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Diffusion pump oil synthesis method

A synthesis method and technology of diffusion pump oil, applied in the direction of silicon organic compounds, etc., can solve the problems of difficulty in rectification separation, high energy consumption, low product purity, etc., and achieve the effect of reducing purification energy consumption and energy consumption.

Active Publication Date: 2017-02-01
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: (a) it is necessary to rectify and separate high-boiling methyldiphenylethoxysilane and methylphenyldiethoxysilane, which has high energy consumption; (b) adopts a highly irritating and carcinogenic Toxic pyridine or amines are used as condensation reaction catalysts and acid binding agents, and the investment in environmental protection and occupational health is high
The disadvantage of the method is (a) that high-boiling dimethyltetraphenyldisilane and 274 or 275 need to be rectified and separated, and the energy consumption is high; (b) due to the equilibrium method, the product components are complex, mainly including dimethyltetraphenyldisilane Disilane, 274 and 274 homologues increase the difficulty of rectification separation, resulting in low purity products

Method used

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  • Diffusion pump oil synthesis method

Examples

Experimental program
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Effect test

Embodiment 1

[0064] Example 1: Synthesis of 274 diffusion pump oil

[0065] This embodiment is the synthesis of 274 diffusion pump oil, which specifically includes the following steps:

[0066] (1) Prepare liquid A with 150ml of absolute ethanol, 54g of distilled water (3mol) and 2 drops of concentrated hydrochloric acid (concentration of 36.5 to 37.5%) and add them to a 250ml constant pressure dropping funnel for later use.

[0067] Add 1283.8g of methyltriethoxysilane (7.2mol) into a 2000ml three-necked flask, stir and slowly drop A liquid under cooling in an ice-water bath, and continue to react in an ice-water bath for 2 hours after dripping for 3 hours. Finally, the reaction product is distilled to 90°C to remove most of the ethanol, and the temperature is reduced to 60°C, and then the remaining ethanol and excess methyltriethoxysilane are removed by distillation under reduced pressure. The temperature of the solution reaches 120°C, the vacuum degree is -0.095MPa, and the solution is mainta...

Embodiment 2

[0073] Example 2: Synthesis of 274 diffusion pump oil

[0074] The difference between this embodiment and embodiment 1 is that 1123.3 g of methyltriethoxysilane (6.3 mol) is added in step (1), and the yield is 85% based on methyltriethoxysilane.

Embodiment 3

[0075] Example 3: Synthesis of 274 diffusion pump oil

[0076] The difference between this embodiment and embodiment 1 is that 2139.6 g of methyltriethoxysilane (12 mol) is added in step (1), and the yield is 51% based on methyltriethoxysilane.

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Abstract

The invention relates to the chemical industry field, particularly to a diffusion pump oil synthesis method, which specifically comprises: (1) carrying out a hydrolysis reaction on methyl triethoxysilane to obtain 1,3-dimethyl-1,1,3,3-tetraethoxydisiloxane (short for compound B); (2) under a strong alkali condition, carrying out balanced telomerization on the compound B and a dimethyl ring body or methylphenyl ring body to obtain a compound D; (3) carrying out a sodium condensation reaction on the compound D, chlorobenzene and sodium to obtain the diffusion pump oil. According to the present invention, the reaction order is re-combined, and the method has advantages of low energy consumption and environmentally friendly process compared to the method in the prior art.

Description

Technical field [0001] The invention relates to the field of chemical engineering, in particular to a method for synthesizing diffusion pump oil. Background technique [0002] As a high-vacuum diffusion pump oil, special toluene-based silicone oil has extremely low saturated vapor pressure, extremely high ultimate vacuum; excellent chemical stability, oxidation stability and thermal stability. Suitable for high vacuum diffusion pumps, such as cathode ray tubes, capacitor coating systems, ultra-pure silicon production, optical instrument coatings, mass spectrometers and other high vacuum systems. It has a wide range of applications in the field of national defense, military industry and civil high vacuum technology. Among them, methyl phenyl silicone oil with the following two structures has the best effect. [0003] [0004] Structure I is 1,1,5,5-tetraphenyl-1,3,3,5-tetramethyltrisiloxane, which is called 274 diffusion pump oil in China and 704 diffusion pump oil in the United S...

Claims

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Application Information

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IPC IPC(8): C07F7/08
Inventor 张建新李志超宋振虎涂世俭
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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