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Ternary copper catalyst prepared from copper powder recovered from waste organic silicon contacts and preparation method thereof

A technology of organosilicon waste contacts and catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxides/metal hydroxide catalysts, etc., can solve the problems of high energy consumption, rising copper raw material prices, Problems such as high cost, to achieve the effect of reducing pollution, saving production cost, and easy to oxidize

Inactive Publication Date: 2012-11-21
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of ternary copper catalysts in the above methods all use commercial copper raw materials, the cost is high, the energy consumption is large, and the price of copper raw materials is generally rising at present, and the preparation of copper catalysts is facing huge cost pressure.

Method used

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  • Ternary copper catalyst prepared from copper powder recovered from waste organic silicon contacts and preparation method thereof
  • Ternary copper catalyst prepared from copper powder recovered from waste organic silicon contacts and preparation method thereof
  • Ternary copper catalyst prepared from copper powder recovered from waste organic silicon contacts and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033]Weigh 100.0g waste contact body and add it to 300ml nitric acid solution (3mol / L), stir at 40°C for 5h, then filter under reduced pressure, raise the temperature of the filtrate to 80°C, add 14.0g reduced iron powder, and the solution immediately appears dark The red copper powder was filtered and washed after the reduction reaction was completed, and vacuum-dried at 80° C. for 12 hours to finally obtain 13.5 g of copper powder with a yield of 96%. The copper powder was put into a muffle furnace at 250° C. for calcination and oxidation, and the oxidation time was 4 hours to obtain 15.2 g of partially oxidized copper powder. Take 10.0g of partial copper oxide powder and put it into a ball mill, add 50.0g of ball milling beads (diameter φ=5mm) for ball milling, the ball milling time is 6h, filter and wash after the ball milling, and vacuum dry at 80°C for 12h to obtain the medium particle size (D50) It is a ternary copper catalyst of 1.8μm. Gained copper catalyst is compo...

Embodiment 2

[0041] Weigh 100.0g waste contact body and add it to 100ml concentrated sulfuric acid, stir at 60°C for 5h, then add 200ml deionized water to dilute, after vacuum filtration, heat the filtrate to 70°C, add 15.0g zinc powder, Dark red copper powder appeared immediately. After the reduction reaction was completed, it was filtered and washed, and vacuum-dried at 80° C. for 12 hours to finally obtain 13.3 g of copper powder with a yield of 95%. The copper powder was put into a muffle furnace at 300° C. for calcination and oxidation, and the oxidation time was 3 hours to obtain 15.0 g of partially oxidized copper powder. Take 10.0g of partial copper oxide powder and put it into a ball mill, add 50.0g of ball milling beads (diameter φ=5mm) for ball milling, the ball milling time is 6h, filter and wash after the ball milling, and vacuum dry at 80°C for 12h to obtain the medium particle size (D50) The ternary copper catalyst is 2.0μm. The obtained copper catalyst is composed as follo...

Embodiment 3

[0043] Weigh 100.0g of waste contact body and add it to 250ml of hydrochloric acid solution (3mol / L) containing 10g of hydrogen peroxide, stir at 20°C for 8h, then filter under reduced pressure, heat the filtrate to 80°C, add 14.0g of reduced iron powder, the solution Dark red copper powder appeared immediately in the solution. After the reduction reaction was completed, it was filtered and washed, and vacuum-dried at 80° C. for 12 hours to finally obtain 13.0 g of copper powder with a yield of 93%. The copper powder was put into a muffle furnace at 250° C. for roasting and oxidation, and the oxidation time was 4 hours to obtain 14.8 g of partially oxidized copper powder. Take 10.0g of partial copper oxide powder and put it into a ball mill, add 50.0g of ball milling beads (diameter φ=5mm) for ball milling, the ball milling time is 6h, filter and wash after the ball milling, and vacuum dry at 80°C for 12h to obtain the medium particle size (D50) The ternary copper catalyst is ...

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Abstract

The invention relates to the field of recovery and utilization of waste organic silicon contacts and especially relates to a ternary copper catalyst prepared from copper powder recovered from waste organic silicon contacts and a preparation method thereof. The preparation method comprises the following steps of 1, carrying out an extraction process on waste organic silicon contacts by an oxidizing acid or an oxidant-containing acid liquor at a temperature of 20 to 90 DEG C for 4 to 8 hours, and filtering to obtain a Cu<2+>-containing acid solution, 2, adding a reducing agent into the Cu<2+>-containing acid solution obtained by the step 1 so that Cu<2+> is reduced into copper powder, 3, oxidizing a part of the copper powder obtained by the step 2 to obtain a complex of copper oxide, cuprous oxide and copper, and 4, carrying out ball-milling of the complex of copper oxide, cuprous oxide and copper to obtain the ternary copper catalyst having a particle size of 0.5 to 10 microns. The preparation method saves a copper catalyst production cost and realizes recycle of a copper catalyst used in an organic silicon industry. The ternary copper catalyst obtained by the preparation method has obvious environmental protection benefits and catalytic effects better than catalytic effects of commercial catalysts.

Description

technical field [0001] The invention relates to the field of recycling and utilization of organosilicon waste contacts. Specifically, the invention relates to a ternary copper catalyst prepared from copper powder recovered from organosilicon waste contacts and a preparation method thereof. Background technique [0002] Dimethyldichlorosilane is the most important organosilicon monomer used in the preparation of organosilicon materials and is the foundation and pillar of the entire organosilicon industry. The monomer production process mainly adopts the direct method (Rochow method), that is, copper is used as the main catalyst, other metal powders are used as co-catalysts, and methyl chloride and silicon powder are directly reacted. Due to the limitation of existing technology and reaction kinetics, in the production process of organosilicon, when the conversion rate and selectivity of monomer products reach a certain level, it is necessary to discharge the remaining silicon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72
Inventor 苏发兵车红卫王莹利赵丽润宋莲英贾昭翟世辉朱德洪
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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