Method for synthesizing short-chain hydroxyl silicone oil

A technology of short-chain hydroxysilicone and a synthesis method, which is applied in the field of synthesis of short-chain hydroxysilicone oil, can solve the problems of difficult process control, high cost and high viscosity, and achieves easy control of reaction conditions, fast reaction generation speed, and easy availability of raw material costs. Effect

Inactive Publication Date: 2008-07-23
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, in method (1) D 3 The output is less, the price is high, and the low-cost octamethylcyclotetrasiloxane (D 4 ), ordinary acid clay can not be effectively catalyzed; the viscosity of the synthetic hydroxy silicone oil of method (2) is at 350-3500CS / 25°C, the viscosity is too high, and the hydroxyl content is too low, which is not suitable for the needs of organic synthesis; in method (3) To use a large amount of sodium hydroxide to catalyze and neutralize with a large amount of sulfuric acid, the cost is higher; method (4) needs to use acetic anhydride as end-capping agent, except that the price is high, adopting this method has poor process stability and is difficult to control
In method (5), the hydrolysis reaction of chlorosilane is too violent, the process is difficult to control, and a large amount of waste acid is produced, which requires post-processing, and the cost is relatively high
In addition, the above five methods synthesized are all short hydroxyl silicone oils with methyl side groups, and do not contain hydrogen, C 2 -C 7 Alkyl chains, vinyl and nitrile ethyl and other functional side chains with rich functions cannot meet the needs of special industries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Mix 5g acid clay, 3g water, 110g acetone, 100gD 4 Put it into a three-necked flask equipped with a reflux device, add 1.0 g of concentrated sulfuric acid under stirring, and react at 50 to 60 ° C for 16 hours; after the reaction, add 5 g of magnesium oxide and stir for 10 minutes, suction filtration, and rotate the filtrate with The acetone was recovered by distillation at 45° C. with an evaporator, and then 150 ml of sodium carbonate aqueous solution was added to neutralize it for 3 hours at 30-60° C., and the mixture was left to stand for stratification. Add 200 ml of water to the organic layer of the upper layer to wash 1 to 2 times, and then let stand for stratification to remove water, then the organic layer is sent to a rotary evaporator to heat up to 95 ° C, and the low boilers are removed under reduced pressure to obtain a small molecular hydroxy silicone oil. The viscosity was 19.4CS and the yield was 98.0%.

Embodiment 2

[0012] 2g acid clay, 8g water, 110g acetone, 100gD 4 Put it into a three-necked flask equipped with a reflux device, add 1.0 g of concentrated sulfuric acid under stirring, and react at 50 to 60 ° C for 24 hours; the rest of the process conditions are the same as in Example 1, and the viscosity of the obtained small molecular hydroxy silicone oil is 10.5 CS, 85.5% yield.

Embodiment 3

[0014] Mix 10g acid clay, 4g water, 110g acetone, 80gD 4 , 20g of tetraethylcyclotetrasiloxane were added into the three-necked flask equipped with the reflux device, and 0.65g of concentrated sulfuric acid was added under stirring, and the reaction was carried out at 50 to 60 ° C for 16 hours; the remaining process conditions were the same as in Example 1, The viscosity of the prepared small molecular hydroxy silicone oil was 11.5CS, and the yield was 82.2.0%.

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Abstract

The invention relates to a synthetic method for short-chain hydroxyl silicone oil. Firstly, the materials are proportionally measured according to raw materials components, then adding acid clay, water, and cyclotetrasiloxanes to a three-mouth flask with a reflux device, adding concentrated sulfuric acid in agitation condition, and reacting by controlling the reaction temperature, when the reaction is completed, adding magnesia and agitating about 10 minutes, then processing pumping filtration, distilling and recovering acetone using a rotary evaporimeter used for filtrating under the temperature of 45 DEG C, then adding sodium carbonate solution for neutralization under controllable temperature for stratification; then watering and washing the organic layer on the upper layer once or twice, then discharging water through stratification, and then feeding the organic layer into the rotary evaporimeter for warming up to 95 DEG C, depressing and detracting low-boiling residues, obtaining micromolecule hydroxyl silicone oil. The synthetic method for short-chain hydroxyl silicone oil has the advantages of simple technological process, easy controllable reaction condition, low cost and easily available raw materials, fast reaction generating speed, good product quality and high reactivity, and wide application range.

Description

Technical field: [0001] The invention relates to a method for synthesizing short-chain hydroxy silicone oil, in particular to a method for synthesizing side groups using acid clay and concentrated sulfuric acid as dual catalysts, which are hydrogen, C 1 -C 7 The method of small molecule hydroxy silicone oil of alkyl chain or vinyl, nitrile ethyl. Background technique: [0002] Short-chain hydroxy silicone oil is a structure control agent for high-temperature vulcanized silicone rubber, and can also be used for the synthesis of silicone resins or organic compounds. At present, its main synthesis methods are as follows: (1) U.S. Patent Publication No. USP3853932, published on In October 1974, a patent for the production of low-molecular-weight silanol-terminated polymers disclosed a method for catalyzing hexamethylcyclotrisiloxane (D 3 ) method for synthesizing low molecular weight hydroxysilicone oil; (2) Chinese Patent Authorization Announcement No. CN 1025861C, the author...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/08C08G77/16
Inventor 蔺存国王利
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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