A kind of synthesis method of diffusion pump oil

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

Active Publication Date: 2019-02-19
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • 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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  • A kind of synthesis method of diffusion pump oil
  • A kind of synthesis method of diffusion pump oil
  • A kind of synthesis method of diffusion pump oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Embodiment 1: the synthesis of 274 diffusion pump oils

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

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

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

Embodiment 2

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

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

Embodiment 3

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

[0076] The difference between this example and Example 1 is that 2139.6 g of methyltriethoxysilane (12 mol) was added in step (1), and the yield was 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 industry, in particular to a method for synthesizing diffusion pump oil. Background technique [0002] As a high vacuum diffusion pump oil, special methylphenyl silicone oil has extremely low saturated vapor pressure, extremely high ultimate vacuum; excellent chemical stability, oxidation stability and thermal stability. It is 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 is widely used in the fields of national defense and military industry and civilian high vacuum technology. Among them, the 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 Uni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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