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Method preparing catalyzer through liquid phase ball-milling partial reduction method and ternary copper catalyzer

A catalyst and ternary copper technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve difficult ternary copper composite materials, long reaction process, product purity impact, etc. problems, to achieve the effect of easy control of shape and particle size, high product purity, and adjustable component composition

Active Publication Date: 2013-06-05
JIANGXI INST OF RARE EARTHS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above studies all use copper salts as raw materials, and the corresponding acid radical ions are easily carried in the product, and other metal ions are introduced during the adjustment process of pH, which makes the reaction process longer and the purity of the product is affected; moreover, the obtained products are all single-phase Copper or cuprous oxide materials, it is difficult to directly obtain a ternary copper composite material in which copper, cuprous oxide and cupric oxide exist simultaneously

Method used

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  • Method preparing catalyzer through liquid phase ball-milling partial reduction method and ternary copper catalyzer
  • Method preparing catalyzer through liquid phase ball-milling partial reduction method and ternary copper catalyzer
  • Method preparing catalyzer through liquid phase ball-milling partial reduction method and ternary copper catalyzer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Put 5.0g of analytically pure copper oxide powder and 25g of grinding beads into a stainless steel ball mill jar, add 5.0g of water and 0.5g of hydrazine hydrate in turn; grind on a planetary ball mill for 6 hours, filter the resulting product, dry and disperse it, and then The ternary copper catalyst can be obtained; after chemical analysis, the composition is: 10.1% Cu, 51.5% Cu 2 O and 38.4% CuO.

[0043] The ternary copper catalyst material prepared above was subjected to an XRD test on an X'Pert PRO MPD multifunctional X-ray diffractometer produced by Panalytical Company of the Netherlands (Panalytical).

[0044] The particle size analysis of the ternary copper catalyst material prepared above was performed on a Dandong Baite BT-9300Z laser particle size distribution analyzer.

[0045] The surface morphology of the ternary copper catalyst material prepared above was observed with a JSM7100F field emission scanning electron microscope produced by Japan Electronics ...

Embodiment 2

[0050] Put 10.0g of copper oxide powder calcined from copper oxalate, 0.25g of zinc oxide powder and 25g of grinding beads into a grinding pot, add 20.0g of water and 5.0g of formaldehyde in sequence; grind on a stirring mill for 8 hours, and pump the resulting product After filtering, drying and dispersing, the ternary copper catalyst can be obtained; after chemical analysis, the composition is: 20.2% Cu, 33.3% Cu 2 O and 46.5% CuO.

[0051] Figure 4 It is the XRD figure of the copper-based catalyst that embodiment 2 obtains, wherein 2θ=36.4 ° is Cu 2 The characteristic peak of O, the shoulder peak composed of 2θ=35.5° and 2θ=38.7° is the characteristic peak of CuO, and 2θ=43.3° is the characteristic peak of Cu. It can be seen that the catalyst prepared by this method is composed of Cu, Cu 2 A ternary copper catalyst composed of O and CuO.

[0052] Figure 5 For the particle size analysis of the copper-based catalyst obtained in Example 2, it can be seen from the figure ...

Embodiment 3

[0055] Put 5.0g of copper oxide powder oxidized from copper powder and 50g of grinding beads into the drum mill, add 5.0g of water and 10.0g of hydrazine hydrate in turn; grind on the drum mill for 24h, filter the obtained product with suction, dry and disperse After that, the copper-based catalyst can be obtained; after chemical analysis, the composition is: 90.0% Cu, 5.0% Cu 2 O and 5.0% CuO, the particle diameters of which are all less than 50 microns, and most of them are 10-20 microns; the particles of the copper-based catalyst are sheet-like, with a large diameter of about 10-20 microns and a very thick sheet. Thin, substantially less than 1 micron.

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Abstract

The invention relates to a method preparing a copper catalyzer used for dimethyldichlorosilance synthetic reaction through a liquid phase ball-milling partial reduction method. The method includes the steps of taking copper oxide as raw material, adding solvent media containing reducing substances, enabling copper oxide particles to become small and achieve partial reduction through mechanical ball-milling, obtaining the copper-based catalyzer containing the ternary components of copper, cuprous oxide, copper oxide after suction filtration, drying and smashing, and obtaining the ternary copper catalyzer with adjustable components and controllable particles through adjusting the parameters of reducing agent types, concentration and ball-milling conditions. In catalytic reaction of organosilicone monomer synthesis, the catalyzer is high in catalytic activity and selectivity and helpful for improving the processing ability of an existing organosilicone monomer device, reduces production cost, and improves the yield of target products. The method preparing the catalyzer through the liquid phase ball-milling partial reduction method is simple in process, mild in condition and convenient to operate, and brings convenience to achieve large scale production.

Description

technical field [0001] The invention relates to the field of catalysts used in the synthesis reaction of dimethyldichlorosilane, in particular, the invention relates to a method for preparing copper-based catalysts by a liquid-phase ball milling partial reduction method. Background technique [0002] Silicone materials are both inorganic materials (Si-O) and organic materials (Si-CH 3 ) dual performance, not only widely used in civilian use, but also has special military use, which plays an extremely important role in national economic and social development. Dimethyldichlorosilane (Me 2 SiCl 2 , referred to as M 2 ), as the most important monomer used in the preparation of silicone products, is the foundation and important pillar of the silicone industry. m 2 It is synthesized by heating Si powder and monochloromethane (MeCl) under the action of a copper-based catalyst. This is the direct synthesis method invented by E.G. Rochow in 1940. The reaction may also be accom...

Claims

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Application Information

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IPC IPC(8): B01J23/72C07F7/16
CPCC07F7/16B01J23/72B01J23/835B01J23/80B01J37/16
Inventor 苏发兵王莹利宋莲英翟世辉
Owner JIANGXI INST OF RARE EARTHS CHINESE ACAD OF SCI
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