A kind of preparation method of silicone oil

A silicone oil and organosilicon technology, applied in the field of preparation of silicone oil, can solve the problems of reducing the hydrogen chloride gas efficiency of the aqueous solution, increasing the proportion of ammonia water, etc., and achieve the effects of increasing the equilibrium reaction rate, speeding up the neutralization speed, and increasing the neutralization effect.

Active Publication Date: 2021-08-03
山东盛宇新材料有限公司
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Problems solved by technology

[0005] In order to make up for the deficiencies in the prior art, the present invention proposes a method for preparing silicone oil. The present invention is mainly used to solve the problem that most of the existing aqueous solutions are sprayed into the kettle body through a high-pressure nozzle. When spraying the aqueous solution, it is easy to reduce the efficiency of the aqueous solution to absorb hydrogen chloride gas, and then increase the proportion of ammonia water used during neutralization, resulting in the need to add a large amount of ammonia water to carry out the neutralization reaction during the neutralization step

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  • A kind of preparation method of silicone oil
  • A kind of preparation method of silicone oil
  • A kind of preparation method of silicone oil

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Embodiment Construction

[0025] use Figure 1-Figure 4 A method for preparing a silicone oil according to an embodiment of the present invention is described as follows.

[0026] Such as Figure 1-Figure 4 Shown, the preparation method of a kind of silicone oil of the present invention, this method comprises the following steps:

[0027] S1: Raw material ratio: 100 parts by weight of organosilicon high boiler; 30-40 parts by weight of raw material methanol with 80%-90% by weight; 15-18 parts by weight of methanol co-solvent and the same amount of urea; 27% by weight of ammonia water 1.0~1.5 copies;

[0028] S2: Alcoholysis: add 100 parts by weight of organosilicon high boilers into the reaction kettle body 1 through the feeding pipe at 20°C to 25°C, and add 30 to 40 parts by weight of raw material methanol with a weight percentage of 80% to 90% dropwise , added dropwise for 6 to 8 hours; the initial drop rate was 3 parts / hour, and added dropwise for 2 to 3 hours; gradually raised to 10 parts / hour; ...

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Abstract

The invention belongs to the technical field of preparation of silicone oil, and specifically relates to a preparation method of silicone oil; the method includes the following steps: S1: Raw material ratio: 100 parts by weight of organic silicon high-boiler; 30-40 parts by weight of methanol; 15-18 parts of solvent and the same amount of urea; 1.0-1.5 parts of ammonia water; S2: alcoholysis: add 100 parts by weight of organosilicon high boilers into the reactor body through the feeding pipe, and add 30-40 parts by weight of methanol dropwise; The crude high-boiling silicone oil obtained by neutralizing and stratifying in step S3 is filtered through the discharge box provided in the reactor body, and the acid water and impurities are filtered out through the discharge pipe; The hydrogen chloride gas produced in the water is sprayed and absorbed; the aqueous solution of the spray device is mixed with 0.2 to 0.5 parts of ammonia water; the evaporation of ammonia water lower than the weight percentage can neutralize the hydrochloric acid, thereby reducing the amount of ammonia water added during neutralization. At the same time, it speeds up the neutralization speed of high boiling silicone oil.

Description

technical field [0001] The invention belongs to the technical field of preparation of silicone oil, in particular to a preparation method of silicone oil. Background technique [0002] Silicone is an important emerging material, which has a wide range of applications in many fields. With the rapid development of the organosilicon industry, a large amount of silane high boilers are produced during the synthesis of organosilicon monomer methylchlorosilane. [0003] The traditional method for the preparation of silicone oil is to put the organic silicon high boiler into the reaction kettle, add anhydrous methanol alcohol to carry out the alcoholysis reaction, raise the temperature to catch the acid for h; then add 2 times the solvent and 4 times the water to the alcoholysis product, and carry out Hydrolysis reaction, after the reaction, stand to separate the acid water, wash the upper product to neutral, and distill under reduced pressure to obtain the hydrolyzate; mix the hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/10C08G77/06C08G77/04
CPCC08G77/04C08G77/06C08G77/10
Inventor 不公告发明人
Owner 山东盛宇新材料有限公司
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