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United States Patent (19) 11 Patent Number: 4,824,877 Glover Et Al

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United States Patent (19) 11 Patent Number: 4,824,877 Glover Et Al United States Patent (19) 11 Patent Number: 4,824,877 Glover et al. (45) Date of Patent: Apr. 25, 1989 54 HIGH POLYMER CONTENT SILICONE 4,244,849 1/1981 Saam ................................... 525/477 EMULSIONS 4,620,878 11/1986 Gee ..................................... 252/312 75 Inventors: Shedric O. Glover; Daniel Graiver, OTHER PUBLICATIONS both of Midland, Mich. U.S. Patent Application Ser. No. 809,090. 73) Assignee: Dow Corning Corporation, Midland, Primary Examiner-Morton Foelak Mich. Attorney, Agent, or Firm-Edward C. Elliott (21) Appl. No.: 151,686 57 ABSTRACT 22) Filed: Feb. 2, 1988 A polydiorganosiloxane emulsion having a combination (51) Int. Cl." .............................................. C08L 53/04 of high polymer content and low viscosity can be pro (52) ... 523/221; 524/588 duced by blending a high polymer content polydiorgan (58) Field of Search ......................... 523/221; 528/588 osiloxane macroemulsion, having a polymer content of greater than 60 percent by weight and an average parti 56 References Cited cle size of greater than 0.14 micrometers, and a high U.S. PATENT DOCUMENTS polymer content polydiorganosiloxane microemulsion, 3,294,725 12/1966 Findlay et al. ..................... 260/29.2 having a polymer content of from 20 to 30 percent by 3,433,780 3/1969 Cekada et al. .. ... 260/29.2 weight and an average particle size of less than 0.14 3,975,294 8/1976 Dumoulin ....... ... 252/354 micrometers, with the ratio of the average particle size 4,052,331 10/1977 Dumoulin ... ... 252/312 of the macroemulsion to the average size of the micro 4,146,499 3/1979 Rosano ............ ... 252/186 emulsion of from 5 to 15. 4,221,688 9/1890 Johnson et al. ... 525/19 4,244,844 1/1981 Molinier et al. ... ... 428/39 4. Claims, No Drawings 4,824,877 1. 2 ganosiloxane microemulsion having a high polymer HIGH POLYMER CONTENT SILICONE content. EMULSIONS DESCRIPTION OF THE INVENTION BACKGROUND OF THE INVENTION 5 This invention relates to a method of producing a 1. Field of the Invention polydiorganosiloxane emulsion having a high polymer This invention relates to the use of silicone micro content of greater than 40 percent by weight and a emulsions in conjunction with silicone macroemulsions relatively low viscosity of less than 25 Pa.s at 25 C. to produce high polymer content emulsions of lower comprising. mixing 100 parts by weight of a high poly than normal viscosity. 10 mer content polydiorganosiloxane macroemulsion hav 2. Background Information ing a polymer content of greater than 60 percent by Findley and Weyenberg developed methods of form weight and particle diameters greater than 0.14 micron ing stable polymeric emulsions from siloxane oligomers. eters with from 1 to 70 parts by weight of a high poly Their methods are taught in U.S. Pat. No. 3,294,725. mer content polydiorganosiloxane microemulsion hav issued Dec. 27, 1966. 15 ing a polymer content of from 20 to 30 percent by Johnson et al. developed a silicone emulsion which weight and particle diameters less than 0.14 microme gave an elastomeric product upon removal of the water, ters, with the ratio of the average particles size of the as shown in U.S. Pat. No. 4,221,688, issued Sept. 9, 1980. The dispersed phase comprised an anionically macroemulsion to the average particle size of the micro stabilized hydroxylated polydiorganosiloxane and a 20 emulsion being from 5 to 15 and the particle size distri colloidal silica. bution of each of the parent emulsions being broad. Another aqueous silicone emulsion is described in A high polymer content polydiorganosiloxane mac U.S. Pat. No. 4,244,849, issued Jan. 13, 1981, which roemulsion is defined as one in which the polymer phase provides an elastomeric product upon removal of the of the emulsion comprises greater than 60 percent by water under ambient conditions. The dispersed phase is 25 weight of the total weight of the emulsion. The emul a graft copolymer of a hydroxyl endblocked polydior sion has a high viscosity under zero shear, such as a ganosiloxane and an alkali metal silicate. viscosity of greater than 25 Pa.s at 25 C. An emulsion Emulsions having particle sizes in the range of below having a viscosity of greater than 25 Pa.s is such that it 0.1 micrometers (1000 Angstroms) have been devel becomes difficult to work with in normal plant mixing oped. 30 equipment such as stirred mixing kettles and in pumping Cekada and Weyenberg prepared colloidal suspen through pipes during transfer of the emulsion to other sions of silisesquioxanes by adding silane to a water-sur processing equipment or to storage containers. The factant mixture with agitation, at a slow rate as de preferred polymer content is from 60 to 80 percent by scribed in U.S. Pat, No. 3,433,780, issued Mar. 18, 1969. weight. A macroemulsion is one that has particles A surface active composition which may be used as 35 which scatter appreciable amounts of light. The aver an emulsifier with diorganopolysiloxanes to form trans age diameter of the emulsion particles exceeds 0.14 parent microemulsions or transparent gels is described micrometers. Preferably the particles exceed diameters in U.S. Pat. No. 3,975,294, issued Aug. 17, 1976 and in of greater than 0.25 micrometers with a preferred range U.S. Pat. No. 4,052,331, issued Oct. 4, 1977. of 0.25 to 0.5 micrometers. The high polymer content A unique method for the preparation of oil-in-water polydiorganosiloxane macroemulsion can be prepared microemulsions is described in U.S. Pat. No. 4,146,499, by any of the methods known. Examples of macroemul issued Mar. 27, 1979. The four step process uses two sions are found in U.S. Pat. Nos. 3,294,725, 4,221,688, different surfactants which are selected based upon 4,244,844, and 4,244,849, all of which are hereby incor their solubility in the oil phase and in the water phase. porated by reference to show polydiorganosiloxane A method of preparing polyorganosiloxane emul 45 macroemulsions and means for their preparation. sions having small particle size is taught in U.S. Pat. No. The high polymer content polydiorganosiloxane 4,620,878, issued Nov. 4, 1986. A translucent oil concen macroemulsion is preferably prepared by following the trate is prepared by mixing a polar group containing method found in U.S. Pat. No. 3,294,725. An organosi polyorganosiloxane, surfactant and water. The concen loxane is polymerized while in the dispersed state in an trate is then rapidly dispersed in water to form a micro 50 aqueous medium in the presence of a surface active emulsion with an average particle size of less than 0.14 sulfonic acid. The siloxane and surface active sulfonic micrometers. acid catalyst are dispersed in water to form a stable Graiver and Tanaka developed methods of making emulsion. The emulsion is then allowed to stand with or stable silicone microemulsions by emulsion polymeriza without agitation at the desired temperature until the tion. Their methods are taught in U.S. application Ser. 55 siloxane has reached the desired state of molecular ag No. 809,090, filed Dec. 12, 1985. gregation. In any of these methods, as the solids content of the A high polymer content polydiorganosiloxane micro emulsion is raised, the viscosity of the emulsion rises. emulsion is an emulsion having from 20 to 30 percent by For applications which require a flowable emulsion, the weight polymer phase based upon the total weight of rise in viscosity limits the polymer content which can be the emulsion. The emulsion particles do not exceed achieved. diameters of 0.14 micrometers. Preferred are emulsions having particle diameters of less than 0.1 micrometers, SUMMARY OF THE INVENTION with diameters of less than 0.05 micrometers most pre An emulsion of polydiorganosiloxane having a high ferred. polymer content and yet a relatively low viscosity is 65 The high polymer content polydiorganosiloxane mi produced by blending 100 parts by weight of a polydi croemulsion can be prepared by following the methods organosiloxane macroemulsion having a high polymer found in U.S. Pat. Nos. 3,433,780, 3,975,294, 4,052,331, content with from 1 to 70 parts by weight of a polydior 4,146,499, and 4,620,878, all of which are hereby incor 4,824,877 3 4. porated by reference to show methods of producing will flow out to a smooth surface, yet give a good coat microemulsions and the microemulsions. ing because of the high polymer content. By the addi A microemulsion of polydiorganosiloxane may be tion of fillers, it is possible to produce emulsions having prepared by sequentially adding precursor emulsion a viscosity like a paste for use as sealants which can be comprised of cyclopolydiorganosiloxane, surfactant, 5 extruded from a storage tube and yet have very little and water to a polymerization medium comprised of shrinkage on drying because of the high polymer con water and an effective amount of a polymerization cata tent; i.e. low volatility content. lyst, while mixing, wherein the rate of addition of the The method of this invention enables a manufacturer precursor emulsion is effective to form a clear, stable to use high polymer content, high viscosity macroemul microemulsion which has polydiorganosiloxane drop-10 sions in a plant in a practical manner. For example, by lets of less than 0.14 micrometer in diameter, and which putting a microemulsion, having a viscosity of less than contains a surfactant to polydiorganosiloxane weight 25 Pa.s for example, into a mixing kettle first and then ratio of 0.15 to 0.65.
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