US5763505A — Process for the preparation of aqueous emulsions …

Claim 1

Independent Claim 285 words

A process for the preparation of an aqueous emulsion of organopolysiloxane selected from the group consisting of silicone oils, gums, resins and mixtures thereof, consisting essentially of the step of kneading a mixture comprising (i) 100 parts by weight of a silicone phase having a dynamic viscosity at 25° C. at least equal to 3 Pa·s or having a consistency expressed in tenths of a millimeter per minute, as measured by a penetrometer at 25° C., of less than 2000, said silicone phase comprising at least one polyorganosiloxane oil, gum, resin or mixture thereof; (ii) 2 to 20 parts by weight of water; and (iii) either 3 to 20 parts by weight of one or more surface-active agents or a combination of 0.5 to 10 parts by weight of at least one surface-active agent and 2.5×10 -4 to 20 parts by weight of at least one water-soluble thickening polymer having a mass greater than 10,000 g/mol, wherein said one or more surface-active agents have an HLB value of at least 10 and the relative amounts of components (ii) and (iii) are such that the viscosity or the consistency of said mixture of components (ii) and (iii) is greater than about one-tenth of the viscosity or consistency of said silicone phase (i); wherein said entire kneading step is carried out for a period of time in a mixer equipped with one or more stirrers in which the moving part of said one or more stirrers does not rotate at more than 500 revolutions/min with a tangential speed at the end of the moving part not exceeding 2.5 m/s, wherein said entire kneading step produces an oil-in-water emulsion having a particle size of 0.1 to 5 micrometers.

Claim 2

Dependent Claim 285 words

A process for the preparation of an aqueous emulsion of organopolysiloxane selected from the group consisting of silicone oils, gums, resins and mixtures thereof, consisting essentially of the step of kneading a mixture comprising (i) 100 parts by weight of a silicone phase having a dynamic viscosity at 25° C. at least equal to 3 Pa·s or having a consistency expressed in tenths of a millimeter per minute, as measured by a penetrometer at 25° C., of less than 2000, said silicone phase comprising at least one polyorganosiloxane oil, gum, resin or mixture thereof; (ii) 2 to 20 parts by weight of water; and (iii) either 3 to 20 parts by weight of one or more surface-active agents or a combination of 0.5 to 10 parts by weight of at least one surface-active agent and 2.5×10 -4 to 20 parts by weight of at least one water-soluble thickening polymer having a mass greater than 10,000 g/mol, wherein said one or more surface-active agents have an HLB value of at least 10 and the relative amounts of components (ii) and (iii) are such that the viscosity or the consistency of said mixture of components (ii) and (iii) is greater than about one-tenth of the viscosity or consistency of said silicone phase (i); wherein said entire kneading step is carried out for a period of time in a mixer equipped with one or more stirrers in which the moving part of said one or more stirrers does not rotate at more than 500 revolutions/min with a tangential speed at the end of the moving part not exceeding 2.5 m/s, wherein said entire kneading step produces an oil-in-water emulsion having a particle size of 0.1 to 5 micrometers.

Claim 3

Dependent Claim 65 words

Process according to claim 1 wherein the silicone phase (A) is selected from the group consisting of polyorganosiloxane oils, gums, resins, mixtures thereof, and mixtures of said polyorganosiloxanes with at least one solvent of said oil, gum or resin, with at least one silane, or with at least one siliceous or non-siliceous filler, which silicone phase has a viscosity at least equal to 3 Pa·s.

Claim 4

Dependent Claim 71 words

Process according to claim 2, wherein the silicone phase (A) is selected from the group consisting of polyorganosiloxane oils, gums, resins, mixtures thereof, and mixtures of said polyorganosiloxanes with at least one solvent of said oil, gum, or resin, with at least one silane, or with at least one siliceous or non-siliceous filler, which silicone phase has a viscosity of 30 to 2,500 Pa·s or a consistency of 200 to 2,000.

Claim 5

Dependent Claim 158 words

Process according to claim 1 wherein the polyorganosiloxane oils and gums comprise units of formula R'.sub.3-a R.sub.a SiO.sub.1/2 and R.sub.2 SiO wherein a is an integer from 0 to 3; the R radicals are identical or different and represent a saturated or unsaturated aliphatic hydrocarbon group containing from 1 to 10 carbon atoms; an aromatic hydrocarbon group containing from 6 to 13 carbon atoms; a polar organic group bonded to the silicon by an Si--C or Si--O--C bond; or a hydrogen atom; and the R' radicals are identical or different and represent an OH group; an alkoxy or alkenyloxy group containing from 1 to 10 carbon atoms; an aryloxy group containing from 6 to 13 carbon atoms; an acyloxy group containing from 1 to 13 carbon atoms; a ketiminoxy group containing from 1 to 8 carbon atoms; or an amino- or amidofunctional group containing from 1 to 6 carbon atoms, bonded to the silicon by an Si--N bond.

Claim 6

Dependent Claim 20 words

Process according to claim 4 wherein at least 80% of the R radicals of said oils represent a methyl group.

Claim 7

Dependent Claim 173 words

Process according to claim 1 wherein the polyorganosiloxane resins comprise units of formulae RSiO.sub.3/2 (T unit) and/or SiO.sub.2 (Q unit) in combination with units of formula R'.sub.3-a R.sub.a SiO.sub.1/2 (M unit) and/or R.sub.2 SiO (D unit) wherein a is an integer from 0 to 3; the R radicals are identical or different and represent: a saturated or unsaturated aliphatic hydrocarbon group containing from 1 to 10 carbon atoms; an aromatic hydrocarbon group containing from 6 to 13 carbon atoms; a polar organic group bonded to the silicon by an Si--C or Si--O--C bond; or a hydrogen atom; and the R' radicals are identical or different and represent an OH group; an alkoxy group or alkenyloxy group containing from 1 to 10 carbon atoms; an aryloxy group containing from 6 to 13 carbon atoms; an acyloxy group containing from 1 to 13 carbon atoms; a ketiminoxy group containing from 1 to 8 carbon atoms; or an amino-or amidofunctional group containing from 1 to 6 carbon atoms, bonded to the silicon by an Si--N bond.

Claim 8

Dependent Claim 227 words

Process according to claim 2 wherein the silane is a by-product from the synthesis of said polyorganosiloxane oils, gums or resins and is present in an amount of 0 to 10 parts by weight per 100 parts by weight of said: polyorganosiloxane oil(s), gum(s), or resin(s), or is a crosslinking agent of said oils, gums or resins and is present in amounts of 0.5 to 30 parts by weight per 100 parts by weight of said oil(s), gum(s), or resin(s), said silane having the formula (R b )Si(OR') 4-b , wherein b is an integer from 0 to 4, the R radicals are identical or different and represent: a saturated or unsaturated aliphatic hydrocarbon group containing from 1 to 10 carbon atoms; an aromatic hydrocarbon group containing from 6 to 13 carbon atoms; a polar organic group bonded to the silicon by an Si--C or Si--O--C bond; or a hydrogen atom; and the R' radicals are identical or different and represent an OH group; an alkoxy group or alkenyloxy group containing from 1 to 10 carbon atoms; an aryloxy group containing from 6 to 13 carbon atoms; an acyloxy group containing from 1 to 13 carbon atoms; a ketiminoxy group containing from 1 to 8 carbon atoms; or an amino-or amidofunctional group containing from 1 to 6 carbon atoms, bonded to the silicon by an Si--N bond

Claim 9

Dependent Claim 30 words

Process according to claim 2 wherein said silane is an aminopropyltriethoxysilane, aminopropylmethyldiethoxysilane or glycidoxypropyltrimethoxysilane, present in an amount to 200% of the weight of said oil(s), gum(s), or resin(s) present.

Claim 10

Dependent Claim 44 words

Process according to claim 2 wherein the siliceous or non-siliceous fillers are reinforcing or semi-reinforcing fillers having a particle size of 0.001 to 300 μm and are present in an amount up to 300% of the weight of said oil(s), gum(s), or resin(s) present.

Claim 11

Dependent Claim 24 words

Process according to claim 1 wherein the surface-active agents are non-ionic, anionic, cationic, zwitterionic or amphoteric, and have an HLB value greater than 10.

Claim 12

Dependent Claim 51 words

Process according to claim 1 wherein component (iii) comprises a combination of at least one surface-active agent and at least one water-soluble thickening polymer selected from the group consisting of poly(vinyl alcohol)s, poly(ethylene glycol)s, polyvinylpyrrolidones, alkali metal polyacrylates, carrageenans, alginates, xanthan gum, carboxymethyl celluloses, methyl celluloses, hydroxypropyl celluloses and hydroxyethyl celluloses.

Claim 13

Dependent Claim 47 words

Process according to claim 1 wherein the silicone phase is emulsified by introducing at least one oil, gums, and or resin into a mixture of water, surface-active agent(s), and optionally, a water-soluble polymer(s) and then kneading the resulting admixture at a temperature from 10° to 50° C.

Claim 14

Dependent Claim 59 words

Process according to claim 2 wherein the silicone phase is emulsified by introducing at least one oil, gum, or resin+optional solvent(s)+optional silane(s) into a water+surface-active agent(s)+optional water-soluble polymer mixture, the optional filler(s) being present in the aqueous mixture or introduced into said aqueous mixture, and then kneading the resulting admixture at a temperature of from 10° to 50° C.

Claim 15

Dependent Claim 37 words

Process according to claim 1 wherein said kneading is carried out in a single- or multiple-screw extruder, a planetary mixer, a hook mixer, a slow disperser, a static mixer or a paddle, propeller, arm or anchor mixer.

Claim 16

Dependent Claim 93 words

The process according to claim 1 wherein component (i) has a dynamic viscosity at 25° C. of at least equal to 30 Pa·s, component (ii) comprises between 3 to 15 parts by weight water and component (iii) comprises either 5 to 15 parts of one or more surface-active agents or 1 to 10 parts by weight of a surface-active agent and 0.001 to 15 parts by weight of a thickening polymer having a molecular mass greater than 100,000; the process yielding an emulsion having a particle size of from 0.2 to 3 micrometers.

Claim 17

Dependent Claim 27 words

The process according to claim 1 wherein component (iii) comprises one or more surface-active agents and wherein said entire kneading step consists essentially of one mixing step.

Claim 18

Dependent Claim 17 words

The process according to claim 1 comprising the additional step of diluting the resulting emulsion in water.

Claim 19

Dependent Claim 29 words

The process according to claim 1 wherein component (iii) comprises one or more surface-active agents and wherein the weight ratio of (ii) to (ii)+(iii) is between 0.2 to 0.7.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	2001-06-08	2001-12-08	2002-06-09	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	2005-06-08	2005-12-08	2006-06-09	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2009-06-08	2009-12-08	2010-06-09	$7700.00	Window Closed / Lapsed

Process for the preparation of aqueous emulsions of silicon oils and/or gums and/or resins

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