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Method for producing boron trichloride

A boron trichloride and manufacturing method technology, applied in the direction of boron halide compounds, boron halides, etc., can solve the problems of reduced manufacturing efficiency, blockage of manufacturing pipelines, etc., and achieve the effects of efficient manufacturing and suppression of by-products

Active Publication Date: 2019-01-11
RESONAC CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In these methods for producing boron trichloride, if there is water in the reaction system, the produced boron trichloride is hydrolyzed to lower the production efficiency of boron trichloride.
In addition, there is a problem that boric acid and boron oxide produced by the hydrolysis of boron trichloride may clog the production line of boron trichloride
However, in Patent Document 3, there is no description about the removal of water from boron carbide.

Method used

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  • Method for producing boron trichloride

Examples

Experimental program
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Effect test

Embodiment 1

[0073] use with figure 1 The same boron trichloride manufacturing apparatus as the boron trichloride manufacturing apparatus operates in the same manner as in the above embodiment to react boron carbide and chlorine gas to manufacture boron trichloride. As the chlorine-containing gas, commercially available high-purity chlorine gas having a purity of 99.999% by volume and a water content of 0.9 ppm by volume was used. For boron carbide, the following powder is used: when the particle size is measured through a dry sieve, the undersize of a dry sieve with an opening of 5.60 mm is 100% by mass, and a sieve that cannot pass through a dry sieve with an opening of 1 mm The upper amount is 65% by mass or more.

[0074] Pack 20 g of this boron carbide powder into a tubular reaction vessel made of graphite (with an inner diameter of 22 mm, a height of 700 mm, and a volume of a reaction part filled with boron carbide of 19 cm 3 ), nitrogen with a flow rate of 500ccm was introduced in...

Embodiment 2

[0079] The reaction was carried out in the same manner as in Example 1, except that the following chlorine gas was used instead of the high-purity chlorine gas as the chlorine-containing gas used in the dehydration treatment of boron carbide. That is, commercially available industrial chlorine gas with a purity of 99.9% by volume and a moisture content of 5 ppm by volume is passed through a 1 L SUS cartridge filled with molecular sieve 3A to reduce the moisture content to 1 ppm by volume or less, and the resulting chlorine gas is referred to as chlorine-containing gas. gas use.

[0080] As a result, the reaction was completed in 6 hours, the amount of boron trichloride obtained was 167 g, and the yield was 99% by mass. In addition, the amount of by-generated hydrogen chloride was 1 mg.

Embodiment 3

[0082] The reaction was carried out in the same manner as in Example 1, except that the following gas was used instead of the high-purity chlorine gas as the chlorine-containing gas used in the dehydration treatment of boron carbide. That is, as the chlorine-containing gas, a mixed gas obtained by mixing equal amounts of commercially available high-purity chlorine gas and nitrogen gas and having a water content of 1 volume ppm or less was used.

[0083] As a result, the reaction was completed in 6 hours, the amount of boron trichloride obtained was 167 g, and the yield was 99% by mass. In addition, the amount of by-generated hydrogen chloride was 1 mg.

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Abstract

Provided is a method for producing boron trichloride such that boron trichloride can be efficiently produced by suppressing the generation of byproducts resulting from water by sufficiently removing water from a reaction system. The method for producing boron trichloride includes: a dehydration step of bringing into contact a chlorine-containing gas which contains chlorine gas and has a water content of 1 volume ppm or less with boron carbide at a temperature lower than a generation starting temperature, at which the generation of the boron trichloride starts, by the reaction between the boroncarbide and the chlorine gas, and causing the water in the boron carbide to react with the chlorine gas in the chlorine-containing gas to remove the water contained in the boron carbide; and a generation step of causing the boron carbide dehydrated in the dehydration step to react with the chlorine gas to generate the boron trichloride.

Description

technical field [0001] The present invention relates to the manufacture method of boron trichloride. Background technique [0002] As boron trichloride (BCl 3 ) manufacturing method, boric acid (B(OH) 3 ) loaded on activated carbon to make it react with chlorine gas (Cl 2 ) react method (refer to for example patent document 1, 2), make boron carbide (B 4 C) A method of reacting with chlorine gas (see, for example, Patent Document 3) is known. In these methods for producing boron trichloride, if water exists in the reaction system, the generated boron trichloride is hydrolyzed to lower the production efficiency of boron trichloride. In addition, there is a problem that boric acid and boron oxide produced by the hydrolysis of boron trichloride may clog the production line of boron trichloride. [0003] Therefore, in the method for producing boron trichloride disclosed in Patent Document 1, before reacting boric acid and chlorine gas, moisture contained in boric acid and a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/06
CPCC01B35/061C01P2006/82
Inventor 毛利早纪栗原秀行
Owner RESONAC CORPORATION
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