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Phenoxymethyldisilane and its preparation method

A technology of phenoxymethyldisilane and methylphenoxymethyldisilane, which is applied in the field of phenoxymethyldisilane and its preparation, can solve the problem of short molecular chain segments, less research on silicone oil, and easy increase in viscosity Large and other problems, to achieve the effect of outstanding heat resistance, convenient product purification, and controllable structure

Inactive Publication Date: 2016-07-13
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the structure of silicone oil is mainly polysiloxane, which can be subdivided into hydrocarbon-based silicone oil, carbon-functional silicone oil, silicon-functional silicone oil and inactive modified silicone oil. Used as heat transfer oil
Other silicone oil structures such as Si-C, carbosilicon and other structures are difficult to crosslink under high temperature conditions due to the short molecular chain, and their viscosity changes little at high temperature, which is suitable for the application of high temperature heat transfer oil. Less research on silicone oil

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The etherification reaction prepares phenoxymethyldisilane, and the main steps are as follows:

[0046] a, ingredients: take high-boiling point chlorosilane waste liquid and phenol; carry out etherification reaction according to the molar ratio of chlorine atoms in high-boiling point chlorosilane waste liquid: phenol is 1:1.1; the content of chlorine atoms in high-boiling point chlorosilane waste liquid Alkali titration is 13mol / L;

[0047] b. Etherification reaction: first add 538g of phenol (5.72mol) into a round bottom flask equipped with a constant pressure dropping funnel, anhydrous calcium chloride drying tower, and HCl tail connector, and add 400mL of phenol into the constant pressure dropping funnel. (containing 5.2mol of chlorine) high-boiling point chlorosilane waste liquid, slowly add the high-boiling point chlorosilane waste liquid into the reaction device at 40°C; There is no longer any HCl release in the receiver;

[0048] c. Separation and purification:...

Embodiment 2

[0051] The etherification reaction prepares phenoxymethyldisilane, and the main steps are as follows:

[0052] a. Ingredients: take high-boiling point chlorosilane waste liquid and phenol; carry out etherification reaction according to the molar ratio of chlorine atoms in high-boiling point chlorosilane waste liquid: phenol is 1:1; the content of chlorine atoms in high-boiling point chlorosilane waste liquid Alkali titration is 13mol / L;

[0053] b. Etherification reaction: First, add 489g of phenol (5.2mol) into a round bottom flask equipped with a constant pressure dropping funnel, anhydrous calcium chloride drying tower, and HCl tail connector, and add 400mL of phenol into the constant pressure dropping funnel. (containing 5.2mol of chlorine) high-boiling point chlorosilane waste liquid, slowly add the high-boiling point chlorosilane waste liquid into the reaction device at 40°C; There is no longer any HCl release in the receiver;

[0054] c. Separation and purification: a...

Embodiment 3

[0057] The etherification reaction prepares phenoxymethyldisilane, and the main steps are as follows:

[0058] a. Ingredients: take high-boiling point chlorosilane waste liquid and phenol; carry out etherification reaction according to the molar ratio of chlorine atoms in high-boiling point chlorosilane waste liquid: phenol is 1:1; the content of chlorine atoms in high-boiling point chlorosilane waste liquid Alkali titration is 13mol / L;

[0059] b. Etherification reaction: first add 587g of phenol (6.24mol) into a round bottom flask equipped with a constant pressure dropping funnel, anhydrous calcium chloride drying tower, and HCl tail connector, and add 400 mL of phenol into the constant pressure dropping funnel. (containing 5.20 mol of chlorine) high-boiling point chlorosilane waste liquid, slowly add the high-boiling point chlorosilane waste liquid into the reaction device at 40°C; There is no longer any HCl release in the receiver;

[0060] c. Separation and purification...

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Abstract

The invention discloses phenoxylmethyl siloxane shown as the formula (I) and a preparation method of phenoxylmethyl siloxane. The preparation method of the compound comprises the following steps of: taking raw materials according to the mole ratio of helium atoms in high-boiling-point chlorosilane waste liquid to phenol being 1: (1-1.5); adding phenol into a reactor, and dropwise adding the high-boiling-point chlorosilane waste liquid into the reactor at the temperature of 40 DEG C; after the dropwise adding operation is ended, heating to 60-100 DEG C, and reacting for 8-13h until no HCl is discharged; and carrying out reduced pressure distillation on the reacted materials, removing byproducts distilled at the temperature lower than 170 DEG C and incompletely-reacted phenol, and then, collecting a fraction, i.e., phenoxylmethyl siloxane as a product distilled at the temperature of 230-260 DEG C. The high-boiling-point chlorosilane waste liquid as an industrial waste is used as the raw material, and obtained phenoxylmethyl siloxane has good thermal stability, oxidation resistance and a high flash point and is suitable for hydraulic oil, diffusion pump oil and conduction oil. The formula of phenoxylmethyl siloxane is shown as (RO)nSi-Si(CH3)6-n (I).

Description

technical field [0001] The invention belongs to a silicon compound and a method for preparing the silicon compound by mainly using waste, and relates to a phenoxymethyldisilane and a preparation method thereof. The phenoxymethyldisilane compound obtained by the invention can be applied to heat-resistant and oxidation-resistant heat-conducting oils. Background technique [0002] Silicone monomers (methylchlorosilane, phenylchlorosilane, vinylchlorosilane, etc.) are the basis for the development of the entire silicone material industry, and the production of methylchlorosilane is the backbone of the development of the silicone industry. At present, the industrial production of organosilicon mainly adopts the direct synthesis of copper catalyzed chloroform and silicon powder to prepare methylchlorosilane, while organosilicon chemical industry produces organosilicon products by direct method, and a large amount of by-products (15% of the total output) are also produced. ~25%), ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/02C09K5/10
Inventor 杨军校刘天洋曹克黄亚文
Owner SOUTHWEAT UNIV OF SCI & TECH
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