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purify sicl 4 and/or sihcl 3 The liquid-solid phase photocatalytic purification method of the crude product

A photocatalytic, liquid-solid phase technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problems of Si-Cl bond absorption loss, inferiority, etc.

Active Publication Date: 2017-06-30
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, metal oxides and sulfide semiconductors are used in industrial products SiCl 4 and SiHCl 3 There is no literature report on the purification treatment of impurities in
At present, there have been direct photolysis of about 330nm ultraviolet light to purify industrial SiCl 4 The report of the method (such as Mao Wei et al. in 2010 "Inorganic Salt Industry" 42,37-30), but this kind of method can only remove SiHCl 3 This type of impurity containing Si-H bonds, and because of the use of very short-wavelength UV light, the incident light is absorbed by most of the Si-Cl bonds, which is far inferior to metal oxide photocatalysts such as TiO 2 light utilization efficiency

Method used

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  • purify sicl <sub>4</sub> and/or sihcl <sub>3</sub> The liquid-solid phase photocatalytic purification method of the crude product
  • purify sicl <sub>4</sub> and/or sihcl <sub>3</sub> The liquid-solid phase photocatalytic purification method of the crude product

Examples

Experimental program
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Effect test

Embodiment 1

[0047] P25-TiO 2 (Germany Degussa company) solid 1g, put into 50ml and contain the methanol solution of 0.01gPt ion, N 2 Deoxygenated airtight. Under UV irradiation, Pt was reduced according to conventional methods, and the reaction was terminated after 24 hours of irradiation. The solid was filtered off and washed with deionized water. Centrifuged, washed three times like this, vacuum-dried under the solid room temperature, obtained the surface loaded precious metal Pt (weight 1%) / TiO 2 Photocatalyst particles, the particle size is 0<particle size≤1mm; spare.

[0048] According to Pt(1% by weight) / TiO 2 and SiCl 4 The mass ratio of industrial crude product 1:1000, will 0.1g Pt (weight 1%) / TiO 2 into the loaded SiCl 4In the reboiler of industrial crude products, connect the continuous reflux reactor and keep 0.1MPa of H 2 The reaction atmosphere was irradiated under a 300W xenon lamp for 1 hour, and stirred during the irradiating process to obtain a suspended photocata...

Embodiment 2

[0052] P25-TiO 2 (Germany Degussa company) solid 1g, put into 50ml and contain the methanol solution of 0.01gPt ion, N 2 Deoxygenated airtight. Under UV irradiation, Pt was reduced according to conventional methods, and the reaction was terminated after 24 hours of irradiation. The solid was filtered off and washed with deionized water. Centrifuged, washed three times like this, vacuum-dried under the solid room temperature, obtained the surface loaded precious metal Pt (weight 1%) / TiO 2 Photocatalyst particles, the particle size is 0<particle size≤1mm; spare.

[0053] According to Pt(1% by weight) / TiO 2 and SiCl 4 The mass ratio of industrial crude product 1:1000, will 0.1gPt (weight 1%) / TiO 2 into the loaded SiCl 4 In the reboiler of industrial crude products, connect a continuous reflux reactor, keep the reaction atmosphere as air, and irradiate for 1 hour under a 300W xenon lamp, and stir during the irradiating process to obtain a suspended photocatalytic system aft...

Embodiment 3

[0057] P25-TiO 2 (Germany Degussa company) solid 1g, put into 50ml and contain the methanol solution of 0.01gPt ion, N 2 Deoxygenated airtight. Under UV irradiation, Pt was reduced according to conventional methods, and the reaction was terminated after 24 hours of irradiation. The solid was filtered off and washed with deionized water. Centrifuged, washed three times like this, vacuum-dried under the solid room temperature, obtained the surface loaded precious metal Pt (weight 1%) / TiO 2 Photocatalyst particles, the particle size is 0<particle size≤1mm; spare.

[0058] According to Pt(1% by weight) / TiO 2 and SiCl 4 The mass ratio of industrial crude product 1:1000, will 1g Pt (weight 1%) / TiO 2 into the load with 5 liters of SiCl 4 In the reboiler of industrial crude products, connect the continuous reflux reactor and keep 0.1MPa of H 2 The reaction atmosphere was irradiated under a 300W xenon lamp for 1 hour, and stirred during the irradiating process to obtain a suspe...

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Abstract

The present invention relates to a liquid-solid phase photocatalytic purification method for purifying a SiCl4 and / or SiHCl3 crude product. The method is as follows: semiconductor photocatalyst particles or a semiconductor photocatalyst film are or is placed in the SiCl4 and / or SiHCl3 industrial crude product to obtain a semiconductor-photocatalyst-particle-containing suspension photocatalytic system or a semiconductor-photocatalyst-film-containing film photocatalytic system, then an UV light source, a visible light source or a mixed UV light and visible light source is used for illumination to obtain an illuminated suspension photocatalytic system or film photocatalytic system, and then a SiCl4 or SiHCl3 pure product for production of high quality quartz fiber can be obtained by solid-liquid separation of the illuminated suspension photocatalytic system or film photocatalytic system. The infrared absorption of the obtained purified SiCl4 and / or SiHCl3 can be tested by use of a 10cm optical path of liquid tank, a corresponding OH peak basically disappears, and the maximum absorbance of a corresponding saturated-CH peak is less than 0.5.

Description

technical field [0001] The invention belongs to purified industrial product SiCl 4 and SiHCl 3 The crude product method, especially involves the removal of industrial SiCl by photocatalytic purification method 4 and / or SiHCl 3 A liquid-solid phase photocatalytic purification method for trace soluble impurities in the crude product. Background technique [0002] Industrial SiCl 4 It is generally chlorinated from crude silicon (Si+Cl 2 , 400 ~ 500 ℃) production, more from the industrial by-products of polysilicon production. In the process of producing polysilicon by the traditional Siemens method, about 10-15 tons of SiCl will be produced for every ton of polysilicon produced. 4 by-product. According to statistics in 2012, the production capacity of polysilicon projects under construction and under construction in my country has reached 300,000 tons. When the projects reach production capacity, there may be about 2.7 million to 4.5 million tons of SiCl per year. 4 Req...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/107B01J23/42B01J23/66B01J23/652B01J23/89B01J23/46
Inventor 赵进才马万红闫研籍宏伟陈春城车延科
Owner INST OF CHEM CHINESE ACAD OF SCI