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Method for recycling copper oxide and zinc oxide from organosilicon spent contact mass

A technology of organosilicon waste contact body and copper oxide, which is applied in copper oxide/copper hydroxide, chemical instruments and methods, zinc oxide/zinc hydroxide, etc., can solve the problems of secondary environmental pollution treatment cost, complex process flow, etc. , to achieve the effect of being conducive to large-scale treatment, high economic benefits, and no three-waste emissions

Inactive Publication Date: 2012-11-28
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a copper oxide recovery method for organosilicon waste contacts in order to overcome the problems of complex process flow, easy to cause secondary pollution to the environment and high processing cost in the current organic silicon waste contact body treatment and recovery copper process. and zinc oxide method

Method used

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  • Method for recycling copper oxide and zinc oxide from organosilicon spent contact mass
  • Method for recycling copper oxide and zinc oxide from organosilicon spent contact mass
  • Method for recycling copper oxide and zinc oxide from organosilicon spent contact mass

Examples

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Embodiment 1

[0034]72.0kg of ammonia (25.0wt%) and 34.0kg of ammonium carbonate are added to 250.0kg of water to form a mixed solution (the mol ratio of ammonia to ammonium carbonate is 3.0), and then 100.0kg of waste contacts (containing copper 15.0wt%, zinc 1.5wt%, the mass ratio of ammonia-ammonium salt to waste contact body is 1.06), and stirred in air at 20°C for 8h. After filtering or centrifuging, the solid slag was washed and dried to obtain 80.0kg of silicon powder. Raise the temperature of the mother liquor after centrifugation to 40°C and keep it warm for 10 hours. A large amount of blue-green precipitates will be produced in the solution. At the same time, the released ammonia gas can be absorbed by 10wt% ammonia water and can be recycled as a raw material for impregnating waste contacts. After filtration or centrifugal separation, the precipitate was washed, dried, and calcined at 450° C. for 5 hours to obtain 18.0 kg of finished copper oxide with a purity of 97% and a total re...

Embodiment 2

[0041] 80.0kg of ammonia water (25.0wt%) and 45.0kg of ammonium carbonate are added to 200kg of water to form a mixed solution (the mol ratio of ammonia to ammonium carbonate is 2.5), and then 100.0kg of waste contacts (containing copper 15.0wt%, zinc 1.5 wt%, the mass ratio of ammonia-ammonium salt to waste contact body is 1.25), stirred at 70°C with air for 6h, filtered or centrifuged, washed and dried the solid slag to obtain 78.0kg of silicon powder. Raise the temperature of the separated mother liquor to 80° C. and keep it warm for 5 hours. A large amount of blue-green precipitates will be produced in the solution. At the same time, the released ammonia gas can be absorbed by 10wt% ammonia water and can be recycled as a raw material for impregnating waste contacts. After filtration or centrifugation, the precipitate was washed, dried, and calcined at 500°C for 4 hours to obtain 18.5kg of finished copper oxide with a purity of 96% and a total recovery of 98%. Add 3.5kg of ...

Embodiment 3

[0043] Add 91.0kg of ammonia water (25.0wt%) and 40.0kg of ammonium carbonate into 200kg of water to form a mixed solution (the mol ratio of ammonia to ammonium carbonate is 3.2), then add 100.0kg of waste contacts (containing copper 15.0wt%, zinc 1.5 % by weight, the mass ratio of ammonia-ammonium salt to waste contact body is 1.31), stirred at 100° C. with air for 1 h, filtered or centrifuged, washed and dried the solid slag to obtain 79.5 kg of silicon powder. Raise the temperature of the mother liquor after centrifugation to 100°C and keep it warm for 1 hour. A large amount of blue-green precipitates will be produced in the solution. At the same time, the released ammonia gas can be absorbed by 10wt% ammonia water and can be recycled as a raw material for impregnating waste contacts. After filtration or centrifugation, the precipitate was washed, dried, and calcined at 500°C for 6 hours to obtain 18.2kg of finished copper oxide with a purity of 96% and a total recovery of 9...

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Abstract

The invention relates to the field of recycling of organosilicon spent contact masses, particularly a method for recycling copper oxide and zinc oxide from an organosilicon spent contact mass, which comprises the following steps: 1) extracting a spent contact mass with an oxidizer-containing ammonia-ammonium salt mixed solution at 20-100 DEG C for 1-8 hours, separating to obtain a copper-ammonia zinc-ammonia complex solution and a solid, and washing and drying the solid to obtain silicon powder; 2) evaporating ammonia from the copper-ammonia zinc-ammonia complex solution at 40-100 DEG C for 1-10 hours to precipitate a copper compound precipitate, separating to obtain the precipitate and a zinc-containing mother solution, washing the precipitate, drying and roasting to obtain copper oxide powder; and 3) adding an ammonium salt into the zinc-containing mother solution obtained in the step 2), regulating the temperature to 20-80 DEG C and the pH value to 4-8 to obtain a basic zinc carbonate precipitate, separating, washing, drying and roasting to obtain zinc oxide powder. The yield and purity of the copper oxide obtained by treating the spent contact mass with an ammonia process are respectively higher than 95%.

Description

technical field [0001] The invention relates to the field of recycling organosilicon waste contacts, in particular, the invention relates to a method for recycling copper oxide and zinc oxide from organosilicon waste contacts. Background technique [0002] In the production process of organosilicon, silicon and methyl chloride are used as raw materials for production, and ternary copper catalyst (main catalyst) and zinc (auxiliary agent) are often used to promote the synthesis of organosilicon monomers such as dimethyldichloromethane. When the conversion rate of silicon powder and the selectivity of methyl chlorosilane monomer reach a certain level, it is necessary to discharge the remaining silicon powder and spent catalyst out of the reactor to form industrial waste, which is called organosilicon waste contact body. The main components of the waste contact body are silicon, copper, carbon, zinc, etc., and their weight contents in the waste contact body are 65% to 80%, 3% t...

Claims

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Application Information

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IPC IPC(8): C01G3/02C01G9/02C01B33/021
Inventor 苏发兵车红卫王莹利翟世辉朱德洪
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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