Novel method for preparing 1,1,1,3,5,5,5-heptamethyltrisiloxane by adopting solid superacid

A technology of heptamethyltrisiloxane and solid superacid, which is applied in chemical instruments and methods, silicon organic compounds, physical/chemical process catalysts, etc., can solve the problem of no fixed mode, etc., and achieve easy separation and low production cost , the effect of mild reaction conditions

Inactive Publication Date: 2014-08-27
JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current modification research directions mainly include: using metal oxides ZrO2, TiO2 and Fe2O3 as the matrix, adding other metals or oxides to form multi-component solid superacids; introducing rare earth elements and transition elements for modification; introducing specific molecular sieves and Nanoscale metal oxides, etc.; while the combined use of catalysts is related to the specific reaction system in practical applications. There is no fixed model to apply. Only by constantly exploring and researching in the process of production practice can we truly grasp the application effect of each combination

Method used

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  • Novel method for preparing 1,1,1,3,5,5,5-heptamethyltrisiloxane by adopting solid superacid
  • Novel method for preparing 1,1,1,3,5,5,5-heptamethyltrisiloxane by adopting solid superacid

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Embodiment 1

[0030] The preparation method of 1,1,1,3,5,5,5-heptamethyltrisiloxane comprises the following steps: mixing 202 hydrogen-containing silicone oil, hexamethyldisiloxane, and solid superacid catalyst in a mass ratio of 6.2 :1:0.27 is placed in a reactor with mechanical stirring, thermometer and reflux condenser, the temperature is raised under stirring, the temperature is controlled at 70°C for 7 hours, and it is left to stand for 2 hours, and the supernatant is filtered to obtain the filtrate, which is used Distillation in the rectification tower to obtain 1,1,1,3,5,5,5-heptamethyltrisiloxane product;

[0031] The solid superacid catalyst of the present invention is SO 4 2- / ZrO 2 -Fe 2 o 3 -Sm 2 o 3 , SO 4 2- / TiO 2 , SO 4 2- / ZrO 2 -Ce 2 (SO 4 ) 3 ; And the mass ratio of each catalyst is 2:3:1.6;

[0032] The preparation method of solid superacid catalyst is as follows:

[0033] SO 4 2- / TiO 2 Preparation of solid superacid catalyst: under constant stirring...

Embodiment 2

[0038] The preparation method of 1,1,1,3,5,5,5-heptamethyltrisiloxane of the present invention comprises the following steps: 202 hydrogen-containing silicone oil, hexamethyldisiloxane, solid superacid catalyst by mass The ratio of 3:1:0.08 is placed in a reactor equipped with mechanical stirring, a thermometer and a reflux condenser, the temperature is raised under stirring, the temperature is controlled at 50°C for 5 hours, and it is left to stand for 1 hour. The supernatant is filtered to obtain the filtrate, and the The filtrate is rectified by a rectification tower to obtain 1,1,1,3,5,5,5-heptamethyltrisiloxane product;

[0039] The solid superacid catalyst of the present invention is SO 4 2- / TiO 2 ;

[0040] The preparation method of solid superacid catalyst is as follows:

[0041] SO 4 2- / TiO 2 Preparation of solid superacid catalyst: under constant stirring, TiCl 4Add it to ammonia water with a mass fraction of 20%, adjust the pH value to 9, hydrolyze, let it...

Embodiment 3

[0044] The preparation method of 1,1,1,3,5,5,5-heptamethyltrisiloxane of the present invention comprises the following steps: 202 hydrogen-containing silicone oil, hexamethyldisiloxane, solid superacid catalyst by mass The ratio 10:1:0.66 is placed in a reactor with mechanical stirring, a thermometer and a reflux condenser, the temperature is raised under stirring, the temperature is controlled at 90°C for 9 hours, and the reaction is allowed to stand for 3 hours. The supernatant is filtered to obtain the filtrate, and the The filtrate is rectified by a rectification tower to obtain 1,1,1,3,5,5,5-heptamethyltrisiloxane product;

[0045] The solid superacid catalyst of the present invention is SO 4 2- / ZrO 2 ;

[0046] The preparation method of solid superacid catalyst is as follows:

[0047] SO 4 2- / ZrO 2 Preparation of solid superacid catalyst: under constant stirring, ZrCl 4 Add it to ammonia water with a mass fraction of 24%, adjust the pH value to 9, hydrolyze, le...

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Abstract

The invention relates to a novel method for preparing 1,1,1,3,5,5,5-heptamethyltrisiloxane by adopting solid superacid. The novel method comprises the following steps that: high-hydrogen-content silicone oil and hexamethyldisiloxane with the mass ratio of (3-10):1 are adopted as raw materials; a kettle type reaction is carried out under the catalytic effect of the solid superacid at a reaction temperature of 50 to 90 DEG C, and the reaction time is 5 to 9 hours; the 1,1,1,3,5,5,5-heptamethyltrisiloxane is prepared; and a product obtained after the reaction is rectified, and the product with the purity higher than 99.3 percent is obtained. The novel method provided by the invention has the advantages that the process is simple and continuous; the reaction conditions are mild; corrosion to equipment is avoided; the harm to environment is little; products can be easily separated; the production cost is low; the industrial continuous production can be realized; the catalytic efficiency of catalysts is high; the cost is reduced; and meanwhile, the product purity is improved.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a new method for preparing 1,1,1,3,5,5,5-heptamethyltrisiloxane by using solid superacid. Background technique [0002] 1,1,1,3,5,5,5-Heptamethyltrisiloxane (bistrimethylsiloxymethylsilane, CAS No. 1873-88-7) is a synthetic trisiloxane-like surface The synthesis and purification of intermediates of active agents are becoming more and more important. At present, the methods for synthesizing heptamethyltrisiloxane mainly include halosilane synthesis method, ring-opening copolymerization method and high hydrogen-containing silicone oil telomerization method, wherein the synthesis method of high hydrogen-containing silicone oil and hexamethyldisiloxane has a reaction Mild conditions, simple reaction process and so on. [0003] 1,1,1,3,5,5,5-heptamethyltrisiloxane can be synthesized from high hydrogen-containing silicone oil and hexamethyldisiloxane under the action of a c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08B01J27/053
Inventor 吴艳金王三跃欧阳建松贺志江
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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