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A kind of preparation method of branched chain silicone oil

A branched-chain silicone oil and siloxane technology, which is applied in the field of preparation of branched-chain silicone oil, can solve the problems of difficulty in precise control of branched-chain content of branched-chain silicone oil, easy environmental pollution, unstable product quality, etc. Low cost and good low temperature performance

Active Publication Date: 2019-03-29
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this process, due to the step-by-step reaction, not only the process is complicated, but also there are strong acids such as methanesulfonic acid in the reaction, which is easy to cause pollution to the environment. In addition, in the current preparation process, due to the use of vacuum high-temperature dehydration and other processes, here During the process, it is easy to cause D4, MM and other raw materials to be distilled out of the reaction system together with water, which makes it difficult to accurately control the branched chain content in the branched chain silicone oil, which in turn causes the instability of product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 Preparation of branched chain silicone oil with polymethylsilsesquioxane

[0016] Add 500g of octamethylcyclotetrasiloxane, 8g of polymethylsilsesquioxane, and 5g of hexamethylsiloxane into the polymerization kettle, stir and mix evenly, add 2g of potassium hydroxide, and keep stirring at 120°C For the reaction, when the polymethylsilsesquioxane in the polymerization kettle is completely dissolved, cool down to room temperature, add 3.9g of trimethylchlorosilane, and keep stirring for 1-2 hours, filter to remove the precipitate, and distill under reduced pressure to obtain the silicone oil product .

Embodiment 2

[0017] Example 2 Preparation of branched chain silicone oil with polyphenylsilsesquioxane

[0018] Add 1000g of octamethylcyclotetrasiloxane, 15g of polyphenylsilsesquioxane, and 5g of hexamethylsiloxane into the polymerization kettle, stir and mix evenly, add 4g of potassium hydroxide, and keep stirring at 120°C For the reaction, when the polyphenylsilsesquioxane in the polymerization kettle is completely dissolved, cool down to room temperature, add 7.8g of trimethylchlorosilane, and keep stirring for 1-2 hours, filter to remove the precipitate, and distill under reduced pressure to obtain the silicone oil product .

Embodiment 3

[0019] Example 3 Preparation of branched chain silicone oil with dimethyl silicone oil

[0020] Add 1200g of dimethyl silicone oil and 18g of polymethylsilsesquioxane into the polymerization kettle, stir and mix evenly, add 4g of potassium hydroxide, and keep stirring at 120°C to make it react. When the polymethylsilsesquioxane in the polymerization kettle After the hemioxane is completely dissolved, cool down to room temperature, add 7.8 g of trimethylchlorosilane, and keep stirring for 1-2 hours, filter to remove the precipitate, and distill under reduced pressure to obtain the silicone oil product.

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Abstract

The present invention discloses a preparation method of branched silicone oil. Siloxane, silsesquioxane and hexamethylsiloxane are mixed, potassium hydroxide is added, the mixture is stirred continuously at a temperature of 100-150 DEG C until the silsesquioxane is completely dissolved, then the temperature of the mixture is lowered to room temperature, an end-capping reagent is added to terminate the reaction, the mixture is subjected to filtration, and the filtered mixture is distilled to obtain the branched silicone oil. The preparation method overcomes the shortcomings that the process is complicated, the environment is polluted, and the process repeatability is poor in traditional branched silicone oil preparation processes, and at the same time can also precisely control the content of branched chains in the silicone oil. By adding different amounts of the silsesquioxane and hexamethylsiloxane, a series of viscosity controllable branch chain type silicone oil can be prepared. The prepared silicone oil has characteristics of being controllable in viscosity, good in low temperature performance, low in production cost, simple in technology, etc. The preparation method can greatly improve the traditional preparation technology of silicone oil and can be widely applied in the aviation and other machinery fields.

Description

technical field [0001] The invention relates to a preparation method of branched chain silicone oil. Background technique [0002] As a kind of oil with a wide application background, silicone oil is widely used in machinery manufacturing, cosmetics, instrumentation and other fields. In the mechanical field, a very low temperature is often required, so the silicone oil used is required to have an extremely low freezing point. Therefore, in the process of synthesizing silicone oil, it is a common method to introduce a certain amount of branched chain structure into the silicone oil molecule. When the branched chain is introduced, the freezing point of silicone oil can be lowered to below -70°C, which meets the requirements of different machines. At present, the process of preparing branched silicone oil is usually divided into two steps: first, methyltriethoxysilane, octamethylcyclotetrasiloxane (D4) and hexamethylsiloxane (MM) are used Methanesulfonic acid catalyzes the r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/44C08G81/00C08G77/06
Inventor 乔旦冯大鹏王海忠
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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