CN102558559B - 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 with active group hydroxyl, is the desirable constitution controller of silicon rubber.The method of preparing micromolecular hydroxyl silicone oil has multiple, and to use more be D4 (DMC) and acetic anhydride to suitability for industrialized production at present, but product has acetic acid taste.
Summary of the invention
The invention provides a kind of method of continuous processing synthesizing small molecular hydroxy silicon oil, the by product D obtaining in producing with organosilicon methyl cyclosiloxane
3for raw material, make hydroxy silicon oil, 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, 120 grams of 1000 grams of hexamethyl cyclotrisiloxanes, 1400 grams, acetone, water are joined in the 3000ml four-hole bottle that band stirs, heat up and keep 40-60 ℃, after dissolving and mixing, adopt peristaltic pump continuously by 2 fixed beds that are added with 100 grams of 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, after the thick frequent pressure-off solvent of product, decompression 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, D001, KY-2, KY-23.
The inventive method be take hexamethyl cyclotrisiloxane as raw material, and technique can be produced in serialization, reproducible; Product yield is high, and stability in storage is better, and the shelf lives can reach more than 6 months, and product appearance is colourless transparent liquid, and viscosity is at 15-30mm
2/ s, hydroxy radical content is between 6-10%; In production process, technique is polluted without " three wastes ", and solvent and low-boiling-point substance can be recycled, can industrialized production.
Stability was embodied in after 6 months shelf liveves, and product appearance is colourless transparent liquid, not stratified, and after 6 months shelf liveves, hydroxy radical content is measured and to be no more than 5% with comparing before the shelf lives to decline.
Embodiment
Embodiment 1:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil, by 1000 grams of hexamethyl cyclotrisiloxanes, 1400 grams, acetone, 120 grams, water joins in the 3000ml four-hole bottle that band stirs, heat up and keep 50 ℃, after dissolving and mixing, adopt peristaltic pump continuously by the fixed bed of 100 grams of D001 strong-acid ion exchange resins and the fixed bed of 100 grams of KY-23 strong-acid ion exchange resins, each fixed bed reaction temperature 50 C, the residence time is controlled at 50 seconds, obtain the thick product of micromolecular hydroxyl silicone oil, after the thick frequent pressure-off solvent of product, decompression removes low component again, obtain micromolecular hydroxyl silicone oil, viscosity 22CS, hydroxy radical content 9%, yield 94.6%.
Stability was embodied in after 6 months shelf liveves, and product appearance is colourless transparent liquid, not stratified, and after 6 months shelf liveves, hydroxy radical content is measured and to be no more than 2% with comparing before the shelf lives to decline.
Embodiment 2:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil, by 1000 grams of hexamethyl cyclotrisiloxanes, 1400 grams, acetone, 120 grams, water joins in the 3000ml four-hole bottle that band stirs, heat up and keep 40 ℃, after dissolving and mixing, adopt peristaltic pump continuously by being added with the fixed bed of 100 gram of 732 ion exchange resin and the fixed bed of 100 grams of KY-2 ion exchange resin, 40 ℃ of each fixed bed reaction temperature, the residence time is controlled at 30 seconds, obtain the thick product of micromolecular hydroxyl silicone oil, after the thick frequent pressure-off solvent of product, decompression removes low component again, obtain micromolecular hydroxyl silicone oil, viscosity 24CS, hydroxy radical content 8%, yield 90.1%.
Stability was embodied in after 6 months shelf liveves, and product appearance is colourless transparent liquid, not stratified, and after 6 months shelf liveves, hydroxy radical content is measured and to be no more than 5% with comparing before the shelf lives to decline.
Embodiment 3:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil, by 1000 grams of hexamethyl cyclotrisiloxanes, 1400 grams, acetone, 120 grams, water joins in the 3000ml four-hole bottle that band stirs, heat up and keep 60 ℃, after dissolving and mixing, adopt peristaltic pump by 2, to be added with the fixed bed of 100 grams of D001 strong-acid ion exchange resins and the fixed bed of 100 grams of KY-2 ion exchange resin continuously, each fixed bed reaction temperature 60 C, the residence time is controlled at 70 seconds, obtain the thick product of micromolecular hydroxyl silicone oil, after the thick frequent pressure-off solvent of product, decompression removes low component again, obtain micromolecular hydroxyl silicone oil, viscosity 20CS, hydroxy radical content 9%, yield 93.9%.
Stability was embodied in after 6 months shelf liveves, and product appearance is colourless transparent liquid, not stratified, and after 6 months shelf liveves, hydroxy radical content is measured and to be no more than 5% with comparing before the shelf lives to decline.
Embodiment 4:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil, by 1000 grams of hexamethyl cyclotrisiloxanes, 1400 grams, acetone, 120 grams, water joins in the 3000ml four-hole bottle that band stirs, heat up and keep 35 ℃, after dissolving and mixing, adopt peristaltic pump continuously by 1 fixed bed that is added with 100 gram of 732 ion exchange resin, 38 ℃ of each fixed bed reaction temperature, the residence time is controlled at 27 seconds, obtain the thick product of micromolecular hydroxyl silicone oil, after the thick frequent pressure-off solvent of product, decompression removes low component again, obtain micromolecular hydroxyl silicone oil, viscosity 13CS, hydroxy radical content 5%, yield 70.7%.
Stability was embodied in after 6 months shelf liveves, and product appearance is colourless transparent liquid, not stratified, and after 6 months shelf liveves, hydroxy radical content is measured and to be no more than 8% with comparing before the shelf lives to decline.
Embodiment 5:
A kind of method of continuous processing synthesizing small molecular hydroxy silicon oil, by 1000 grams of hexamethyl cyclotrisiloxanes, 1400 grams, acetone, 120 grams, water joins in the 3000ml four-hole bottle that band stirs, heat up and keep 65 ℃, after dissolving and mixing, adopt peristaltic pump continuously by 1 fixed bed that is added with 100 grams of KY-23 strong-acid ion exchange resins, 65 ℃ of each fixed bed reaction temperature, the residence time is controlled at 75 seconds, obtain the thick product of micromolecular hydroxyl silicone oil, after the thick frequent pressure-off solvent of product, decompression removes low component again, obtain micromolecular hydroxyl silicone oil, viscosity 10CS, hydroxy radical content 11%, yield 72.8%.
Stability was embodied in after 6 months shelf liveves, and product appearance is colourless transparent liquid, not stratified, and after 6 months shelf liveves, hydroxy radical content is measured and to be no more than 10% with comparing before the shelf lives to decline.
Claims (2)
1. the method for a continuous processing synthesizing small molecular hydroxy silicon oil, it is characterized by: by 1000 grams of hexamethyl cyclotrisiloxanes, 1400 grams, acetone, 120 grams, water joins in the 3000ml four-hole bottle that band stirs, heat up and keep 40-60 ℃, after dissolving and mixing, adopt peristaltic pump continuously by 2 fixed beds that are added with 100 grams of strongly acidic styrene type cation exchange resins, each fixed bed reaction temperature 40-60 ℃, the residence time is controlled at 50 ± 20 seconds, obtain the thick product of micromolecular hydroxyl silicone oil, after the thick frequent pressure-off solvent of product, decompression removes low component again, obtain 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, has the following trade mark: 732, D001.
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| CN102898646B (en) * | 2012-09-06 | 2015-01-28 | 江苏梅兰化工有限公司 | Continuous production process for silicone oil |
| 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 |
| CN108440757A (en) * | 2018-03-29 | 2018-08-24 | 李卓瑾 | A kind of constitution controller and production technology |
| US11359056B2 (en) * | 2018-05-17 | 2022-06-14 | Evonik Operations Gmbh | Linear polydimethylsiloxane-polyoxyalkylene block copolymers of the structure type ABA |
| 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 |
| CN111234192B (en) * | 2020-03-26 | 2023-04-07 | 邦弗特(山东)新材料有限公司 | 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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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. |