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Production method for preparing high-boiling silicone oil by alcoholysis of organosilicon high-boiling components

A high-boiling silicone oil and a production method are applied in the production field of preparing high-boiling silicone oil by alcoholysis of organosilicon high-boiling substances, which can solve the problems of difficulty in product neutralization, complicated process, harsh reaction conditions and the like, and achieve good neutralization effect. , High reaction controllability, the effect of reducing the content of organic chlorine

Active Publication Date: 2013-07-03
TANGSHAN SANYOU SILICON IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Due to its complex composition, pungent smell and strong corrosiveness, organic silicon high boiling substances are difficult to store and use, causing serious environmental protection and safety problems
At present, domestic and foreign studies on the comprehensive utilization of organosilicon high boilers mainly include cracking method and alcoholysis method. The problems in the preparation of monosilane by cracking method are: complex process, harsh reaction conditions, high production cost, and low yield of monosilane Wait
The main problems of the alcoholysis method are: the molecular weight is difficult to control, the product is difficult to neutralize, the oil production rate is low, the product is easy to return to acid, the waste alkyd solution produced cannot be recycled, and a large amount of three wastes are generated, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: A kind of production method that utilizes organosilicon high boiler alcoholysis to prepare high boiling silicone oil, its steps are as follows:

[0025] ①Add 100 parts by weight of organosilicon high boilers to the reaction kettle. At room temperature, drop 30 parts by weight of methanol into the kettle to control the reaction speed. , start to heat up, control the reaction temperature at the end of the dropwise addition to be 70°C, and keep the reflux reaction at this temperature for 3 hours;

[0026] 2. Add 2 parts by weight of water dropwise in the reactor, keep the reflux reaction for 1 hour, and simultaneously send the hydrogen chloride gas generated by the reaction into the water spray tower for absorption through the exhaust device;

[0027] ③ Move the reaction solution into the acid separator and let it stand for stratification to obtain crude acidic silicone oil and alkyd solution;

[0028] ④ Inject the crude acidic silicone oil into the deacidif...

Embodiment 2

[0031] Embodiment 2: A kind of production method that utilizes organosilicon high boiler alcoholysis to prepare high boiling silicone oil, its steps are as follows:

[0032] ①Add 100 parts by weight of organosilicon high boilers to the reaction kettle, and drop 60 parts by weight of methanol into the kettle at room temperature to control the reaction speed. , start to heat up, control the reaction temperature at the end of the dropwise addition to be 60°C, and keep the reflux reaction at this temperature for 2 hours;

[0033] 2. drop 5 parts by weight of water in the reactor, keep the reflux reaction for 0.5 hour, and simultaneously send the hydrogen chloride gas generated by the reaction into the water spray tower for absorption through the draft device;

[0034] ③ Move the reaction solution into the acid separator and let it stand for stratification to obtain crude acidic silicone oil and alkyd solution;

[0035] ④ Inject the crude acidic silicone oil into the deacidificati...

Embodiment 3

[0038] Embodiment 3: A kind of production method that utilizes organosilicon high boiler alcoholysis to prepare high boiling silicone oil, its steps are as follows:

[0039] ①Add 100 parts by weight of organosilicon high boilers to the reaction kettle. At room temperature, drop 40 parts by weight of ethanol into the kettle to control the reaction speed. , start to heat up, control the reaction temperature at the end of the dropwise addition to be 80°C, and keep the reflux reaction at this temperature for 2 hours;

[0040] 2. Add 3 parts by weight of water dropwise in the reactor, keep the reflux reaction for 1 hour, and simultaneously send the hydrogen chloride gas generated by the reaction into the water spray tower for absorption through the exhaust device;

[0041] ③ Move the reaction solution into the acid separator and let it stand for stratification to obtain crude acidic silicone oil and alkyd solution;

[0042] ④ Inject the crude acidic silicone oil into the deacidifi...

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Abstract

The invention belongs to a production method of high-boiling silicone oil and specifically relates to a production method for preparing high-boiling silicone oil by alcoholysis of an organosilicon high-boiling component. The production method comprises the following steps of: adding dropwisely excess alcohol into an organosilicon high-boiling component at room temperature, heating to 70-80 DEG C,and carrying out an alcoholysis reaction for 2-3 hours; adding dropwisely a little water into a reaction solution for continuous reaction; placing the reaction solution into an acid distributor and standing for layering to obtain crude acidic silicone oil and an alcohol acid solution; injecting the crude acidic silicone oil into a depickling reaction vessel for depickling to obtain a refined acidic silicone oil, injecting the refined acidic silicone oil into a neutralization reaction vessel for neutralization reaction, and filtering the neutralized reactant to obtain the high-boiling siliconeoil. A hydrogen chloride gas generated during the reaction is sent through an updraft ventilator to a water spray scrubber for absorption. The alcohol obtained after rectification and purification ofthe alcohol acid solution generated during the reaction is continuously applied in the alcoholysis reaction. The production method has advantages of low production cost, less amount of the neutralizer, high oil yield, stable product performance and controllable molecular weight, and is suitable for industrial production.

Description

Technical field: [0001] The invention belongs to a production method of high-boiling silicone oil, in particular to a production method for preparing high-boiling silicone oil by alcoholysis of organosilicon high-boiling matter. Background technique: [0002] Due to its complex composition, pungent smell and strong corrosiveness, organosilicon high boilers are difficult to store and utilize, causing serious environmental protection and safety problems. At present, domestic and foreign studies on the comprehensive utilization of organosilicon high boilers mainly include cracking method and alcoholysis method. The problems in the preparation of monosilane by cracking method are: complex process, harsh reaction conditions, high production cost, and low yield of monosilane Wait. The main problems of the alcoholysis method are: the molecular weight is difficult to control, the product is difficult to neutralize, the oil production rate is low, the product is easy to return to ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06C08G77/34
Inventor 李索海张建敏李允浩曹鹤郭佺
Owner TANGSHAN SANYOU SILICON IND
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