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Method for preparing silicate ester by recycling chlorosilane slag slurry residual liquid

A chlorosilane and silicate technology, which is applied in the field of recovering chlorosilane slurry residue to prepare silicate, can solve problems such as environmental pressure and waste of resources

Active Publication Date: 2014-07-30
吴娟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In view of this, the technical problem to be solved in the present invention is to provide a reasonable and feasible way to treat the chlorosilane slurry residue with an organic solvent, reclaim the useful components in the chlorosilane slurry residue to the greatest extent, and generate extremely Valuable silicate, while creating value, it also solves the problem of waste of resources and environmental pressure caused by the discharge of a large amount of slurry residue in the production process of chlorosilane

Method used

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  • Method for preparing silicate ester by recycling chlorosilane slag slurry residual liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The chlorosilane slurry raffinate treated here is taken from the cold hydrogenation unit in polysilicon production, and its main components are shown in Table 2:

[0050] Table 2 Main components in slurry raffinate

[0051] components main ingredient Content (WT)% Chlorosilane STC 73.0 catalyst CuCl 5.0 Silica fume Si powder 14.0 other High boilers, chlorides 8.0

[0052] Take 200g of chlorosilane slag slurry, let it stand for a period of time, let the solid settle at the bottom of the container, and the upper layer is a relatively clear chlorosilane solution. After the upper layer solution was sucked out, it weighed 116.0g, and its main component was STC, but the impurity content was relatively high, and the main content of STC was 94%. It must be rectified to meet the requirements of cold hydrogenation STC raw material. Nitrogen gas at about 100°C is introduced into the solid to try to blow away the incompletely separa...

Embodiment 2

[0054] Take 200.0 g of the same chlorosilane slag slurry as in Example 1 as the initial raw material, first add about 30.0 g into a 1000 ml reaction flask, and then slowly add the remaining slag residue and 200.0 g of absolute ethanol at the same time at room temperature, while adding While stirring, the temperature of the system gradually increased, and hydrogen chloride gas was continuously generated. Condensate the reaction tail gas with condensed water at 25°C and discharge it into the alkaline solution for absorption. Since the esterification reaction between chlorosilane and ethanol is very fast, the reaction is basically completed after the addition is completed and the stirring is continued for 0.5 h. Stirring was stopped to obtain a viscous yellow-green solution. After standing for a while, it was observed that the solids all sank to the bottom of the reactor, and the upper layer was a cleaner liquid.

[0055] Using a suction filtration device, transfer the reaction ...

Embodiment 3

[0067] Get 20.00g of the silicon powder recovered in Example 1 as the initial material, slowly add it into a reaction flask filled with 100ml of ethanol, stir while adding, heat will be released continuously, if adding too fast or insufficient stirring, bumping will occur, After the addition, start heating and stirring, make the silicon powder and ethanol react under reflux (82°C) for 5 hours, then stop heating. After the reaction solution was cooled to room temperature, the reaction solution was transferred to a suction filter funnel for suction filtration. The filtrate was a viscous slightly yellow liquid, and the filter cake was a black solid. The filter cake was rinsed three times with 30g*3 absolute ethanol, and finally drained to obtain a black solid substance with metallic luster, which weighed 13.6g after drying. The filtrates were combined, and the filtrate was distilled at atmospheric pressure with a distillation device. After all the solvents were evaporated, the di...

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Abstract

The invention provides a method for recycling silicon powder and catalysts and / or preparing silicate ester by treating chlorosilane slag slurry residual liquid by virtue of an organic solvent. By using the special characteristics that chlorosilane is easy to react with some materials to generate corresponding ester and the characteristics that impurity materials in slag slurry residual liquid are easy to be dissolved into some organic solvents, impurities in the chlorosilane slag slurry residual liquid can be effectively removed by adopting the method disclosed by the invention so as to ensure that the silicon powder and / or the catalysts are completely recycled, and valuable silicate ester also can be produced. The method is simple in involved device and convenient and fast in operation; the problems of serious raw material waste and three-waste treatment in the production of polysilicon and various chlorosilanes at present can be solved by adopting the method.

Description

technical field [0001] The invention relates to a method for recovering useful components in chlorosilane slag residue and preparing silicate by using an organic solvent, aiming at recycling chlorosilane, silicon powder and catalyst in chlorosilane slag residue with high efficiency and high quality. Not only can it meet the energy saving and emission reduction requirements of almost 100% recycling of materials, but it can also produce valuable chemical raw material silicate while reducing the cost of production materials and environmental protection pressure, which belongs to the field of environmental protection and new chemical materials. Background technique [0002] In recent years, with the rapid development of the photovoltaic industry, the demand for semiconductor silicon (including polycrystalline silicon, single crystal silicon and thin film silicon) for solar cells is also increasing. Crystalline silicon is the most important photovoltaic material, with a market sh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04C01B33/02
CPCY02P20/584
Inventor 吴娟
Owner 吴娟
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