands were conveyed without difficulty to the Wedco mill where they were reduced to a rice-like form
which was ideal for packaging as crumb. Moisture contents of the material from the first cyclone to the
Wedco mill and from the second cyclone were both about 1 percent. Data for Test 2 is shown in Table III:

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*

10
 I 079 596

Following this test the transport line from the first cyclone to tne weaco mm was revisea 10 diiuw d
more complete exchange of air. This allowed the system to dry the rubber to less than 0.5 per cent
moisture. Later tests demonstrated that Solprene 1205 could be dried to a very low moisture content with
the revised system.
5 Example 5
A second Solprene 1205 test was made after the Wedco mill and the second cyclone were added to the
PEC system as shown in Figure 6. The expander die plate contained three one-hole dies (0,24 cm (3/32-inch)
holes) and the Wedco mill was fitted with a 0,95 cm (3/8-inch) screen, 0,63 cm (1/4-inch) cutting blocks with
0,63 cm (1/4-inch) clearance, and was operated at 33,3 Hz (2000 RPM). The polymer was dry almost
o immediately after a successful start-up and the product form appeared satisfactory for packaging as crumb.
The dryer line was operated for 5h hours to produce 734 kg (1620 pounds) of crumb, packaged in BC-4
boxes for sampling. During the 5i hour run dryer conditions were varied slightly to increase the amount of
volatiles from a very low level to a level near the top of the moisture specification. Data at the higher
volatile levels indicated that additional drying was occurring as the polymer passed through the Wedco mill
5 and the segond cyclone. Data for the second Solprene 1205 test is shown in Table IV:

TABLE IV

PRODUCT EDUCTOR CONVEYOR

:o
Solprene 1205 Test 2
(3-1 hole (0,24 cm (3/32-inch) holes))

Volatiles, 7o
:xpander Product Temp (F.)C
Rate From From
(RPM) Hz Temp.(F*)C #/hr Expeller Expander Final To Mill Final
Amps

42 (150)2,50 (380)193 310 - 0.20 0.20 (167)75,0 (113)45,0

jo
46 (150)2,50 (353)178 430 6.0 0.25 0.25 (167)75,0 (122)50,0

50 (117)1,95 .(333)167 372 8.0 1.25 0.90 (167)75,0 (113)45,0

'5 (172)78,0 (117)47,2
48 (140)2,33 (335)168 380 - 1.00 0.85

*At last breaker bolt

40 During the initial start-up the operator had trouble keeping tne dies seatea in tne aie piaxe. i nib
resulted in several false starts. During one of these starts the rubber overheated and the expander
discharged a cloud of smoke that quickly dissipated. There were no indications of burned polymer. This has
been one of the unexpected advantages of the PEC system. Several times during upset conditions the
expander has reached temperatures that would normally result in burning rubber in the hot box, but with
45 the PEC system no burning polymer has been experienced.
It can be readily seen from the data above that a variety of polymers can be processed through the PEC
of our invention, to produce low volatile content dry products without gel formation. Our PEC system
eliminates the wet spots and gel particles frequently experienced with a conventional extruder hot box
system. The incorporation of a Wedco mill in the PEC pneumatic loop provided a means of controlling the
from
so form of the final products. Clearly, our PEC system reduces the risk of dryer line fires resulting
overheated polymer.
Another option that we have developed, and illustrated in our attached Figure 2, is the use of an
additive, such as talcum, or can be other finely divided material such as calcium carbonate, zinc stearate,
which can be blown to treat the rubbery particles. This system also can be utilized to incorporate a variety
55 of other additives into the final polymer, if desired.
- Presently preferred is a heated air input would involve about 2,36 m3 (5000 cubic feet) per second
(minute) of such as about 63C (146F), by means of a 15,2 cm (6-inch) line at a flow velocity of .130 m/sec
discharging into our closed blocks employing a 30,5 cm (12-inch) diameter die plate, with a funnel of about
39,4 cm (15.5 inches) diameter, openly surrounding the die plate, with a narrow passageway between the
60 cone and the die plate, of about 1,3 cm (0.50 inch) clearance, producing a velocity at that point estimated at
about 195 meters per second, dropping in the cone truncated section to about 65 metres per second, and
then increasing again in the discharge line which conveniently can be such as about 15,2 cm (6-inches) in
diameter, to the original velocity of about 130 meters per second. Preferably and conveniently, in the axially
aligned receiving tube or pipe, can be inserted vanes in order to, in effect, straighten out the air swirl for
65 more convenient air conveying.

11
 0 079 596
In addition to the runs described above, a variety of other materials have been employed, such as a cis-
4-polybutadiene which is a homopolymer of high content cis-butadiene with about 200,000 Mw (weight
average molecular weight).

5 Example 6
The PEC (Pneumatic Educator Conveyor) was used for a series of tests for the drying of Cis-4
polybutadiene rubber. The PEC system was as illustrated in Figure 5, with the talcum eductor of Figure 2.
This PEC system consisted of a positive displacement blower, heat exchanger, air chamber, die plate,
cyclone, associated air conveying piping, and a talcum powder eductor and feeder chamber. A series of six
to tests were made dry Cis-4 polybutadiene. A summary of the tests is as shown in Table V:

15

20

25

30

35

40

45

50

55

60

65

12
 >

o_ x:0 <u a ^ a -
10- S-
0 ca < 0cu5 _T3
a. ^
1" 2 cu cd -a 0 '5
S 73 73 -D 0 -c -Q
_ C O) CD
C g. 2 ^
ro X C! "=
OC fl) CO r-
0 Q- t]}TJ
0 .S g |
g g

O S
!f 12 c> C E
It 2 u cn cdO C O
cd co 0
O d 0 -32 0 0 -2? 0
tt - .c 0 x: x: 0 ^t.
y>-
3 O .C_D x: ,C
_DO CD il._
x: 0
i_ 1
a - 3 2
S 5S 2 rs.
? E E c
1 CO CO C CO CO Z CD
y i 5 ^ .5 g
-J 0 ,j=. 7 3.
T3
,73
Q
O X: x:O .x: -~
x:O -=
O O XI
n; C U C CO
sr C
C O C i -
n"
- a c CO
co CO co @- CO 2
- CO r- CN T-
> > > > CO >
LO .2
E E "T "=>
0 0 0 0 E 0 -p
CD CO CO CO CO O
r"- 3 r"-.c
0 0 0 0 X 0 CM
@ @ - @ 0 ,
ps psO rs ps ' rsOHi
CO C CO CO is. C

M m
013_
^ fO CO U> CO CO
ro ^ x i x i x i ^ x r
g 3 c M C M c o i o c " ( ' '
1DC

+j
N PI ^ II) ID

13
 0 079 596

In spite of problems which required correcting prior to continuing the test runs, a majority of the Cis-4
polybutadiene was dried successfully. However, inspection of the Cis-4 polybutadiene holes after two
weeks showed that a portion of the polymer was actually wet with 0.27 to 1.17 weight percent volatiles. A
portion of the holes appeared to have very small white spots. These white spots were attributed not to the
5 PEC system but to the weigh scale system that allowed rubber to build up and then drop back into the Cis-4
polybutadiene product during the dumping cycle of the weigh scales. Further design could produce an
elimination of the white spots from weigh scale rubber build up.
In summary, the Cis-4 polybutadiene tests of the PEC system were successful in producing dry rubber.
The disclosure, including data, has illustrated the value and effectiveness of our invention. The
10 examples, the knowledge and background of the field of the invention and the general principles of
chemistry and of other applicable sciences have formed the bases from which the broad descriptions of our
invention including the ranges of conditions and the generic groups of operant components have been
developed, and formed the bases for our claims here appended.

is Claims

1. An apparatus for drying water-wet polymers, comprising:

a) a die plate (1) with an inlet side, a discharge side (12), and orifices (2) through said die plate suitable
for extruding a wet polymer,
20 b) a receiver chamber having a large open end and a smaller discharge end, said large open end
closely surrounding said die plate (1) leaving a clearance (5) thereto,
c) a discharge means (6) connected to said smaller end,
d) polymer collector means connected to said discharge means,
e) a closed chamber (7) surrounding said discharge side (12) of said die plate CD and said receiver
25 chamber, said closed chamber (7) having an air inlet into said chamber,
characterized by the fact that
f) said receiver chamber is in the shape of a funnel (3), which has its large open end closely
surrounding said die plate (1), and
g) said air inlet (1 1) is positioned at said closed chamber (7) away from the die plate (1 ) and is designed
30 and arranged for tangential air injection into said chamber (7), the tangentially injected air resulting in a
swirling vortex action at the discharge side of the die plate (1).
2. Apparatus according to claim 1 characterized in that said discharge means comprises a conveying
tube (6).
3. The apparatus according to claim 1 or 2 characterized in that said collector means comprise a hot
35 box (22).
4. The apparatus according to at least one of claims 1 to 3 characterized in that said funnel (3) is a
truncated cone or conoid.
5. The apparatus according to claim 1,2 or 4 characterized in that said collector means comprise, a first
cyclone (41, 61) operably connected to the downstream end of said discharge means (6).
40 6. The apparatus according to claim 5 characterized in that said collecting means comprise in sequence
said first cyclone (61), a grinder (63), a second cyclone (41, Figure 6) and conveying means (64) from said
grinder to said second cyclone (41).
7. The apparatus according to at least one of claims 1 to 6 characterized in that an air input source is
connected to said air inlet (11) to permit an air input rate of the order of about 140m3 per minute at a
45 temperature of about 63C by means of a 15cm inlet line, said die plate employs a 30cm diameter die plate,
said funnel has a diameter of about 40cm, and is openly associated with die plate face permitting about
1.3cm clearance.
8. The apparatus according to at least one of claims 1 to 7 characterized by an additive feeder (27, 28,
29) suitable for feeding an additive into an air stream upstream of said air inlet.
50 9. The apparatus according to at least one of claims 1 to 8 characterized by further incorporating means
for at least one of heating air, cooling air, or controlling humidity of air to be employed as an air stream to
said air inlet.
10. A process for drying a water-wet polymer which comprises extruding said water-wet polymer
through orifices of an extruder die plate, expanding the extruded wet polymer on the discharge side of the
55 die plate, contacting the expanding wet polymer with an air stream, thereby substantially evaporating said
water into said air stream, discharging the extruded polymer and moisture from said die plate into a closely
adjacently positioned open end of a truncated funnel receiver openly surrounding said die plate, and
sealably connecting at its truncated end with a lesser diameter dried polymer conveying means, said die
plate and funnel receiver totally enclosed by a chamber, characterized in that air is tangentially introduced
bo into said chamber, said air is passed along the discharge side of said die plate in a vortex-type swirling
motion, said air inlet means positioned in said chamber, effective for tangential air inlet away from said die
plate means and 'to the rear of said funnel receiver means, thereby stripping said polymer particles from
said die plate into said dried polymer conveying means, thereby resulting in a substantially dried polymer.
11. The process according to claim 10 characterized in that said air stream is input at a pressure of
65 about 1.3 to 2.8 MPa.

14
 0 079 596

12. The process according to claim 10 or 11 characterized in that said polymers are solution
polymerized conjugated diene polymers selected from homopolymers, or copolymers with
monovinylarenes or other CH2=C<group, preferably a 75/25 block copolymer.
13. The process according to at least one of claims 10 to 12 characterized in that said polymer is a linear
5 butadiene/styrene block copolymer, preferably an 85/15 carboxy terminated butadiene/styrene copolymer
or a 70/30 butadiene/styrene copolymer, or is cis-polybutadiene.
14. The process according to at least one of claims 10 to 13, characterized in that said air is input at a
rate of the order of about 140 m3 per minute at a temperature of about 63C by means of a 15 cm inlet line,
said die plate employs a 30cm diameter die plate, said funnel has a diameter of about 40cm, and is openly
10 associated with die plate face permitting about 1.3cm clearance.

Patentanspriiche

75 1. Vorrichtung zum Trocknen wasserfeuchter Polymere mit:

a) einer PreBplatte (1 ) mit einer EinlaBseite, einer Abfuhrungsseite und zum Extrudieren eines feuchten
Polymers geeigneten Offnungen (2) durch die PreBplatte,
b) einer Aufnahmekammer mit einem groBen offenen Ende und einem kleineren Abfiihrungsende,
wobei das groBe offene Ende die Druckplatte (1) eng umgibt und zu dieser einen Freiraum (5) belaBt,
20 c) einer mit dem kleineren Ende verbundenen Abfuhrungseinrichtung (6),
d) einer mit der Abfuhrungseinrichtung verbundenen Polymersammeleinrichtung,
e) einer die Abfuhrungsseite (12) der PreBplatt (1) und die Aufnahmekammer umgebenden
geschlossenen Kammer (7), wobei die geschlossene Kammer (7) einen LufteinlaB in die Kammer hat,
dadurch gekennzeichnet, daB
25 f) die Aufnahmekammer die Gestalt eines Trichters (3) hat, wobei ihr groBes Ende die PreBplatte (1)
eng umgibt, und
g) der LufteinlaB (11) an der geschlossenen Kammer (7) entfernt von der PreBplatte (1) angebracht ist
und zum tangentialen Einblasen von Luft in die Kammer (7) ausgelegt und angeordnet ist, wobei die
tangential eingeblasene Luft zu einem Wirbelstrudel an der Abfuhrungsseite der PreBplatte (1) fuhrt.
30 2. Vorrichtung gemaB Anspruch 1, dadurch gekennzeichnet, daB die Abfuhrungseinrichtung ein
Ubertragungsrohr (6) aufweist.
3. Vorrichtung gemaB Anspruch 1 oder 2, dadurch gekennzeichnet, daB die Sammeleinrichtung einen
Heizkasten (22) enthalt.
4. Vorrichtung. nach mindestens einem der Anspriiche 13, dadurch gekennzeichnet, daB derTrichter
35 (3) ein abgestumpfter Kegel oder Kegelstumpf ist.
5. Vorrichtung gemaB Anspruch 1, 2 oder 4, dadurch gekennzeichnet, da(S die Sammeleinrichtung
einen ersten Zyklon (41, 61) aufweist, der in Arbeitsverbindung mit dem Stromungsabwartsende der
Abfuhrungseinrichtung (6) steht.
6. Vorrichtung gemaB Anspruch 5, dadurch gekennzeichnet, daB die Sammeleinrichtung nacheinander
40 den ersten Zyklon (61), ein Mahlwerk (63), einen zweiten Zyklon (41, Fig. 6) und eine
Uberfuhrungseinrichtung (64) von dem Mahlwerk zu dem zweiten Zyklon (41) aufweist.
7. Vorrichtung gemaB mindestens einem der Anspriiche 16, dadurch gekennzeichnet, daB mit dem
LufteinlaB (11) eine LufteinlaBquelle verbunden ist, urn eine LufteinlaBrate von etwa 140 m3 pro min. bei
einer Temperatur von etwa 63C mit Hilfe einer 15 cm-EinlaBleitung zu ermoglichen, daB fur die PreBplatte
45 eine PreBplatte mit 30 cm Durchmesser eingesetzt wird, daB der Trichter einen Durchmesser von etwa 40
cm hat und in offener Weise mit der PreBplattenflache verbunden ist, wobei ein Freiraum von etwa 1,3 cm
ermoglicht wird.
8. Vorrichtung nach mindestens einem der Anspriiche 17, gekennzeichnet durch einen zusatzlichen
Einspeiser (27, 28, 29), der zum Einspeisen eines Additivs in den Luftstrom stromaufwarts von dem
so LufteinlaB ausgelegt ist.
9. Vorrichtung nach mindestens einem der Anspriiche 18, dadurch gekennzeichnet, daB erweiterhin
eine Einrichtung fur mindestens eine der MaBnahmen der Luftbeheizung, Luftkiihlung oder Steuern der
Feuchtigkeit der Luft beinhaltet, die als Luftstrom fur den LufteinlaB eingesetzt wird.
10. Verfahren zum Trocknen eines wasserfeuchten Polymers, bei dem man das wasserfeuchte Polymer
55 durch Offnungen einer ExtruderpreBplatte extrudiert, das extrudierte feuchte Polymer an der
Abfuhrungsseite der PreBplatte expandiert, das expandierende feuchte Polymer mit einem Luftstrom in
Kontakt bringt, wodurch das Wasser in den Luftstrom im wesentlichen verdampft wird, das extrudierte
Polymer und Feuchtigkeit von der PreBplatte in ein nahe angrenzend angeordnetes offenes Ende eines
abgestumpften Trichteraufnehmers abfiihrt, der die PreBplatte offen umgibt und an seinem abgestumpften
so Ende mit kleinerem Durchmesser mit der Uberfiihrungseinrichtung fur trockenes Polymer, abdichtbar
verbunden ist, wobei die PreBplatte und der Trichter vollig von einer Kammer umgeben sind, dadurch
gekennzeichnet, daB man in die Kammer tangential Luft einfiihrt, die Luft in einer Wirbelstrudelbewegung
entlang der Abfuhrungsseite der PreBplatte fuhrt, wobei die in der Kammer angeordnete
LufteinlaBeinrichtung fur tangentialen LufteinlaB entfernt von der Druckplatteneinrichtung und zum Ende
65 der Trichteraufnahmeeinrichtung hin sorgt, wodurch die Polymerteilchen von der PreBplatte in die

15
 0 079 596

Uberfiihrungseinrichtung fur trockenes Polymer gestrippt werden, was zu einem im wesentlichen

trockenen Polymer fuhrt.
11. Verfahren nach Anspruch 10, dadurch gekennzeichnet, daB der Luftstrom mit einem Druck von
etwa 1,3 2,8 MPa eingefuhrt wird.
5 12. Verfahren nach Anspruch 10 oder 11, dadurch gekennzeichnet, daB die Polymere
losungspolymerisierte konjugierte Dienpolymere sind, ausgewahlt aus Homopolymeren oder
Copolymeren mit Monovinylarenen oder anderen
/
w CH2=C
\
-Gruppen, bevorzugt ein 75/25-Blockcopolymer.
13. Verfahren nach mindestens einem der Anspriiche 1012, dadurch gekennzeichnet, daB das
Polymer ein linerares Butadien/Styrol-Blockcopolymer ist, bevorzugt ein 85/15-Butadien/Styrol-Copolymer
15 mit Carboxyendgruppen oder ein 70/30-Butadien/Styrol-Copolymer oder cis-Polybutadien ist.
14. Verfahren nach mindestens einem der Anspriiche 10 13, dadurch gekennzeichnet, daB die Luft mit
einer Rate von etwa 140 m3 pro min. bei einer Temperatur von etwa 63C mit Hilfe einer 15 cm-
EinlaBleitung zugefiihrt wird, daB fur die PreBplatte eine PreBplatte mit 30 cm Durchmesser eingesetzt
wird, daB der Trichter einen Durchmesser von etwa 40 cm hat und mit der PreBplattenflache offen
20 verbunden ist, wobei ein Freiraum von etwa 1,3 cm ermoglicht wird.
Revendications

1. Dispositif pour le sechage de polymeres humectes d'eau comprenant:

25 a) un filiere (1) avec un cote d'entree, un cote de decharge (12), et des orifices (2) traversant la filiere
convenant a I'extrusion d'un polymere humide,
b) une chambre de recepteur comportant une grande extremite ouverte et une extremite de decharge
plus petite, la grande extremite ouverte entourant etroitement la filiere (1 ) en formant un jeu (5) avec celle-
ci,
so c) un moyen de decharge (6) connecte a la plus petite extremite,
d) un moyen collecteur de polymere connecte au moyen de decharge;
e) une chambre fermee (7) entourant le cote de decharge (12) de la filiere (1) et la chambre du
recepteur, la chambre fermee (7) ayant une entree d'air dans la chambre, caracterise en ce que:
f) la chambre du recepteur a la forme d'un entonnoir (3), qui a sa grande extremite ouverte entourant
35 etroitement la filiere (1), et
g) I'entree d'air (1 1) est piacee au droit de la chambre fermee (7) distante de la filiere (1 ) et est concue et
disposee pour une injection tangentielle d'air dans la chambre (7) I'air injecte tangentiellement provoquant
un effet de tourbillons au cote de decharge de la filiere (1).
2. Dispositif selon la revendication 1, caracterise en ce que le moyen de decharge comprend un tube de
40 convoyage (6).
3. Dispositif selon la revendication 1 ou la revendication 2, caracterise en ce que le moyen de collecteur
comprend une boTte chaude (22).
4. Dispositif selon au moins I'une des revendications 1 a 3, caracterise en ce que I'entonnoir (3) est un
cone ou conoi'de tronque.
45 5. Dispositif selon la revendication 1, la revendication 2, ou la revendication 4, caracterise en ce que le
moyen de collecteur comprend un premier cyclone (41, 61) connecte fonctionnellement a I'extremite aval
du moyen de decharge (6).
6. Dispositif selon la revendication 5, caracterise en ce que le moyen de collecteur comprend a la suite
le premier cyclone (61), un broyeur (63), un second cyclone (41, figure 6) et un moyen de convoyage (64)
so entre le broyeur et le second cyclone (41).
7. Dispositif selon au moins I'une des revendications 1 a 6, caracterise en ce qu'une source d'entree
d'air est connectee a I'entree d'air (11) pour permettre un debit d'air d'entree de I'ordre de 140 m3 par
minute a une temperature d'environ 63C au moyen d'une conduite d'entree de 15 cm, la filiere emploie
une plaque de filiere de 30 cm de diametre, I'entonnoir a un diametre d'environ 40 cm, et est associe de
55 maniere ouverte a la face de la filiere permettant un jeu d'environ 1,3 cm.
8. Dispositif selon au moins I'une des revendications 1 a 7, caracterise par un dispositif s u p p l e m e n t a l
d'alimentation (27, 28, 29) convenant a ('introduction d'un additif dans un courant d'air en amont de
I'entree d'air.
9. Dispositif selon au moins I'une des revendications 1 a 8, caracterise en ce qu'on incorpore en outre
60 un moyen pour au moins I'air de chauffage, ou I'air de refroidissement, ou la commande de I'humidite de
I'air devant etre employe comme courant d'air applique a I'entree d'air.
10. Procede pour le sechage d'un polymere humecte d'eau qui comprend I'extrusion du polymere
humecte d'eau par les orifices d'une filiere d'extrudeuse, la detente du polymere humide extrude sur le
cote de decharge de la filiere, la mise en contact du polymere humide detendu avec un courant d'air, ce qui
65 a pour effet d'evaporer sensiblement I'eau du courant d'air, la decharge du polymere extrude et de

16
 0 079 596
I'humidite a partir de la filiere dans une extremite ouverte placee tres pres d'un recepteur a entonnoir
tronque entourant de facon ouverte la filiere, et connecte de fagon etanche a son extremite tronquee a un
moyen de convoyage de polymere seche de diametre plus faible, la filiere et le recepteur a entonnoir etant
totalement enfermes dans une chambre, caracterise en ce que I'air est introduit tangentiellement dans la
5 chambre, I'air est transmis au cote de decharge de la filiere dans un mouvement tourbillonnant, le moyen
d'entree d'air est place dans la chambre, permettant une entree tangentielle d'air a distance du moyen de
filiere et jusqu'a I'arriere du moyen de recepteur a entonnoir, d'ou I'extraction des particules de polymere
de la filiere et leur entree dans le moyen de convoyage de polymere seche, ce qui permet d'obtenir un
polymere pratiquement seche.
w 11. Procede selon la revendication 10, caracterise en ce que le courant d'air entre a une pression
comprise entre environ 1,3 et 2,8 MPa.
12. Procede selon la revendication 10 ou la revendication 11, caracterise en ce que les polymeres sont
des polymeres dienes conjugues polymerises en solution, choisis parmi les homopolymeres, ou
copolymeres avec des monovinylarenes ou autre groupe CH2=C<, de preference un copolymere sequence
is 75/25.
13. Procede selon au moins I'une des revendications 10 a 12, caracterise en ce que le polymere est un
copolymere sequence de butadiene/styrene lineaire, de preference un copolymere 85/15 de butadiene/
styrene a terminaison carboxy ou un copolymere 70/30 de butadiene/styrene, ou est un cis-polybutadiene.
14. Procede selon au moins I'une des revendications 10 a 13, caracterise en ce que I'air entre a un debit
20 de I'ordre de 140 m3 par minute a une temperature d'environ 63C au moyen d'une conduite d'entree de 15
cm, la filiere emploie une plaque de 30 cm de diametre, I'entonnoir a un diametre d'environ 40 cm, et est
associe en etant ouvert a la face de la filiere, permettant un jeu d'environ 1,3 cm.

25

30

35

40

45

50

55

60

65

17
0 079 596

MR
0 079 596
0 079 596

3
 U 079 596

46 45
_J^__^EXHAUST
bLUWER

r , HOPPER

LX I HUULK

3eS ( 32> ^-43

( FIG. I)
\ Q ATrn i
g nc-Mi en
AIR (OPTIONAL) V8

,53
BALE
HOPPER
 D 079 596

3 3 * :xhaust
DAMPER-^
( CYCLONE \ f h BLOWER
61
5I> .HOPPER ^-"42

V / Y
J | EXTRUDER /62 .43

64-
f(SEE
FIG. I)

GRINDER ,
63^"

,53
3ALE HOPPER

F/cS. 6