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Method for preparing copper(I)-based catalyst used for synthesizing organic silicon monomer

A catalyst and organosilicon technology, which is applied in the field of preparation of copper-based catalysts, can solve the problems of extended catalyst preparation process, cumbersome operation, and high energy consumption, and achieve the effects of easy control, simple preparation process, and avoiding hard agglomeration

Inactive Publication Date: 2011-10-12
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these post-treatment techniques generally need to be carried out in an organic solvent, and finally the organic solvent must be removed, which makes the catalyst preparation process prolong, the operation is cumbersome, and the energy consumption is large.

Method used

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  • Method for preparing copper(I)-based catalyst used for synthesizing organic silicon monomer

Examples

Experimental program
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Effect test

Embodiment 1

[0017] 250g copper sulfate (CuSO 4 ·5H 2 (2, all the same in the following examples) and 58.5g sodium chloride mixed aqueous solution are made into as feed liquid, transfer in the pressure-resistant and corrosion-resistant reaction kettle, then add reducing agent glucose 18g, airtightly heat to 120 ℃, hydrothermal reduction React for 7 hours to generate cuprous chloride crystals, filter after cooling, wash the filtrate successively with dilute hydrochloric acid and ethanol, and vacuum-dry at 70° C. to obtain 80 g of the target product cuprous chloride crystals.

Embodiment 2

[0019] A mixed aqueous solution made of 250g of copper sulfate and 58.5g of sodium chloride was used as a feed liquid, transferred into a pressure-resistant and corrosion-resistant reaction kettle, and then 30g of reducing agent glucose was added, sealed and heated to 140°C, and hydrothermally reduced for 7 hours to form The cuprous chloride crystals were filtered after cooling, and the filtrate was washed successively with dilute hydrochloric acid and ethanol, and vacuum-dried at 70° C. to obtain 85 g of the target product cuprous chloride crystals.

Embodiment 3

[0021] A mixed aqueous solution made of 250g of copper sulfate and 64g of sodium chloride was used as a feed liquid, transferred into a pressure-resistant and corrosion-resistant reaction kettle, and then 36g of reducing agent glucose was added, sealed and heated to 140°C, and hydrothermally reduced for 8 hours to generate chlorine The cuprous chloride crystals were filtered after cooling, the filtrate was washed successively with dilute hydrochloric acid and ethanol, and vacuum-dried at 70° C. to obtain 86 g of the target product cuprous chloride crystals.

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Abstract

The invention discloses a method for preparing a copper(I)-based catalyst used for synthesizing an organic silicon monomer, and belongs to the technical field of chemical engineering. The method comprises the following steps of: (1) dissolving copper (II) salt in a solution A; (2) adding a crystal growth inhibitor, fully stirring, adding an aldehyde group, alcohol group or alcoholic sugar group containing substance serving as a reducing agent, and transferring feed liquor into a pressure-resistant corrosion-resistant reaction kettle; (3) sealing the kettle, heating to the temperature of between 50 and 300DEG C, and ensuring the reaction time is 0.5 to 48 hours; and (4) cooling and filtering the obtained precipitate, and washing and drying by using the conventional method to obtain the regular-shaped target product of copper(I)-based catalyst. The preparation process is simple, is easy to control, and has no harmful gas and waste liquor emission. When the prepared copper(I)-based catalyst is used for synthesizing the organic silicon monomer, the selectivity of the product and the conversion rate of silicon powder can be effectively improved.

Description

technical field [0001] The invention relates to a preparation method of a copper (I)-based catalyst, in particular to a preparation method of a copper (I)-based catalyst used for the synthesis of organosilicon monomers. Background technique [0002] Organosilicon monomers refer to compounds containing Si-C bonds and at least one organic group bonded to silicon atoms, mainly including: methyl chlorosilane (referred to as methyl monomer), phenyl chlorosilane (referred to as phenyl mono body), methylvinylchlorosilane, ethyltrichlorosilane, propyltrichlorosilane, vinyltrichlorosilane, γ-chloropropyltrichlorosilane and fluorosilicone monomer, etc. Among them, methylchlorosilane (including monomethyl, dimethyl, and trimethylchlorosilane) is the most important. Organosilicon materials widely used in industry refer to the general term of high molecular polymers containing O-Si-O main chain and at least one organic group bonded to Si atoms, usually composed of organosilicon monomers...

Claims

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Application Information

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IPC IPC(8): B01J27/122B01J23/72B01J37/10B01J37/16
Inventor 王广建刘光彦张凤霞
Owner QINGDAO UNIV OF SCI & TECH
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