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Modified activated carbon carrier, liquid-phase chlorosilane impurity removal adsorbent and production process of adsorbent

A production process and activated carbon technology, applied in halosilanes, silicon compounds, chemical industries, etc., can solve the problems of solar-grade polysilicon, electronic-grade polysilicon, and high impurity content of trichlorosilane, and achieve excellent adsorption effect. , The effect of improving product quality and less equipment investment

Pending Publication Date: 2022-06-07
MULINSEN ACTIVATED CARBON JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in this process, due to the purity of silicon powder and hydrogen chloride, the impurity content of trichlorosilane is high, which in turn easily leads to the low purity of polysilicon obtained by subsequent reduction, which cannot meet the demand for solar-grade polysilicon, let alone electronic-grade polysilicon.
Among them, the impurities are mainly boron and phosphorus compounds which are very close to the boiling points of silicon chloride and trichlorosilane, and if the boron and phosphorus compounds are controlled to the ppb level, the theoretical plate of the rectification column needs about 55-70, which consumes energy larger

Method used

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  • Modified activated carbon carrier, liquid-phase chlorosilane impurity removal adsorbent and production process of adsorbent
  • Modified activated carbon carrier, liquid-phase chlorosilane impurity removal adsorbent and production process of adsorbent
  • Modified activated carbon carrier, liquid-phase chlorosilane impurity removal adsorbent and production process of adsorbent

Examples

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preparation example 1

[0058] A modified activated carbon carrier, the production process of the carrier comprises the following steps:

[0059] A1 oxidation modification: 2 * 10 in ultrasonic frequency 7 In the ultrasonic environment of Hz, the activated carbon was added to the nitric acid solution with a mass concentration of 30% and impregnated for 2h, and the volume ratio of the activated carbon to the nitric acid solution was 1:2, and the activated carbon was oxidation modified to obtain a mixture; A2 post-treatment: after the mixture is filtered, the filter residue is dried at 110 °C for 5h to obtain a modified activated carbon carrier;

[0060] Among them, the activated carbon is 12 to 30 mesh coconut shell granular activated carbon, and the performance is as follows: strength 99.3%, ash 0.8%, specific surface area of 1400m 2 / g, acetic acid adsorption capacity of 580mg / g.

preparation example 2

[0062] A modified activated carbon carrier, the production process of the carrier comprises the following steps:

[0063] A1 oxidation modification: 2 * 10 in ultrasonic frequency 7 In the ultrasonic environment at Hz, the activated carbon was added to the nitric acid solution with a mass concentration of 35% and impregnated for 3h, and the volume ratio of the activated carbon to the nitric acid solution was 1:2, and the activated carbon was oxidation modified to obtain a mixture; A2 post-treatment: after the mixture is filtered, the filter residue is dried at 110 °C for 5h to obtain a modified activated carbon carrier;

[0064] Among them, the activated carbon is 12~30 mesh coconut shell granule activated carbon, and the performance is as follows: 12~30 mesh coconut shell granular activated carbon, strength 99%, ash 0.8%, specific surface area of 1500m 2 / g, acetic acid adsorption amount of 600mg / g.

preparation example 3

[0066] A modified activated carbon carrier, the production process of the carrier comprises the following steps:

[0067] A1 oxidation modification: 2 * 10 in ultrasonic frequency 7 In the ultrasonic environment of Hz, the activated carbon was added to the nitric acid solution with a mass concentration of 40% and impregnated for 3h, and the volume ratio of the activated carbon to the nitric acid solution was 1:2, and the activated carbon was oxidation modified to obtain a mixture; A2 post-treatment: after the mixture is filtered, the filter residue is dried at 110 °C for 5h to obtain a modified activated carbon carrier;

[0068] Among them, the activated carbon is 12 to 30 mesh coconut shell granule activated carbon, and the performance is as follows: 12 ~ 30 mesh coconut shell granule activated carbon, strength 98.5%, ash 0.5%, specific surface area of 1600m 2 / g, acetic acid adsorption amount of 620mg / g.

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Abstract

The invention relates to the technical field of polycrystalline silicon and monocrystalline silicon production, and particularly discloses a modified activated carbon carrier, a liquid-phase chlorosilane impurity removal adsorbent and a production process of the adsorbent. The production process of the modified activated carbon carrier comprises the following steps: oxidizing and modifying activated carbon by using a nitric acid solution, filtering and drying to obtain the modified activated carbon carrier. The production process of the adsorbent using the modified activated carbon carrier comprises the following steps: dispersing the organic active component in a solvent to prepare a dipping solution; then adding the modified activated carbon carrier into the dipping solution for dipping to obtain an adsorbent precursor; and drying the adsorbent precursor to prepare the liquid-phase chlorosilane impurity removal adsorbent. The adsorbent produced by the invention has an excellent adsorption effect on boron and phosphorus compound impurities in liquid-phase chlorosilane, and is beneficial to improving the purity of the liquid-phase chlorosilane; meanwhile, the adsorbent is relatively long in replacement period and relatively low in energy consumption in the actual application process, and meets the industrial production requirements.

Description

Technical field [0001] The present application relates to polysilicon, monocrystalline silicon production technology field, more specifically, it relates to a modified activated carbon carrier, liquid phase chlorosilane impurity removal adsorbent and the production process of the adsorbent. Background [0002] Polysilicon is a direct raw material for the production of monocrystalline silicon, and is also the electronic information basic material for semiconductor devices such as contemporary artificial intelligence, automatic control, information processing, and photoelectric conversion, with a wide range of applications. The impurity content in polysilicon will directly affect the conversion rate of solar photovoltaics, and high-purity polysilicon is an important material for solar photovoltaic new energy. [0003] At present, the methods of producing polysilicon are chemical method and physical method, of which the chemical purification method mainly includes Siemens method, si...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/22B01J20/32B01J20/30C01B33/107
CPCB01J20/20C01B33/10784B01J20/22B01J20/3204B01J20/3231Y02P20/133
Inventor 李佳佳汤海涌
Owner MULINSEN ACTIVATED CARBON JIANGSU
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