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Preparation method of terminal hydrogen-containing silicone oil

A technology of terminal hydrogen-containing silicone oil and hydrogen content, applied in the chemical industry, can solve the problems of low production efficiency, difficulty in industrial production, and long time, and achieve the effects of high production efficiency, easy separation, and reduced corrosion

Inactive Publication Date: 2016-03-09
JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, concentrated sulfuric acid is used as a catalyst to prepare hydrogen-terminated polysiloxane, and sodium carbonate is added to neutralize and filter. The whole preparation process takes a long time, and it is difficult to realize continuous industrial production, and the production efficiency is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Add raw material 10gM to a 500mL three-necked flask with mechanical stirring, thermometer and reflux condenser H M H , 180gDMC and 12.0gSO 4 -2 / TiO 2 As a catalyst, the temperature is raised to 50°C for 1 hour under stirring, and then the temperature is increased to 70°C for 4 hours, the solid catalyst is filtered out, and the temperature is gradually raised to 160°C at -0.098MPa to remove low boilers. A colorless and transparent oily end-containing hydrogen-containing silicone oil with a viscosity of 15 cp is obtained. The catalyst can be used repeatedly for 10 times, and the viscosity change is within 10%.

Embodiment 2

[0018] Example 2: Add raw material 10gM to a 500mL three-necked flask with mechanical stirring, thermometer and reflux condenser H M H , 180gDMC and 12.0gSO 4 -2 / TiO 2 -Fe 2 O 3 As a catalyst, the temperature is raised to 50°C under reflux for 1h under stirring, and then the temperature is increased to 80°C for 5h, the solid catalyst is filtered out, and the temperature is gradually raised to 160°C at -0.098MPa to remove low boilers. A colorless and transparent oily end-containing hydrogen-containing silicone oil with a viscosity of 15.4cp is obtained. The catalyst can be reused for about 10 times, and the viscosity change is within 10%.

Embodiment 3

[0019] Example 3: Add raw material 10gM to a 500mL three-necked flask with mechanical stirring, thermometer and reflux condenser H M H , 180gDMC and 12.0gSO 4 -2 / Fe 2 O 3 As a catalyst, the temperature is raised to 50°C under reflux for 1h under stirring, and then the temperature is increased to 90°C for 5h, the solid catalyst is filtered out, and the temperature is gradually raised to 160°C at -0.098MPa to remove low boilers. A colorless and transparent oily end-containing hydrogen-containing silicone oil with a viscosity of 15.8 cp is obtained. The catalyst can be reused for about 10 times, and the viscosity change is within 10%.

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Abstract

The present invention discloses a preparation method of terminal hydrogen-containing silicone oil. The method comprises the following steps: using 1,1,3,3-tetramethyl-1,3-dihydrogen disiloxane (MHMH) as a capping agent, and dimethylcyclosiloxane (DMC) or octamethyl cyclotetrasiloxane (D4) as a raw material, under the catalysis of a solid super acid, heating to 50-100 DEG C to perform a telomerization reaction, and performing a reflux reaction for 4 to 8 h to prepare and obtain the terminal hydrogen-containing silicone oil. Compared with a conventional preparation method of the terminal hydrogen-containing silicone oil by using H2SO4 as a catalyst, a solid super acid is adopted as a catalyst, the catalytic effect is good and the catalyst can be repeatedly used, neutralization and washing are not required in the preparation method, the time used in the whole preparation process is short, continuous industrial production is expected to be achieved, and the production efficiency is high.

Description

Technical field [0001] The invention relates to a method for preparing hydrogen-containing silicone oil at the end, which belongs to the technical field of chemical industry. Background technique [0002] Hydrogen-terminated silicone oil refers to a polysiloxane terminated by active hydrogen, which is used as a key starting material and an important silicone intermediate for the production of silicone modified block or graft copolymers. Type hydrogen-containing polysiloxane is easy to design modified molecules, and the chemical bonds formed by the reaction are relatively stable. Double-end hydrogen-containing polysiloxane is mainly used for block copolymer modification of organic polymers, and single-end hydrogen-containing polysiloxane is used for graft modification. [0003] Using hydrogen-terminated silicone oil as the starting material, through the hydrosilation addition reaction, various reactive organic functional groups, such as amino, epoxy, hydroxyl, mercapto, methacrylox...

Claims

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Application Information

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IPC IPC(8): C08G77/12C08G77/08C08G77/06
Inventor 欧阳建松龚佑喜贺志江张磊
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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