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Preparation method of alkyl cyclosiloxane

A technology of hydrocarbyl cyclosiloxane and hydrocarbyl halosiloxane, which is applied in the field of preparation of hydrocarbyl cyclosiloxane, can solve the problems of production hidden dangers and low boiling point of ether, and achieve the effect of saving production costs

Inactive Publication Date: 2015-01-21
江西多林科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ether is recognized as a solvent, with a yield of 80.46%. Ether has a low boiling point and is flammable, which brings hidden dangers to production

Method used

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  • Preparation method of alkyl cyclosiloxane
  • Preparation method of alkyl cyclosiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The hydrolysis experiment of alkylchlorosilane was carried out in a 500ml three-necked flask equipped with a thermometer, a constant pressure dropping funnel and a reflux condenser (the top led out HCl gas). Under magnetic stirring, 95 g of methyldichlorosilane was uniformly dropped into a three-necked flask filled with 95 g of water and 95 g of 6-crown-2. The reaction temperature was controlled below 20°C. After the dropwise addition, the reaction was continued at the same temperature for 0.5 hours, and then the reaction solution was transferred to a separatory funnel for static separation. The supernatant liquid is carried out rectification under reduced pressure, obtains trimethylhydrocyclotrisiloxane (D 3 H ), tetramethylhydrocyclotetrasiloxane (D 4 H ), pentamethylhydrocyclopentasiloxane (D 5 H ), hexamethylhydrocyclohexasiloxane (D 6 H ). The content of each component was analyzed by gas chromatography, and the results are shown in Table 1. After vacu...

Embodiment 2

[0021] The solvent 6-crown-2 in Example 1 was replaced with 9-crown-3 (95 grams), and the others remained unchanged. According to embodiment 1 step operation, the results are shown in Table 1.

Embodiment 3

[0023] The solvent in Example 1 was changed to 12-crown-4, and the others remained unchanged. Operation by embodiment 1, see table 1.

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Abstract

The invention discloses a preparation method of alkyl cyclosiloxane. The preparation method is characterized by comprising the following steps: taking alkyl halogenosilane as a raw material, taking crown ether as a solvent and dropping the alkyl halogenosilane in a mixed solution formed by water and the crown ether while continuously stirring the alkyl halogenosilane; carrying out hydrolysis at a certain temperature to carry out condensation polymerization; standing after the reaction to carry out layering; and directly carrying out decompressed rectification on the obtained hydrolyzed oil to separate trialkylcyclotrisiloxane, tetraalkylcyclotetrasiloxane, pentaalkylcyclopentasiloxane and hexaalkylcyclohexasiloxane. The preparation method has the advantages that alcohols and low-boiling point hydrocarbons are not used as solvents, the crown ether is used as solvent and direct rectification is carried out on the prepared hydrolyzed oil to obtain the alkyl cyclosiloxane, so that the processes of washing, neutralization, drying and filtering are saved; and the solvent which undergoes standing and layering after the hydrolysis can be reused or can be cooled to a certain temperature to separate out the crown ether for recovery, so that the production cost is saved.

Description

technical field [0001] The invention relates to a method for preparing hydrocarbyl cyclosiloxane, in particular to a method for preparing hydrocarbyl cyclosiloxane by using crown ether as a solvent. Background technique [0002] Crown ether is a general term for a class of macrocyclic compounds containing multiple oxygen atoms, and is a heterocyclic organic compound. The common ones are 15-crown-5, 18-crown-6, and the simplest is 6-crown-2. [0003] Hydrocarbyl cyclosiloxane, especially methylhydrogen cyclosiloxane, is a good sealing material for the electronics industry, and it can also be used to prepare hydrogen-containing silicone oil with Si-H bond function, long-chain alkyl silicone oil, polyether silicone oil, epoxy Silicone oil, carboxyl silicone oil, amino silicone oil. It is also used as a crosslinking agent and anti-yellowing agent for silicone rubber. Methyl vinyl cyclosiloxane has been an important raw material for the preparation of silicone rubber, silicone...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 李建勇李凤仪李建辉
Owner 江西多林科技发展有限公司