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Method and device for preparing high-purity boron tribromide

A boron tribromide, high-purity technology, applied in the direction of boron halide compounds, etc., can solve the problems of low purity of synthetic products, affecting the performance of high-purity boron bromide, etc., and achieve the effect of less impurities, simple equipment and high purity

Inactive Publication Date: 2011-01-26
GRIMAT ENG INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, manufacturers at home and abroad generally use elemental boron bromination to produce boron tribromide, but the purity of the synthesized product is low. This is because boron powder contains a large amount of metal impurities, such as Mg, Al, Fe, Ca, Cu, Zn, Sn , Ni and other metals and their oxides. After boron powder is brominated, the boron bromide contains unreacted elemental bromine and bromide impurities of the above metals, which affects the performance of high-purity boron bromide.

Method used

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  • Method and device for preparing high-purity boron tribromide
  • Method and device for preparing high-purity boron tribromide
  • Method and device for preparing high-purity boron tribromide

Examples

Experimental program
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Effect test

Embodiment 1

[0036]500g of industrial boron powder (80%-98%) was washed with 5L0.3mol / L hydrochloric acid to make a boron block and put it into a bromination furnace. After the temperature rose to 600°C, 5kg of liquid bromine (> 99.5%) enters the bromination furnace 2 through the pipeline from the bottom after being vaporized by the vaporizer 1, and the gasification temperature is 45° C. to obtain red fuming gas. , react with the 5N high-purity aluminum sheet in the furnace at a temperature of 50°C to obtain white boron bromide gas, the resulting gas is water-cooled to form a white liquid that flows into the collector 4, and the temperature of the collector 4 is controlled so that boron bromide passes through the outlet of the collector. The pipeline enters the fractionation column 5 for fractionation, and the low-boiling point impurities evaporate before boron bromide, while the high-boiling point impurities remain in the collector 4, and the fraction at 102-105°C is selected, which is the...

Embodiment 2

[0040] 500g industrial boron powder (80%-98%) is made into boron block after being washed with 3L1mol / L sulfuric acid and is packed in the bromination furnace 2. After the temperature rises to 850°C, 5kg liquid bromine (>99.5 %) enters the bromination furnace 2 through the pipeline from the bottom after being gasified by the vaporizer 1, and the gasification temperature is 50° C. to obtain red fuming gas. React with 4N high-purity aluminum flakes in the furnace at a temperature of 150°C to obtain white boron bromide gas. The resulting gas is water-cooled to form a white liquid and flows into collector 4. Control the temperature of collector 4 so that boron bromide passes through the pipe from the outlet of the collector. After entering the fractionation column 5 for fractionation, the low-boiling point impurities evaporate before the boron bromide, and the high-boiling point impurities remain in the collector 4, and the fraction at 95-98°C is selected, which is the evaporation ...

Embodiment 3

[0044] 500g industrial boron powder (80%-98%) is made into boron block after being washed with 2L2mol / L nitric acid and is packed in the bromination furnace 2. After the temperature rises to 770° C., 5 kg of liquid bromine (>99.5 %) enters the bromination furnace 2 through the pipeline from the bottom after being gasified by the vaporizer 1, and the gasification temperature is 60° C. to obtain red fuming gas. React with 6N high-purity aluminum flakes in the furnace at a temperature of 100°C to obtain white boron bromide gas. The resulting gas is water-cooled to form a white liquid and flows into collector 4. Control the temperature of collector 4 so that boron bromide passes through the pipeline from the outlet of the collector After entering the fractionation column 5 for fractionation, the low-boiling point impurities evaporate before the boron bromide, and the high-boiling point impurities remain in the collector 4, and the fraction at 117-120°C is selected, which is the eva...

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Abstract

The invention provides a method and a device for preparing high-purity boron tribromide. The method comprises the following steps of: performing acid-washing on industrial boron powder to prepare boron blocks; performing separatory purification on pure chemical liquid bromine, and performing a reaction on the purified liquid bromine and the industrial boron blocks at the high temperature of between 600 and 850 DEG C in a bromination furnace to obtain boron tribromide liquid containing impurities; removing redundant Br2 in boron tribromide by using high-purity aluminum serving as a debromination agent to obtain white boron tribromide gas, and hydrocooling the white boron tribromide gas to form white boron tribromide liquid; and removing high-boiling point and low-boiling point impurities through fractional distillation of a fractional column to obtain a BBr3 product of which the purity is more than 6N, wherein the fractionation temperature of the boron tribromide is between 85 and 120 DEG C. The device for preparing the high-purity boron tribromide is formed by connecting a vaporizer, the bromination furnace, a bromine removing furnace, a collector, the fractional column and a finished product storage tank sequentially through a pipeline made of high-purity quartz glass. The produced boron tribromide has a few impurities and high purity which can reach over 6N, and the method has the advantages of readily available materials, low cost, simple device, small equipment investment and industrialized production.

Description

technical field [0001] The present invention relates to a method and device for preparing high-purity boron tribromide. Industrial boron powder and liquid bromine are used as raw materials, and BBr with a purity greater than 6N is obtained through bromination, bromine removal, rectification and other steps. 3 The product belongs to the technical field of inorganic chemical industry. Background technique [0002] Boron tribromide is a colorless fuming liquid that is corrosive to metals and rapidly decomposes into boric acid and hydrogen bromide when it meets water. Boron tribromide is an excellent demethylation or dealkylation agent, which can be used as a catalyst and intermediate in polymerization, alkylation and acylation reactions, and has been widely used in the pharmaceutical industry. At the same time, in the application of the electronics industry, high-purity boron tribromide can be used as a boron source to dope semiconductors in the pre-diffusion process, and can ...

Claims

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Application Information

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IPC IPC(8): C01B35/06
Inventor 夏文蒋文全窦维喜傅钟臻于丽敏
Owner GRIMAT ENG INST CO LTD
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