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Method for preparing phenyl-containing mixed cyclic siloxane

A technology of phenyltrichlorosilane and methylphenyldichlorosilane is applied in the field of phenyl-containing mixed bad siloxane, can solve the problem of not finding phenyl-containing mixed cyclosiloxane and the like, and achieves low cost and raw materials. Easy-to-obtain, widely-applied effects

Inactive Publication Date: 2008-07-30
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In previous reports, there was no research on the preparation of phenyl-containing mixed cyclosiloxanes directly using methylphenyldichlorosilane and dialkyldichlorosilane containing phenyltrichlorosilane produced by heat shrinkage as raw materials.

Method used

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  • Method for preparing phenyl-containing mixed cyclic siloxane

Examples

Experimental program
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Embodiment 1

[0029] In a 2000ml three-necked flask equipped with stirring, a thermometer and a dropping funnel, add 510g of water, 100g of gasoline, drop in 387g of dimethyldichlorosilane (dropping time is 2.5h) and 120g of methylbenzene produced by heat shrinkage A mixture of phenyldichlorosilane (the content of phenyltrichlorosilane is 4.0%). The hydrolysis temperature is 30°C. After the dropwise addition is completed, the reaction is continued for 1 h. Leave to layer, wash to neutral. Gasoline was distilled off to obtain 300g colorless and transparent hydrolyzed material with a yield of 98%. The obtained hydrolyzed material was placed in a 500mL device thermometer and a reaction flask of a vacuum distillation device, 7.0g of lithium hydroxide was added, the temperature was raised to 290°C at 10mmHg, and 255g of fractions were collected. The yield was 85.0%. Analyzed by color-mass spectrometry, (Me 2 SiO) n The total content of (MePhSiO) (n=2,3,4,5) is 45%, (Me 2 SiO) n (MePhSiO) ...

Embodiment 2

[0031] In a 2000ml three-necked flask equipped with stirring, a thermometer and a dropping funnel, add 1000g of water, 200g of toluene, drop in 387g of dimethyldichlorosilane (dropping time is 2.0h) and 70g of methylbenzene produced by heat shrinkage A mixture of phenyldichlorosilane (8.0% phenyltrichlorosilane content). The hydrolysis temperature was 70°C. After the dropwise addition was completed, the reaction was continued for 1.5 hours. Leave to layer, wash to neutral. The toluene was evaporated to obtain 258g of colorless and transparent hydrolyzed material with a yield of 95%. The obtained hydrolyzed material was placed in a 500mL device thermometer and a reaction flask of a vacuum distillation device, 5.2g of potassium hydroxide was added, the temperature was raised to 250°C at 5mmHg, and 229g of fractions were collected. The yield was 89%. Analyzed by color-mass spectrometry, (Me 2 SiO) n The total content of (MePhSiO) (n=2,3,4,5) is 38%, (Me 2 SiO) n (MePhSiO) ...

Embodiment 3

[0033] In a 2000ml three-necked flask equipped with stirring, a thermometer and a dropping funnel, add 300g of water, 70g of n-hexane, drop in 387g of dimethyldichlorosilane (dropping time is 3.0h) and 300g of methyl Mixture of phenyldichlorosilane (6.0% phenyltrichlorosilane content). The hydrolysis temperature is 40°C. After the dropwise addition is completed, the reaction is continued for 0.5h. Leave to layer, wash to neutral. The n-hexane was distilled off to obtain 417g of colorless and transparent hydrolyzed material, with a yield of 96%. The obtained hydrolyzed material was placed in a 1000 mL device thermometer and a reaction flask of a vacuum distillation device, 20.0 g of sodium hydroxide was added, the temperature was raised to 290 °C at 20 mmHg, and 379 g of fractions were collected. The yield was 91%. Analyzed by color-mass spectrometry, (Me 2 SiO) n The total content of (MePhSiO) (n=2,3,4) is 8%, (Me 2 SiO) n (MePhSiO) 2 The total content of (n=1,2,3) is ...

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Abstract

The invention discloses a preparation method for organosilicon, in particular to a preparation method for hydrocyclosiloxane containing phenyl. The invention adopts the steps that dialkyl dichlorosilane and the mixture of methyl phenyl dichlorosilane produced through a thermal shrinkage method are uniformly mixed and slowly added into a water insoluble nonpolar organic solvent charged with water, and complete hydrolytic reaction is performed at 0 to 80 DEG C; an organic layer is taken out, and is washed through water to be neutral, the organic solvent is removed, and thus hydrolytic material is obtained; the hydrolytic material and a catalyst are then added into a reactor, the temperature is raised to be 250 to 300 DEG C gradually under the condition that the vacuum degree is not lower than 20 mmHg, the hydrocyclosiloxane is generated through cracking, and hydrocyclosiloxane mixture containing phenyl and dialkyl cyclic siloxane is obtained after condensation. The invention has the advantages of easy obtaining of raw material, and low cost, etc., thereby being widely applied to aviation and spaceflight, electronics, machinery, and other industries.

Description

technical field [0001] The invention belongs to a method for preparing organosilicon, in particular to a method for phenyl-containing mixed bad siloxane. technical background [0002] A series of methylphenyl silicone materials such as methylphenyl silicone oil and methylphenyl silicone rubber are widely used in aerospace due to their excellent high and low temperature resistance, radiation resistance, physiological inertness, and electrical properties. , electronic and electrical, transportation, medical and health, people's daily life, etc., has increasingly become an important new type of silicone polymer in the national economy. Phenyl-containing mixed cyclosiloxane is one of the necessary raw materials for the preparation of methylphenyl silicone materials, and has important application value. [0003] Methylphenyldichlorosilane is one of the important organic silicon raw materials. There are three main production methods: (1) Thermal condensation method, that is, meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 李美江来国桥蒋剑雄邱化玉苏丽金哲
Owner HANGZHOU NORMAL UNIVERSITY
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