CN102558559A - Method of synthetizing small molecule hydroxyl silicone oil through using continuation method - Google Patents
Method of synthetizing small molecule hydroxyl silicone oil through using continuation method Download PDFInfo
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Abstract
The invention relates to a method of synthetizing small molecule hydroxyl silicone oil through using a continuation method. The method comprises the steps as follows: adding the1,000 g of hexamethyl cyclotrisiloxane, 1,400 g of acetone and 120 g of water into a 3,000 ml four-mouth bottle with the stirring function, heating and keeping the temperature to 40 DEG C to 60 DEG C, melting and mixing uniformly; adopting a peristaltic pump to continuously pass through two fixed beds added with 100 g of strongly acidic styrene cation exchange resin, wherein the strongly acidic styrene cation exchange resin comprises a macroporous type and a gel type, and has the following grades: 732, D001, KY-2 and KY-23; obtaining a small molecule hydroxyl silicone oil crude product after the each fixed bed reaction temperature is 40 DEG C to 60 DEG C and the retention time is controlled to 30-70 seconds; and obtaining small molecule hydroxyl silicone oil after the crude product is subject to normal pressure desolvation, decompression and removal of low component. The method has the advantages of continuation production, high reproducibility and high product yield; and moreover, the product is colorless transparent liquid from the appearance, the viscosity is 15-30 mm2/s, and the hydroxyl content is in the range of 6-10%.
Description
Technical field
The present invention relates to a kind of method of synthesizing small molecular hydroxy silicon oil, especially a kind of method of continuous processing synthesizing small molecular hydroxy silicon oil.
Background technology
Micromolecular hydroxyl silicone oil is the material that has the reactive group hydroxyl, is Zylox ideal constitution controller.The method for preparing micromolecular hydroxyl silicone oil has multiple, and suitability for industrialized production is used more be D4 (DMC) and acetic anhydride at present, but product has the acetic acid taste.
Summary of the invention
The present invention provides a kind of method of continuous processing synthesizing small molecular hydroxy silicon oil, with the by product D that obtains in the production of organosilicon methyl cyclosiloxane
3Be raw material, make hydroxy silicon oil, the digestion by product, the added value of raising by product, yield is high, and product can be used by oneself or export trade.
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil; Hexamethyl cyclotrisiloxane 1000 grams, acetone 1400 grams, water 120 grams are joined in the 3000ml four-hole bottle of band stirring; Heating up also keeps 40-60 ℃, dissolve mix after, adopt peristaltic pump continuously through 2 fixed beds that are added with 100 gram strongly acidic styrene type cation exchange resins; 40-60 ℃ of each fixed bed reaction temperature, the residence time are controlled at 30-70 second; Obtain the thick product of micromolecular hydroxyl silicone oil, reducing pressure behind the thick frequent pressure-off solvent of product removes low component again, obtains micromolecular hydroxyl silicone oil.
Wherein strongly acidic styrene type cation exchange resin comprises macroporous type and gel-type, comprises the following trade mark: 732, and D001, KY-2, KY-23.
The inventive method is raw material with the hexamethyl cyclotrisiloxane, and technology can serialization production, good reproducibility; Product yield is high, and stability in storage is better, and the shelf lives can reach more than 6 months, and product appearance is a colourless transparent liquid, and viscosity is at 15-30mm
2/ s, hydroxy radical content is between 6-10%; Technology does not have " three wastes " pollution in the production process, and solvent and low-boiling-point substance can be recycled, but industrialized production.
After stability was embodied in 6 months shelf liveves, product appearance is colourless transparent liquid, and was not stratified, after 6 months shelf liveves hydroxy radical content measure with the shelf lives before compare to descend and be no more than 5%.
Embodiment
Embodiment 1:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil joins hexamethyl cyclotrisiloxane 1000 gram, acetone 1400 grams, water 120 grams in the 3000ml four-hole bottle that band stirs, and heats up and keeps 50 ℃; Dissolve mix after, adopt peristaltic pump continuously through the fixed bed of 100 gram D001 strong-acid ion exchange resins and the fixed bed of 100 gram KY-23 strong-acid ion exchange resins, 50 ℃ of each fixed bed reaction temperature, the residence time were controlled at 50 seconds; Obtain the thick product of micromolecular hydroxyl silicone oil; Reduce pressure again behind the thick frequent pressure-off solvent of product and remove low component, obtain micromolecular hydroxyl silicone oil, viscosity 22CS; Hydroxy radical content 9%, yield 94.6%.
After stability was embodied in 6 months shelf liveves, product appearance is colourless transparent liquid, and was not stratified, after 6 months shelf liveves hydroxy radical content measure with the shelf lives before compare to descend and be no more than 2%.
Embodiment 2:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil joins hexamethyl cyclotrisiloxane 1000 gram, acetone 1400 grams, water 120 grams in the 3000ml four-hole bottle that band stirs, and heats up and keeps 40 ℃; Dissolve mix after, adopt the peristaltic pump fixed bed through being added with 100 grams, 732 ion exchange resin and the fixed bed of 100 gram KY-2 ion exchange resin continuously, 40 ℃ of each fixed bed reaction temperature, the residence time were controlled at 30 seconds; Obtain the thick product of micromolecular hydroxyl silicone oil; Reduce pressure again behind the thick frequent pressure-off solvent of product and remove low component, obtain micromolecular hydroxyl silicone oil, viscosity 24CS; Hydroxy radical content 8%, yield 90.1%.
After stability was embodied in 6 months shelf liveves, product appearance is colourless transparent liquid, and was not stratified, after 6 months shelf liveves hydroxy radical content measure with the shelf lives before compare to descend and be no more than 5%.
Embodiment 3:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil joins hexamethyl cyclotrisiloxane 1000 gram, acetone 1400 grams, water 120 grams in the 3000ml four-hole bottle that band stirs, and heats up and keeps 60 ℃; Dissolve mix after, adopt peristaltic pump to be added with the fixed bed of 100 gram D001 strong-acid ion exchange resins and the fixed bed of 100 gram KY-2 ion exchange resin through 2 continuously, 60 ℃ of each fixed bed reaction temperature, the residence time were controlled at 70 seconds; Obtain the thick product of micromolecular hydroxyl silicone oil; Reduce pressure again behind the thick frequent pressure-off solvent of product and remove low component, obtain micromolecular hydroxyl silicone oil, viscosity 20CS; Hydroxy radical content 9%, yield 93.9%.
After stability was embodied in 6 months shelf liveves, product appearance is colourless transparent liquid, and was not stratified, after 6 months shelf liveves hydroxy radical content measure with the shelf lives before compare to descend and be no more than 5%.
Embodiment 4:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil joins hexamethyl cyclotrisiloxane 1000 gram, acetone 1400 grams, water 120 grams in the 3000ml four-hole bottle that band stirs, and heats up and keeps 35 ℃; Dissolve mix after, adopt peristaltic pump continuously through 1 fixed bed that is added with 100 grams, 732 ion exchange resin, 38 ℃ of each fixed bed reaction temperature, the residence time were controlled at 27 seconds; Obtain the thick product of micromolecular hydroxyl silicone oil; Reduce pressure again behind the thick frequent pressure-off solvent of product and remove low component, obtain micromolecular hydroxyl silicone oil, viscosity 13CS; Hydroxy radical content 5%, yield 70.7%.
After stability was embodied in 6 months shelf liveves, product appearance is colourless transparent liquid, and was not stratified, after 6 months shelf liveves hydroxy radical content measure with the shelf lives before compare to descend and be no more than 8%.
Embodiment 5:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil joins hexamethyl cyclotrisiloxane 1000 gram, acetone 1400 grams, water 120 grams in the 3000ml four-hole bottle that band stirs, and heats up and keeps 65 ℃; Dissolve mix after, adopt peristaltic pump continuously through 1 fixed bed that is added with 100 gram KY-23 strong-acid ion exchange resins, 65 ℃ of each fixed bed reaction temperature, the residence time were controlled at 75 seconds; Obtain the thick product of micromolecular hydroxyl silicone oil; Reduce pressure again behind the thick frequent pressure-off solvent of product and remove low component, obtain micromolecular hydroxyl silicone oil, viscosity 10CS; Hydroxy radical content 11%, yield 72.8%.
After stability was embodied in 6 months shelf liveves, product appearance is colourless transparent liquid, and was not stratified, after 6 months shelf liveves hydroxy radical content measure with the shelf lives before compare to descend and be no more than 10%.
Claims (3)
1. the method for a continuous processing synthesizing small molecular hydroxy silicon oil; It is characterized by: hexamethyl cyclotrisiloxane 1000 grams, acetone 1400 grams, water 120 grams are joined in the 3000ml four-hole bottle of band stirring; Heating up also keeps 40-60 ℃, dissolve mix after, adopt peristaltic pump continuously through 2 fixed beds that are added with 100 gram strongly acidic styrene type cation exchange resins; 40-60 ℃ of each fixed bed reaction temperature, the residence time were controlled at 50 ± 20 seconds; Obtain the thick product of micromolecular hydroxyl silicone oil, reducing pressure behind the thick frequent pressure-off solvent of product removes low component again, obtains micromolecular hydroxyl silicone oil.
2. the method for a kind of continuous processing synthesizing small molecular hydroxy silicon oil as claimed in claim 1 is characterized by: strongly acidic styrene type cation exchange resin comprises macroporous type and gel-type, and the following trade mark is arranged: 732, and D001, KY-2, KY-23.
3. the method for a kind of continuous processing synthesizing small molecular hydroxy silicon oil as claimed in claim 1; It is characterized by: hexamethyl cyclotrisiloxane 1000 grams, acetone 1400 grams, water 120 grams are joined in the 3000ml four-hole bottle of band stirring; Heating up also keeps 50 ℃, dissolve mix after, adopt peristaltic pump continuously through the fixed bed of 100 gram D001 strong-acid ion exchange resins and the fixed bed of 100 gram KY-23 strong-acid ion exchange resins; 50 ℃ of each fixed bed reaction temperature, the residence time were controlled at 50 seconds; Obtain the thick product of micromolecular hydroxyl silicone oil, reducing pressure behind the thick frequent pressure-off solvent of product removes low component again, obtains micromolecular hydroxyl silicone oil.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898646A (en) * | 2012-09-06 | 2013-01-30 | 江苏梅兰化工有限公司 | Continuous production process for silicone oil |
| CN105754102A (en) * | 2016-04-27 | 2016-07-13 | 广州道林合成材料有限公司 | Hydroxyl silicone oil and continuous preparation method thereof |
| CN107722276A (en) * | 2017-10-18 | 2018-02-23 | 广州道林合成材料有限公司 | Silicone oil and its continuous preparation method |
| CN108440757A (en) * | 2018-03-29 | 2018-08-24 | 李卓瑾 | A kind of constitution controller and production technology |
| CN110527482A (en) * | 2019-09-17 | 2019-12-03 | 陕西杨凌磐基新材料科技有限公司 | Railway ballastless track special dual-component filleting waterproof gasket cement and preparation method thereof |
| CN110606953A (en) * | 2019-09-26 | 2019-12-24 | 唐山三友硅业有限责任公司 | Low-viscosity hydroxyl-terminated vinyl methyl silicone oil and continuous preparation method thereof |
| CN111234192A (en) * | 2020-03-26 | 2020-06-05 | 山东福司特新材料科技有限公司 | Preparation method of organic silicon modified saturated polyester resin with high weather resistance |
| CN112119111A (en) * | 2018-05-17 | 2020-12-22 | 赢创运营有限公司 | Linear polydimethylsiloxane-polyoxyalkylene block copolymers of the ABA structure type |
| CN112625241A (en) * | 2020-10-12 | 2021-04-09 | 湖北兴瑞硅材料有限公司 | Synthesis method of low-viscosity hydroxyl silicone oil |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898646B (en) * | 2012-09-06 | 2015-01-28 | 江苏梅兰化工有限公司 | Continuous production process for silicone oil |
| CN102898646A (en) * | 2012-09-06 | 2013-01-30 | 江苏梅兰化工有限公司 | Continuous production process for silicone oil |
| CN105754102A (en) * | 2016-04-27 | 2016-07-13 | 广州道林合成材料有限公司 | Hydroxyl silicone oil and continuous preparation method thereof |
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| CN105754102B (en) * | 2016-04-27 | 2018-08-21 | 广州道林合成材料有限公司 | A kind of hydroxy silicon oil and its continuous preparation method |
| CN107722276B (en) * | 2017-10-18 | 2020-08-07 | 广州福泽新材料有限公司 | Silicone oil and continuous preparation method thereof |
| CN107722276A (en) * | 2017-10-18 | 2018-02-23 | 广州道林合成材料有限公司 | Silicone oil and its continuous preparation method |
| CN108440757A (en) * | 2018-03-29 | 2018-08-24 | 李卓瑾 | A kind of constitution controller and production technology |
| CN112119111A (en) * | 2018-05-17 | 2020-12-22 | 赢创运营有限公司 | Linear polydimethylsiloxane-polyoxyalkylene block copolymers of the ABA structure type |
| CN110527482A (en) * | 2019-09-17 | 2019-12-03 | 陕西杨凌磐基新材料科技有限公司 | Railway ballastless track special dual-component filleting waterproof gasket cement and preparation method thereof |
| CN110527482B (en) * | 2019-09-17 | 2021-06-29 | 陕西杨凌磐基新材料科技有限公司 | Special two-component caulking waterproof sealant for railway ballastless track and preparation method thereof |
| CN110606953A (en) * | 2019-09-26 | 2019-12-24 | 唐山三友硅业有限责任公司 | Low-viscosity hydroxyl-terminated vinyl methyl silicone oil and continuous preparation method thereof |
| CN111234192A (en) * | 2020-03-26 | 2020-06-05 | 山东福司特新材料科技有限公司 | Preparation method of organic silicon modified saturated polyester resin with high weather resistance |
| CN112625241A (en) * | 2020-10-12 | 2021-04-09 | 湖北兴瑞硅材料有限公司 | Synthesis method of low-viscosity hydroxyl silicone oil |
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| CN102558559B (en) | 2014-03-05 |
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Address after: 330300 Yangjialing, Yongxiu County, Jiujiang City, Jiangxi Province Patentee after: JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. Address before: 330319 Spark Industrial Park, Yongxiu County, Jiujiang City, Jiangxi Province Patentee before: Jiangxi Star-Fire Silicone Factory of Bluestar New Chemical Materials Co.,Ltd. |