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Synthesis method of low-viscosity hydroxyl silicone oil

A synthesis method and technology of hydroxy silicone oil, applied in the field of chemical production, can solve problems such as waste water generation and need to be washed, and achieve the effects of avoiding waste water, convenient storage and stable structure

Pending Publication Date: 2021-04-09
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And this method also needs washing, can produce a large amount of waste water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 111g of hexamethylcyclotrisiloxane, 400g of acetone, and 50g of water into a 500ml three-neck flask, start stirring, raise the temperature to 45°C, add 0.01g of potassium hydroxide, keep the temperature at 50°C after the dropwise addition, and the reaction time is 2h . Add 0.012g phosphoric acid to neutralize after the reaction finishes. After adding the neutralizing agent and maintaining the reaction for 30 minutes, the solvent is removed to obtain a transparent low-viscosity hydroxy silicone oil. The measured viscosity is 23mm 2 / s, the hydroxyl content is 10.2%. After 180 days at room temperature, the measured viscosity is 24mm 2 / s, the hydroxyl content is 10.4%. The content of monohydrogen phosphate and dihydrogen phosphate in the product prepared by the method is 130ppm, wherein the molar ratio of monohydrogen phosphate and dihydrogen phosphate is 0.87:1. Viscosity and hydroxyl content have no significant change, indicating that the low-viscosity hydroxyl...

Embodiment 2

[0023] Add 111g of hexamethylcyclotrisiloxane, 400g of acetone, and 50g of water into a 500ml three-neck flask, start stirring, raise the temperature to 45°C, add 0.01g of potassium hydroxide, keep the temperature at 70°C after the dropwise addition, and the reaction time is 2h . Add 0.012g phosphoric acid to neutralize after the reaction finishes. After adding the neutralizing agent and maintaining the reaction for 30 minutes, the solvent is removed to obtain a transparent low-viscosity hydroxy silicone oil. The measured viscosity is 40mm 2 / s, the hydroxyl content is 8.2%. After 180 days at room temperature, the measured viscosity is 42mm 2 / s, the hydroxyl content is 8.5%. The content of monohydrogen phosphate and dihydrogen phosphate in the product prepared by the method is 125ppm, wherein the molar ratio of monohydrogen phosphate and dihydrogen phosphate is 0.82:1. Viscosity and hydroxyl content have no significant change, indicating that the low-viscosity hydroxyl s...

Embodiment 3

[0026] Add 111g of hexamethylcyclotrisiloxane, 400g of acetone, and 50g of water into a 500ml three-neck flask, start stirring, raise the temperature to 45°C, add 0.01g of potassium hydroxide, keep the temperature at 30°C after the dropwise addition, and the reaction time is 4h . After the reaction, add 0.012g of phosphoric acid for neutralization, add the neutralizing agent and keep the reaction for 30min, then remove the solvent to obtain transparent low-viscosity hydroxy silicone oil. The measured viscosity is 25mm 2 / s, the hydroxyl content is 9.6%. After 180 days at room temperature, the measured viscosity is 24mm 2 / s, the hydroxyl content is 9.4%. The content of monohydrogen phosphate and dihydrogen phosphate in the product prepared by this method is 136ppm, wherein the molar ratio of monohydrogen phosphate and dihydrogen phosphate is 0.93:1. Viscosity and hydroxyl content have no significant change, indicating that the low-viscosity hydroxyl silicone oil prepared b...

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Abstract

The invention relates to a synthesis method of low-viscosity hydroxyl silicone oil, which comprises the following steps: by using hexamethylcyclotrisiloxane and a solvent as raw materials and one or more of sodium hydroxide, potassium hydroxide and tetramethylammonium hydroxide as a catalyst, carrying out ring-opening equilibrium, neutralization and desolvation to obtain the transparent low-viscosity hydroxyl silicone oil. The viscosity of the synthesized hydroxyl silicone oil is 20-35 mm <2> / s, and the hydroxyl content is 6-12%.

Description

technical field [0001] The invention belongs to the field of chemical production, and in particular relates to a method for synthesizing low-viscosity hydroxyl silicone oil. Background technique [0002] Silicone products are mainly divided into four categories: silicone oil, silicone rubber, silicone resin and silane coupling agent. Among them, silicone oil and its secondary processing products are one of the most widely used and most consumed varieties of silicone products. Low-viscosity hydroxy silicone oil is also called small molecule hydroxy silicone oil. As an important silicone oil product, it has a good structure control effect and is a structure control agent for preparing high-performance high-temperature vulcanized silicone rubber materials. Generally, it is added in high-temperature rubber formulations. 4~6%. At present, the viscosity of low-viscosity hydroxy silicone oil used in the domestic market is 20-35mm 2 / s, the hydroxyl content is 6-12%. As an import...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/06
CPCC08G77/04C08G77/06
Inventor 李少平李书兵李海娟孙刚陈泽雨李岩松肖靖
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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