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emulsion polymerization method

An emulsion and polymer technology, applied in chemical instruments and methods, pharmaceutical formulations, detergent compositions, etc., can solve problems such as limiting the stability of emulsions

Active Publication Date: 2017-06-20
DOW SILICONES CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

US6235834B1 describes an emulsion polymerization, but uses a variety of specific anionic surfactants and the particle size must exceed 1 micron, which is not suitable for many applications because it limits the stability of the emulsion

Method used

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Examples

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example 1

[0066] First, to provide a composition comprising acid, base and starting polymer, 400 g of triethanolamine was added to a change-over mixer, followed by 400 g of Marlon AS3 (alkylbenzene sulfonic acid). The mixture was mixed gently with a spatula at 30 rpm. Then 150 g of distilled water were added under stirring (60 rpm). Then 4400 g of Me with a viscosity of about 50,000 mPa sec. (cP) and a number average molecular weight of about 64,000 were added 2 SiOH terminated dimethylpolysiloxane. The mixture was stirred at 3500 rpm for 20 minutes. A thick oil-in-water emulsion is obtained. 2548 g of dilution water are then poured slowly. The masterbatch emulsion had an average particle size of 0.233 microns.

[0067] 545 g of this masterbatch emulsion were further diluted with 202 g of water in a 1 liter double wall glass reactor. The temperature was lowered until 21 °C and to start the emulsion polymerization, 92.8 g of 10% sulfuric acid were added under stirring (500 rpm) ove...

example 2

[0069] First, to provide a composition comprising acid, base and starting polymer, 402 g of triethanolamine was added to the change-over mixer, followed by 464 g of Marlon AS3 (alkylbenzene sulfonic acid). The mixture was mixed gently with a spatula at 30 rpm. Then 150 g of distilled water were added under stirring (60 rpm). Then 4400 g of Me with a viscosity of about 14,000 mPa sec. (cP) and a number average molecular weight of about 44,000 were added 2 SiOH terminated dimethylpolysiloxane. The mixture was stirred at 3500 rpm for 20 minutes. A thick oil-in-water emulsion is obtained. Then slowly pour 2550 g of dilution water. The masterbatch emulsion had an average particle size of 0.196 microns.

[0070] 652 g of this masterbatch emulsion was further diluted with 101.2 g of water in a 1 liter double wall glass reactor. The temperature was lowered until 21 °C and to start the emulsion polymerization, 99.8 grams of 10% sulfuric acid were added under stirring (500 rpm) ov...

example 3

[0072]First, to provide a composition comprising acid, base and starting polymer, 400 g of triethanolamine was added to a change-over mixer, followed by 464 g of Marlon AS3 (alkylbenzene sulfonic acid). The mixture was mixed gently with a spatula at 30 rpm. Then 150 g of distilled water were added under stirring (60 rpm). Then 4400 g of Me with a viscosity of about 5,000 mPa sec. (cP) and a number average molecular weight of about 33,000 were added 2 SiOH terminated dimethylpolysiloxane. The mixture was stirred at 3500 rpm for 35 minutes. A thick oil-in-water emulsion is obtained. Then slowly pour 2550 g of dilution water. The masterbatch emulsion had an average particle size of 0.200 microns.

[0073] 700.1 g of this masterbatch emulsion was further diluted with 100.2 g of water in a 1 liter double-walled glass reactor. The temperature was lowered until 21 °C and to start the emulsion polymerization, 97.6 grams of 10% sulfuric acid were added under stirring (500 rpm) ov...

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Abstract

The present invention relates to a process for preparing silicone-in-water emulsions by emulsion polymerization. The emulsion contains particles of an organopolysiloxane polymer having an average particle size of less than 1 μm. The method comprises: -combining a silanol-terminated organosiloxane starting polymer, water and a surfactant; the starting polymer has a viscosity of at least 2 Pa.s, preferably at least 2.5 Pa.s, preferably at least 3.5 Pa.s, preferably at least 4 Pa.s and up to 150 Pa.s; - emulsifying the starting polymer by agitating or shearing the ingredients; - polymerizing the starting polymer to form longer A chained silanol-terminated organopolysiloxane polymer; wherein at least a part of said polymerizing step is carried out at a temperature lower than or equal to 16°C, preferably lower than or equal to 15°C.

Description

technical field [0001] The present invention relates to a process for preparing silicone-in-water emulsions by emulsion polymerization. Background technique [0002] Silicone-in-water emulsions can traditionally be prepared by mechanical emulsification of silicone or by emulsion polymerization. Typically, mechanical emulsification is used when relatively low viscosity silicones need to be emulsified. Of course, beyond a certain viscosity (600 Pa.s), silicones can no longer be emulsified using conventional mixers without the particle size becoming too high. [0003] Therefore, in order to prepare emulsions with high-viscosity silicones, polymerization is necessary. [0004] Various cyclosiloxanes including octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5) are widely used as monomers because of their cost-effectiveness and availability in large quantities. However, ring-opening polymerization of cyclosiloxanes is not complete and sometimes leaves large am...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K8/89C08J3/03C08L83/04
CPCA61K8/062A61K8/891A61K2800/21A61Q5/02A61Q5/12A61Q19/00C08G77/16C08J3/03C08J2383/04C08L83/04A61K8/89C08G77/06A61K8/06A61Q19/10C08J3/05C11D17/0021
Inventor 塞维林·科万B·万罗伊本诺特·拉沙特阿尔贝托·彼得罗西诺索菲·汉森斯
Owner DOW SILICONES CORP
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