Process and devices for the plasticized matter division and products obtained.

AS AFRICAN INDUSTRIAL PROPERTY AND THE MALAGASY PATENT

P. 887

international Patent Classification yaoundê (Cameroon): 29 no. 02459 b.

O A'm>e. I request 28 June 1967 to 8 hr 30 min. to roro.a.m.p.i. (G.P. № 52,989) by

the company anonymous said: National firm oils Aquitaine, residing in France

5 May 1970 delivered

Published at official ballot № 1 of 1970

PRIORITY:

Patent applications filed in France under the no. 67818 67819 1 July 1966 and on behalf of the applicant.

Method and devices for the division of plasticized material and products.

The present invention provides a novel method for the division of various materials plasticized, for the preparation of pieces with at least two divisions are very small the j it aims in particular to produce parts

5 such as particles, granules, granulates, wire, filament, rods, small cylinders, and the like, from a mass of plasticized material, which may be a resin and - particularly sulfur rendered plastic by the addition of suitable substances, it also concerns a device for performing the inventive method 10. The invention further relates to a novel type of pieces, in particular particles, beads, pellets, wire, filament, rod, or other small cylinders, plasticized material} especially it comprises granules of various sizes in plasticized sulfur "

Of Monte * for the division of the plastics are well known in 1 * industrie T-it is known to prepare powders "granules, wires and c *" lily by conventional means grinding "scattering" spinning "molding" c *" from most existing resins 1 * heure to current. However "difficulties arise" when it comes to turn each divided form each material containing a substantial proportion of plasticizer f be the plasticized material being more or less moderated "or softens at lesser échauffextent" milling becomes very difficult T-year that legal rights the method of spinning "optionally followed by cutting" it suffers from slowness "with which solidify in general materials highly plasticized" primarily with certain plasticizers. This dlfficulté was dressed "with the epoch" by the creation of the "plastisol", particularly those chloride polyvinyls "it is-to-th e. resin dispersions in softeners" but the problem has not been solved for plasticizers that " into which the resin nsec not inflate cold *

The difficulties mentioned have an cannot transform seeks to divide a mass of plasticized sulfur "such masses have at present several interesting applications" their use is economical, and is known to easily prepare these produced in various ways "in particular" by plasticizing molten sulfur " by any plasticizer known to plasticize the sulfur. Gold, these masses have the property of solidifying into very slowly I when they are cast into ingot molds " solidification request several hours, or even a full day, according to their plasticizer content. The d * on the other hand, grinding the resulting ingots provides powder which has each rapid caking tendency. Ultimately obtaining divided pieces, as grain, wires and the like, from plastic compounds of sulfur, is awkward, and even more so as the plasticizer content is high. This disadvantage is eliminated by the present invention which provides for rapid, by operations, simple and economical, the various kinds of shapes of parts it may be desirable in industry, particularly powders and granules more or less fine, easy to bagging, non-caking.

The new method according to the invention comprises contacting the plasticized material, taken in the liquid state, in the form of drops or/and nets, causing these drops or/and threads in contact with a powder of the Laddie-state material unplasticized, and cool them to solidification.

The realization of this process can give rise to several variations, some of which are indicated below without limitation.

According to a possible procedures, the threads and/or drops of liquid are introduced into the powder of the same material, but free of plasticizer. After cooling and solidification of the grains or/and resultant wires, they are separated from the excess powder, by sieving, blowing or any other known means.

Another embodiment includes applying the drops or/and threads liquids on a non-plasticized powder layer. This can be done conveniently, for example on a conveyor belt, a bucket chain or other similar means, which is also suitable to cooling.

In an alternative embodiment of the new method, the non-plasticized material powder is projected on the drops and/or threads of the plasticized material liquid, and can possibly drive them to a cooling zone and/or separation of the powder. The respective trajectory drops or threads and powder may be parallel, perpendicular or inclined at any desired angle relative to each other.

In one embodiment, drops of rain fall, under their own weight, into a chamber traversed horizontally by a stream of non-plasticized material powder.

If this skxakx last is drove by a carrier gas, especially, it is easy to obtain the necessary cooling, during the same operation, by properly adjusting the temperature of this gas to its inlet, in said chamber.

Although the flow of the liquid material under its own weight, th through openings of proper size and shape, such as holes, slots, andc gates ", either in a convenient, it may be recommendable deliver liquid from all pressure by projection means and/or spray, such as nozzles, nozzles, atomizers or other. This increases the interest th inject liquid, divided into drops, drops, threads or plies, from bottom to top, within EMI layer dandelion plasticized material powder.

Generally, the shape and dimensions

parts corresponding parameters depend on obtaining drops or/and threaded processed. Lice of preparing granules regular "it is preferable to deliver liquid into discrete drops" while wires or filaments can be made from fillets of liquid.

One highly advantageous

the method of the invention is to employ powder ' dobby unplasticized state of fluidized bed /|the drops or threads and the plasticized material, liquid "were inserted into bed by a means set forth above" especially by free fall or by injection or spraying, the encounter of the liquid with the powder can occur in cocurrent, in countercurrent, an angle or transversely. Introduction of the drops or liquid streams under their own weight, and the counter flow of the fluidized bed, is strong practical and allows operation industrial very satisfying.

The use of the fluidized bed makes it possible, in particular, the manufacture very uniform granules of any desired size, what is strong appreciable for the masses of plasticized sulfur. Indeed, the fluidized bed of powder has a uniform temperature which can be easily maintained constant, due to the thermal inertia of the bed, this permits the solidification of the granules to a temperature well determined.

On the other hand, due to the very good heat exchange coefficients, within the bed, the sensible heat drops and their heat of solidification are readily removed by GaT- fluidizing, it is to say the Xe air more often. It is " in effect, easy for modifying the flow rate of this gas or/and on its temperature at the inlet of the bed, for performing the required refroidisseraent granules formed from the droplets and of the powder. Further_C. some heat may be removed through the walls of the apparatus used " with the proper exchange coefficient between the fluidizing bed and the walls.

Cooling of product during the process of the invention can be realized in a variety of ways "© I-known" some of which are mentioned above. 11 may be equally useful cool previously powder not plasticized. A convenient "applicable in most cases" injected "into the medium operational" a certain amount of water "preferably pulverized" whose evaporation removes heat.

For the method described for the, noncrystalline powder plasticized "very various sizes" are applicable "for example from dust extrafine of the order of one micron or less" up to grains that can measure a few tenths of a millimeter|in general are well suited the powders to granules having an average size is about 0 "01 to 0.5 mm, in the case of sulfur" precautions are commendable "especially the agitation of the formed granules" when the powder unplasticized "employed" contains particles of dimensions inféxbures th about 0.05 mm) from the finesse of a caking can manifest.

The acceleration of the solidification of the plasticized sulfur liquid "under sulfur particles unplasticized" to be attributable a phenomenon of incipient crystallization|said particles "acting as nucleation" would cease supercooling the plasticized sulfur.

The method of the invention gives excellent results with "for example" the masses of plasticized sulfur described in French patents company National oils is Aquitaine no. 1,373 025 "sulfur plastic mass" of the 6 May 1963, to adding to that Patent no. 84,831 of 12 November 1963, I-1,418 067 degrees. "plasticized sulfur" of the 23 · · 7 64, no. 1,438 363 "resins to sulfur, modified, of high adhesiveness" of the 23.3, 65, n °

1,470 133 of the 14, 5.65 "preparation sulfur nonflammable * and no. 1,480 194 of the 11 March 1966" plasticized sulfur to adhesive properties containing an olefin polymer ". These masses of plasticized sulfur can contain, if ya, a certain proportion of fillers, pigment, dye, or the like and/or drops of liquid threads these masses are produced in general between 100° and 250 °c.

Another example of the application of the new method is in the production of filaments made from polyvinyl chloride highly plasticized. In this case, for example, liquid streams of polyvinyl chloride with 20 40% of H plasticizer such as a phthalic ester or phosphoric acid, is contacted with the powder leads polyvinyl chloride free of any plasticized. The coating liquid streams with same, and simultaneously cooling, cause rapid solidification, handleable with filament formation, which does not stick to each other.

Similarly, the method applies-T it, for example,

hr other vinyl resins, to retinas acrylic, cellulosic *, epoxy, a polyester, or other thiorésines, containing a substantial proportion of a suitable plasticizer.

The products according to the invention are components of which at least two dimensions are very small, especially particles, seed, pellets, queue, filament, rods, small cylinders and so on, in a plasticized material, having this by " ticularity as including a surface layer of the same material but not plasticized,

Dane-these products, the eouche surface constitutes, most often, 0.1 hr 10% of the total weight of each piece.

A special shape products according to the invention is a granule, the dimensions of which can vary, for example from about 0.5 to 5 mm, and whose core, formed of plasticized material, is more or less coated with material of a mime type, but non-plasticized, of a thickness equal to about 0.2 2.2% th th of the average size of the granule,

Uh to particular product consists of such granules having a core of the Tooling eoufre plasticized and the surface layer in-sulfur free of plasticizer *

In shapes of the new product, the surface layer is granular or even discontinuous, which may animal that observed microscopically,

The device for implementing the method according to the invention comprises means for holding a plastic mass in the liquid state, means for splitting into drops had threads, and means for creating a powder bed unplasticized.

The means for dividing a plastic mass in drops can be constituted by ramps, apples, gutters, watering cans, capillary tubes, and so on said means can be constituted by a box of which the bottom door of puncture " whose diameter is preferably constant.

The bottom is preferably a polytetrafluoroethylene.

A vibration generating device, such electromagnet, is, according to a particular trait of the invention, associated with the drop forming device.

The powder bed unplasticized is preferably a fluidized powder bed.

The powder bed unplasticized can cover a conveyor belt.

The devices for implementing the method of the invention can be illustrated, but not limited, by a spine embodiments shown in the accompanying drawings.

Figure 1 is a schematic axial section of a device according to the invention.

Figure 2 represents in plan the detail of the bottom of a

pan drop distribution.

Figure 3 shows, in schematic elevation, an alternative means for distributing back drops.

Figure 4 is another variation of drop dispenser, in plan view.

Fig., 5 indicates the corresponding lift hr Figure 4. Figure 6 is schematic axial section um in of another device according to the invention.

The device according to Figure 1 has a roll shell

1, to conical lower portion} a tray 2, annular, the bottom of which consists of each plate have holes bored calibrated vaccinica Teflon, is flush with the top of the ferrule political parties, the DS to ensure perfect horizontality laditsplaqus SS. 4 mT ferrule contains each rotisseries and a stirring device 5 j of the apparatus is flanked the Sn addition of a cyclone 6 for the separated " except fines carried by the air, the DS sieving device 7, a system of recycling fine 14 and a fluidizing air blower 8,

The operation of the device according to Figure 1

is as follows. The fluidizing air enters through the ducts in the ferrule 3 1 F. its flow rate is such that the powder the DS sulfur, introduced into I by 12, from each feed hopper 15 and the cyclone 6, either visually in the form of a fluidized bed, filling at least one high parties the DS space oduc "the unemployment the ferrule 1" the annular tank 2 contains plasticized sulfur molten steel plates drops the DS liquid are produitts by the bottom of the pan, and fall by gravity into the fluidized bed 9, in lequtl it " SSs cover with a thin layer of dust sulfur, the heat of solidification of the sulfur is removed from the system by the air flowing between th at room temperature, and escapes through the tube 10, to a temperature close to that of the sulfur-solidifying. This air is charged fine sulfur, it enters a cyclone 6 where is the separation of the fine realities sulfur. The air escapes in the AT " mosphere by 11, while the fines are rseydées by 12 in the ferrule. The stirring device 5, enables each regular fluidization, and avoid renardageo, solidified accumulating at the bases of the bed portion, maie, 1 * agitation due, their segregation is not complete I a granule mixture and fine sulfur * in a ratio of approximately 50/50, is removed from the ferrule by 13 and supplied to the screening device 7. The fines are returned by sulfur in the cyclone 14 * 6 and recycled into the ferrule 1" a hopper 15 contains the sulfur powder ** for fresh hr supplying the fluidized bed, to replace the coating powder retained by the formed granules.

The figurte 2 to 5 represent different devices drop generators.

Fig. 2 shows in plan the perforated bottom of the annular tank 2; in this bottom holes 16 are preferably relaxed. Peppers circularly, and will not until the center of the bottom.

Fig. 3 is an axial cross section of a bulb 17

terminating at the bottom by a tube 18 drop generator.

This tube 18 is accompanied by a vibration generating device * compound of an electromagnet 22, 23 and a junction elastic metal parts 24 assujeties on the tube.

Figure 4 and 5 are views respectively in

plane and cross-section of a device consisting of an O-ring 19, dispensing drops of liquid plasticized molten * this liquid being supplied hr the annulus via tubes 21, 20 and 20".

In one embodiment of the apparatus according to practical strong fig. ii, the ferrule 1 has a diameter of 60 cm and a height of the cylindrical part of the tote îOOcm the j 2 is of a diameter of 50 cm, its ports 16 measure 0.8 mm in diameter and 4 are arranged in concentric circles whose outer circle is the diameter of 40 cm and the interior of 25 in. The "oufflerit 8 was provided for it can deliver 300 of Ra? / hr air * the agitator has an arm 17 of 50 cm length which can, optionally" be provided with blades 18.

The device according to Figure 6 provides an axial cross-sectional schematic of another system according to the invention.

The plasticized sulfur micropump is brought into a drop generator device 25 of the type described above (fig., 2 to 5)* the drops obtained, well separated, fall on a dust layer of sulfur from a hopper of the ALI " 26 their characteristics, and which covers a band 27 * tranepoxteuse said layer is slightly compacted by a special arrangement of the pouring device 33 32 sulfur, the thickness of said couehe is preferably between 10 to 30 seen the drop falls from a height very low, of the order of 100 th 150 * random access to at least a portion of the drop is in contact with said powder may optionally have * hr the upper portion of the web a scraping device (not shown), to stir said layer, thereby substantially completely coat the granules * separation of the powder takes place on the intend 28 placed in the recycle bin 29. The sulfur powder is returned via the conveyor belt 30 towards the txémis 26 * the rotary drum 31 has a double réle I-removing solidified drops the amounts the DS excess powder CD for distribution of the powder so that the larger portion of said granules are covered * further, said drum acts to break up the agglomerates DS of sulfur powder which may form aurafont * the granules obtained are bagged in 34 *

The following examples " non-limiting, are given

as LC ' illustrative only of the invention,

EXAMPLE 1

A plasticized mass sulfur, prepared according to one of the processes described in the above patents cited, colored with 0.5 kg of yellow pigment and loaded with 0.8 kg of finely powdered calcium carbonate, is maintained liquid f are divided into droplets having a mean dimension of about 2 mm. The drops fall, under their own weight, in the elemental sulfur powder (non-plasticized) fluidized by means of air

admitted to 18 °c at the bottom of a fluidizing chamber, to the speed Ooo

of 0.15 meters/dry. The fluidized bed has a density of deHcg

the COR m to sulfur. The particles of the powder sulfur have mean dimensions of 0.06 to 0.3 RANs. The drops pass through unqhautor of 0.5 meters of fluidized bed, and gather in the form of solid pellets - at the bottom of the chamber, from which they are discharged, under stirring, for screening them then, for separation of the excess powder.

The granules, thus obtained, have average sizes of between 1.5 to 3 DAB % lls have a pebbled surface layer, non-plasticized, forming about 3% of the weight of the granule. Their bagging is very easy, and there is not clumping in the bags, during transportation.

FOR EXAMPLE, 2,

In the chamber of the example 1, the same liquid drops fall rain to the leads rate, in counter-current with air to 18° with 0.15 m in the mimic the speed/dry * that in the example before, ** NAA May powder "oufse" amputation during the these conditions, at beats of the chamber, after having 1 meter "the drops are not solidified, they close a pasty mass at the bottom of the combustion chamber"

" bbbjl

Polyvinyl chloride, plasticized with dibutyl phthalate and 17% 13% phosphate trieresylic, is melted, maintained at 410% and distributed into the fine rain in a chamber covered by an air stream transversely & 2q * C., which takes 70 kg/m is suspended³ powder fine tape chlo "fluoride polyvinyl unplasticized, manufactured by the LS process known in emulsion" after a horizontal path of 3.70 meters, the seed and filaments of polyvinyl chloride, driven by the air stream, are collected hr the solid state, and separate of Ls excess powder which is recycled *

The seeds and filaments have a surface layer of unplasticized polyvinyl chloride|eonditionnables are easily, without gluing antrum them *

Of course, the invention is in no way limited to the described examples, it is likely many autrst variants accessible th to the ordinarily skilled artisan, depending on each particular application, and for example, the density of the fluidized bed can be very variable, without deviating from its spirit of this *