Low phosgene content boron trichloride production device and method

A technology of boron trichloride and production equipment, which is applied in the direction of boron halide compounds, boron halides, etc., can solve problems such as inability to reach, and achieve the effects of reducing possibility, reducing residual chlorine impurity content, and strong controllability

Active Publication Date: 2017-07-18
江西瑞合特种材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Thanks to the rapid development of the global electronics industry, the demand for boron trichloride is increasing, and the requirements for its purity, especially the content of phosgene, are also increasing; and the existing production process, the content of phosgene Above 10ppm-200ppm, it cannot meet the requirements of electronic grade boron trichloride (phosgene content requirement 0.5-10ppm)

Method used

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  • Low phosgene content boron trichloride production device and method
  • Low phosgene content boron trichloride production device and method
  • Low phosgene content boron trichloride production device and method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 6 kg, boron carbide particles 43 with a purity of 97% after pickling and a particle size of 1 to 3 mm are packed into two double-layer reaction tubes 4 of the vertical reaction furnace 3 (the total length of the graphite ring 42 accounts for about 2 / 3 of the total length of the quartz tube 41) , the boron carbide particles 43 loading amount is about 10 mm above the observation hole 32 of the vertical reaction furnace 3, and the average effective reaction cross-sectional area of ​​the double-layer reaction tube 4 is 100 cm 2 After assembling the reaction system, the vertical reaction furnace 3 is heated up to 300°C, and the reaction system is purged by nitrogen (pressure 0.1MPa, flow rate 100m 3 / h) for 1 hour to replace the moisture and air in the system; the double-layer reaction tube 4 continues to heat up to 650 ° C, and after reaching the reaction start temperature, the liquid chlorine is vaporized and buffered and then enters the dryer 1 through a particle size of 1...

Embodiment 2

[0046] 6 kg, boron carbide particles 43 with a purity of 97% after pickling and a particle size of 1 to 3 mm are packed into two double-layer reaction tubes 4 of the vertical reaction furnace 3 (the total length of the graphite ring 42 accounts for about 2 / 3 of the total length of the quartz tube 41) , the boron carbide particles 43 loading amount exceeds about 10 mm above the observation hole 31 of the vertical reaction furnace 3, and the average effective reaction cross-sectional area of ​​the double-layer reaction tube 4 is 100 cm 2 After assembling the reaction system, the vertical reaction furnace 3 is heated up to 300°C, and the reaction system is purged by nitrogen (pressure 0.2MPa, flow rate 200m 3 / h) for 1 hour to replace the moisture and air in the reaction system; the vertical reaction furnace 3 continues to heat up to 750 ° C, and after reaching the reaction start temperature, the liquid chlorine is vaporized and buffered and then enters the dryer 1 through a parti...

Embodiment 3

[0050] 6 kg, boron carbide particles 43 with 97% purity after pickling and a particle size of 1 to 3 mm are packed into 2 double-layer reaction tubes 4 of the vertical reaction furnace 3 (the total length of the graphite ring accounts for about 2 / 3 of the total length of the quartz tube), carbonized The amount of boron particles 43 loaded is about 10 mm above the observation hole 31 of the vertical reaction furnace 3, and the average effective reaction cross-sectional area of ​​the double-layer reaction tube 4 is 100 cm 2 After assembling the reaction system, the vertical reaction furnace 3 is heated to 300°C, and the reaction system is purged by nitrogen (pressure 0.3MPa, flow 300m 3 / h) for 1 hour to replace the moisture and air in the reaction system; the vertical reaction furnace 3 continues to heat up to 850 ° C, and after reaching the reaction start temperature, the liquid chlorine is vaporized and buffered and then enters the dryer 1 through a particle size of 1 mm and a...

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Abstract

The invention relates to a low phosgene content boron trichloride production device. An outlet of a drier is connected with an inlet at the bottom of a vertical reaction furnace; observation holes are formed on the two sides of the vertical reaction furnace; the vertical reaction furnace is internally provided with two fixed double-layer reaction tubes; outer layers of the double-layer reaction tubes are quartz tubes; inner layers of the double-layer reaction tubes are graphite rings internally tangent with the quartz tubes; the graphite rings are filled with boron carbide particles; at the same time, outlets at the upper ends of the double-layer reaction tubes are connected to an inlet of an ash blocker; an outlet of the ash blocker is connected into a condenser; the lower part of the condenser is connected into a storage tank; circulation cooling water is arranged in the condenser and the storage tank; a boron carbide raw material is filled in the double-layer reaction tubes excessively to avoid residual chlorine overflow; at the same time, after boron carbide chlorination reaction, residual carbon is not directly contacted with the quartz tubes; the generation of a phosgene synthesis raw material is avoided; impurity contents of silicon tetrachloride and residual chlorine are reduced; a phosgene content is reduced to below 3ppm; further, the requirement of electronic-grade boron trichloride is met; and a production method is efficient, stable and reliable and can achieve industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical material preparation, in particular to a boron trichloride production device and method with low phosgene content. Background technique [0002] Boron trichloride is a colorless fuming liquid or gas. It is nonflammable and has a pungent acid smell. It decomposes into hydrogen chloride and boric acid when it encounters water, and releases a lot of heat. It decomposes into hydrochloric acid and boric acid ester in alcohol. Boron trichloride has a wide range of uses, and can be used as the basic material of optical fibers and the preparation of diborane, boron fiber, boron powder, and the preparation of boron-containing metal borides such as titanium diboride and pyrolytic boron nitride. The raw material of the compound. At the same time, due to the strong Lewis acid characteristics of its electron-deficient pair, it can be used as an excellent catalyst in many organic reactions. High-purity boron ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/06
CPCC01B35/061Y02P20/10
Inventor 蔡杉蔡京陈永智魏怡清
Owner 江西瑞合特种材料有限公司
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