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Adsorbing resin for removing impurities from chlorosilane and preparation method of adsorbing resin

A technology of adsorption resin and chlorosilane, which is applied in the field of adsorption resin for chlorosilane impurity removal and its preparation, can solve the problems of reduced purity of chlorosilane and increased production cost, and achieves the effect of strong adsorption capacity and reduced disproportionation effect

Inactive Publication Date: 2021-09-17
青海亚洲硅业半导体有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the applicant found in the research that if the amine group in the adsorption resin is a tertiary amine group, the tertiary amine group can disproportionate with the chlorosilane, resulting in a decrease in the purity of the chlorosilane and an increase in production cost, especially for industrial production of high-purity trichlorotrichlorohydrin. Hydrogen silicon, if the disproportionation reaction occurs between the adsorption resin and chlorosilane, a large amount of by-products will be produced in the production process, and the production needs to be further purified

Method used

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  • Adsorbing resin for removing impurities from chlorosilane and preparation method of adsorbing resin
  • Adsorbing resin for removing impurities from chlorosilane and preparation method of adsorbing resin

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[0015] The embodiment of the present application provides a method for preparing an adsorption resin for impurity removal of chlorosilanes, including:

[0016] The chlorine ball is swelled in an organic solvent and then reacted with a reactant to obtain an initial product; the reactant contains polyamines, and the initial product contains tertiary amines.

[0017] Exemplarily, the chlorine spheres are chloromethylated polystyrene microspheres. Optionally, the organic solvent includes any one of toluene, tetrahydrofuran and 1,2-dichloroethylene. Chloromethylated polystyrene microspheres can swell well in toluene tetrahydrofuran or 1,2-dichloroethylene solution.

[0018] Among them, after the chlorine ball is swelled in the organic solvent, it can undergo a cross-linking reaction with the reactant containing polyamine, and the compound modification of polyamine is introduced on the chlorine ball. It should be noted that the initial product contains both the initial resin and c...

Embodiment 1

[0036] This embodiment provides a method for preparing an adsorption resin for impurity removal by chlorosilanes, which includes:

[0037] Swell chloromethylated polystyrene microspheres in toluene, then add diethylenetriamine, react at a temperature of 90°C for 4 hours to obtain a solution containing the initial product, and then filter to obtain a filtrate, alternating water and ethanol The filtrate was washed to neutral and then vacuum-dried to constant weight to obtain the initial product. Wherein, the mass ratio of chloromethylated polystyrene microspheres to diethylenetriamine is 1:12.

[0038] The initial product was mixed with 0.5wt% potassium permanganate solution, stirred and refluxed at 30°C for 2 hours to obtain an adsorption resin, then cooled, washed until neutral, and vacuum-dried at 80°C. Wherein, the ratio of potassium permanganate solution to initial product is 10mL:1g.

Embodiment 2

[0040] This embodiment provides a method for preparing an adsorption resin for impurity removal by chlorosilanes, which includes:

[0041] Swell chloromethylated polystyrene microspheres in toluene, then add triethylenetetramine, and react at a temperature of 120°C for 5 hours to obtain a solution containing the initial product, then filter to obtain a filtrate, alternately with water and ethanol The filtrate was washed to neutral and then vacuum-dried to constant weight to obtain the initial product. Wherein, the mass ratio of chloromethylated polystyrene microspheres to triethylenetetramine is 1:14.4.

[0042] The initial product was mixed with potassium permanganate solution with a concentration of 1.0wt%, stirred and refluxed at 60°C for 4 hours to obtain an adsorption resin, then cooled, washed until neutral, and vacuum-dried at 80°C. Wherein, the ratio of potassium permanganate solution to initial product is 10mL:1g.

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Abstract

The invention provides an adsorbing resin for removing impurities from chlorosilane and a preparation method thereof, and relates to the technical field of high polymer materials. The preparation method of the adsorbing resin for impurity removal of chlorosilane comprises the following steps: swelling chlorine balls in an organic solvent, and reacting with a reactant to obtain an initial product; wherein the reactant contains polyamine, and the initial product contains tertiary amine; and reacting the initial product with an optimization reagent to convert the tertiary amine into secondary amine, thereby obtaining the adsorbing resin. In the adsorbing resin prepared by the preparation method, tertiary amine is converted into secondary amine, so that the disproportionation effect of chlorosilane can be inhibited.

Description

technical field [0001] The application relates to the technical field of polymer materials, in particular, to an adsorption resin for impurity removal of chlorosilanes and a preparation method thereof. Background technique [0002] With the rapid development of electronic information and solar photovoltaic industries, the market demand for polysilicon is increasing. The hydrogen reduction process of trichlorosilane is the main method to produce polysilicon. The purity of chlorosilane used in it determines the quality of polysilicon. The impurities in chlorosilane include metal chlorides, chlorides and hydrides containing boron and phosphorus, and metal compounds. Wait. Adsorption impurity removal has become a research hotspot in recent years. The effective adsorption component of the adsorption impurity removal resin often used in chlorosilane is amine group. However, the applicant found in the research that if the amine group in the adsorption resin is a tertiary amine gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/32C08F8/00C08F8/24C08F112/08B01J20/26B01J20/30
CPCC08F8/32C08F8/00C08F8/24B01J20/267C08F112/08
Inventor 曹玲玲宗冰鲍守珍蔡延国
Owner 青海亚洲硅业半导体有限公司
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