Oct. 29, 1946. E; o. sowERwmE, JR 2,410,315 APPARATUS FOR PREPARING FORMED GELS ‘ Filed May 20, 1945 BY @MW A TTURN 2,410,315 Patented Oct. 29, 1946 ‘UNITED ‘STATES PATENT OFFICE ‘Elbert '0. Sowerivine, Jr., Woodbury,"_N. J., as Socony-Vacuum Oil-Company, Incor a corporation of New York Application May 20, 1943,‘ Serial No. 487,715 (01.252-359) 2 iMy invention contemplates the provision "of This invention relates to apparatus "for'pre novel means for inhibiting gelation on or in the 2 Claims. -1 paring and dividing an aqueous colloidal solution capable of setting to a gel or similar solid'or' semi solid condition. More particularly, the inven tion contemplates the formation and subdivision means for providing streams of sol supplied to of an aqueous $01 which sets'to form a hydrogel bination of mixer and divider. In the'drawing: comprising inorganic oxides in ‘the solid phase. In thecopending applica'tion'Serial No. 461.454, ?led October 9, 194%, by Milton M. Marisic, which a body of liquid immiscible with the'sol. ‘In the accompanying drawing are shown a novel mixing nozzle, a novel divider and a novel com Figure l‘is a diagrammatic showing of a typical apparatus according to my invention; "Figure'Z is a‘ view in vertical section of a mix issued as Patent No. 2,385,217, on ‘September 18, 10 ing nozzle according to my invention; 7 1945, a process is described for forming hard, "Figure 3‘ is ‘a'sectional view of one form of spheroidal beads of ‘inorganic oxides by iniecting divider‘ contemplated by the invention; and t solutions which will ‘gel in a predetermined time Figure it is a view'in‘ partial section of another into a liquid immiscible therewith and permitting form of divider contemplated by theinvention. gelation of ‘resultant globules of the solution in 15 Brie?y, the inventionprovides for} inhibiting the immiscible liquid. The resultant globules of hydrogel are then removed and processed to form the desired ?nal product. 'I-noperation of suchprocesses, difficulties arise due to gelation of small portions of. the solution 20 within the mixing nozzle formingideposits of gel which gradually build up. ‘In the said Marisic application, it is proposed» to- avoid this di?iculty gelation'in the mixing nozzle by'heating the'walls thereof to a‘temperature above ‘the boiling point of the sol to thereby ‘cause vaporization along the walls and provide a ‘protective'vapor layer which prevents gelation'onthe walls. The divider is provided with a surface layer of a solid ‘hav ing a melting point‘below the tem‘peratureofthe ‘sol discharged ‘from the mixing nozzle. ‘The ' sol by means of a‘rota'ry' cleaning member within the falling on the divider melts this surface during nozzle. Deposits can also be avoided by high 25 operation and thus provides a continuously re velocity ?ow within the nozzle. The ?rst means newed surface and any gel which forms there includes a moving member within the nozzle on is carried away by the flow of the sol.> Ac which occupies space and requires packing at the cording to one modi?cation of the invention, the bearings; while high velocity flow impairs the divider is provided with heat exchange means capacity of the device to produce uniformly sized 30 whereby a coating of ice may be built up there globules. on by freezing of water in the sol during one phase A divider for increasing the practicable capac of the operation and melted during another phase, ity of a single mixing nozzle is described in appli thus continuously changing the surface without cation Serial No. 477,168, ?led February 25, 1943, replacement of the divider at the termination of by John W. Payne, Edmund L. Sargent and Henry 35 each melting step. G. Daley. According to the disclosure of the Thetime required for gelation of the sol is de latter application, the stream of aqueous sol pendent upon the temperature of the sol, gela issuing from a mixing nozzle is projected onto tion time decreasing with increase in tempera a downwardly sloping surface so formed as to ture. When using the combination shown in Fig divide the stream into a plurality of smaller 40 ure 1, the sol will be heated as formed in the streams. A typical and preferred form of divider mixing nozzle and subsequently cooled on the is conical in shape and provided with grooves divider and a balance of these factors must be down the sides from the apex. Provision is made made with other variables affecting gelation time, to discharge the stream of aqueous sol onto the for example acidity and concentration‘ of the sol. apex of the cone whereby it is divided into a plu 45 It may be noted that gelation time is decreased rality of smaller streams, each of which is of by increasing either pH or concentration. a size to give the desired subdivision of the sol. Referring speci?cally to Figure 1, a vessel 10 By this means a single nozzle may be used to pro encloses a column of liquid immiscible with the vide many streams, thus greatly reducing the sol, for example, mineral oil. Below the column of number of nozzles required, each of which must 50 oil is a relatively shallow layer of water which be ?tted with at least two metering pumps, or is caused to flow by admitting fresh water at H other suitable controls. In the said application, and withdrawing water containing spheroidal gel the conical divider is described as having a sur globules by pipe i2. Two solutions which will re face not wetted by the aqueous sol, thus prevent act to form the desired sol are admitted to a 55 ing adherence and gelling of the sol on the divider. 2,410,315 mixing nozzle l3 by pipes I4 and [5 from meter A metallic base 26, which may include heat ex ing pumps l6 and I1. change tubes as shown in Figure 3, is covered by The mixing nozzle I3 is constructed in such a layer 21 of a meltable substance such as ice. A manner that heat may be applied to the inner plurality of grooves 28 in the top surface pro walls thereof, as by a heat exchange medium or vide paths for the small streams desired. The direct heating means. In the embodiment of Fig grooves are not essential but do give considerably ure 2, heat is supplied by an electric heating coil smoother operation in dividing the sol. If heat l8 embedded in an outer layer l9 of insulating exchange means are included, circulation of a material. Current is supplied to the coil l8 by leads 2B. The heating coil is adjacent to but in 10 ?uid therethrough can be used to control melt ing away of the surface. In operations using the sulated from a liner 2| which may advanta embodiment of Figure 3, which is also prefer geously be metallic. It will be apparent that so ably grooved, a refrigerant may be circulated lutions admitted by inlet pipes l4 and I5 will be through tubes 25 until a substantial layer of ice rapidly and completely mixed inside the nozzle is built up by freezing out water from the sol, while the hot liner will cause a minor amount of whereupon the refrigerant ?ow is discontinued or vapor to be generated which forms a protective a ?uid of different temperature is circulated, per blanket between the liner and the contents of the mitting melting of the ice. nozzle. Due to the short period of residence of The surface coating of divider 22 should, in the aqueous ?uid in the nozzle, the amount of general, have a melting point below about 100° F. vaporization relative to the total ?uid is slight 20 I claim: and the rise in temperature of the liquid is- only 1. In a device for dividing a stream of a gel a few degrees. able sol into a plurality of smaller streams, a Upon discharge from the nozzle, the sol falls on divider of generally conical shape, means to the apex of a divider 22 which is adapted to split maintain said divider in position with the apex the stream of sol into a plurality of smaller streams. Any type of sloping surface may be used , thereof directed upwardly, the outer surface of said divider having a plurality of grooves extend for this purpose, but best results are to be ob ing down the surface thereof from about the tained by using a conical divider having a plu apex, said grooves being coated with a layer of rality of grooves down its surface from the apex. ice, and means to discharge a stream of gelable sol The divider is supported from the wall of vessel onto the apex of said divider. H] as shown. In the embodiment illustrated, the 2. In a device for dividing a stream of a gel support includes pipes 23 and 24 for circulation able sol into a plurality of smaller streams, a of a heat exchange medium to and from divider divider of generally conical shape, means to main 22. ' tain said divider in position with the apex there -A divider provided with means for conducting a heat exchange medium in heat exchange rela 35 of directed upwardly, the outer surface of said divider having a plurality of grooves extending tionship with the surface of the divider is shown down the surface thereof from about the apex, in Figure 3. Tubes 25 from the heat exchange said grooves being coated with a layer of ice, medium are formed in the divider itself whereby means to conduct a heat transfer ?uid in indirect the surface of the divider may be cooled or heated. ‘In Figure 4 is shown a divider having a sur 40 heat exchange relationship with said surface, and means to discharge a stream of gelable sol onto face formed of a substance which melts at a tem the apex of said divider. perature below that of the sol supplied thereto. ELBERT O. SOWERWINE, JR.