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Preparation method of boron trifluoride and boron trifluoride mixed gas

A boron trifluoride and mixed gas technology, applied in the field of chemical engineering, can solve the problems of too many gas impurities, unable to further increase the use demand, low boron trifluoride yield, etc., to improve the content of F element, and to achieve high reaction conversion efficiency. , the effect of less by-products

Pending Publication Date: 2022-05-31
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the wet method has the disadvantages of low boron trifluoride yield (up to less than 90%) and many gas impurities; while the dry method can greatly improve the product purity, but there are still some impurity gases such as silicon tetrafluoride
In addition, the fluorine content of conventional boron trifluoride gas is a fixed value (the F / B atomic ratio is 3), which cannot be further increased to meet the needs of different fluorine content.

Method used

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  • Preparation method of boron trifluoride and boron trifluoride mixed gas
  • Preparation method of boron trifluoride and boron trifluoride mixed gas
  • Preparation method of boron trifluoride and boron trifluoride mixed gas

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The fluorination reactor is a circular pipe fluorination reactor, the length of the reaction tube is 4.8m, and the inner diameter is 65mm.

[0034] Before the reaction, the pressure in the reaction tube was pumped to 180Pa by a vacuum pump, and the temperature was normal temperature, and then the reaction gas was slowly added to react, wherein the molar ratio of diborane and fluorine gas was controlled to be 1:19.1, and the mass ratio of diborane was 3.2%; in the specific reaction process, diborane enters the above-mentioned fluorination reactor after adjusting the flow rate to 1.8g / h, and the fluorine-containing mixed gas (the mass percentage of fluorine gas is 86%, and the rest is nitrogen) is adjusted to the flow rate of 55.0 g / h, enter the above-mentioned fluorination reactor to react;

[0035] The mixed gas obtained by the reaction is pressurized to a pressure of 0.15 MPa, and is successively subjected to the first-stage condensation separation and the second-stage...

Embodiment 2

[0038] The difference between this example and Example 1 is that the molar ratio of diborane and fluorine gas is controlled to be 1:16.9, and the mass ratio of diborane is 3.2%; in the specific reaction process, the flow rate of diborane is adjusted to 1.8g Enter the above-mentioned fluorination reactor after / h; the fluorine-containing mixed gas (the mass percentage of fluorine gas is 76%, and the rest is nitrogen) adjust the flow rate to 55.0g / h, enter the fluorination reactor according to the conditions described in Example 1 reaction;

[0039] The mixed gas prepared by the reaction is pressurized to a pressure of 0.25 MPa, and the first stage and the second stage are condensed and separated successively, wherein the first stage separation condensation temperature is controlled at -25 ℃, and the second stage separation condensation temperature is controlled at -125 ℃; after secondary condensation, boron trifluoride liquid is obtained; a sample is detected by gas chromatogra...

Embodiment 3

[0042]The difference between this example and Example 1 is that the molar ratio of diborane and fluorine gas is controlled to be 1:10.0, and the mass ratio of diborane is 1.4%; in the specific reaction process, the flow rate of diborane is adjusted to 0.8g Enter the above-mentioned fluorination reactor after / h, the fluorine-containing mixed gas (the mass percentage of fluorine gas is 70%, and the rest is nitrogen), adjust the flow rate to 55.0g / h, enter the fluorination reactor as described in Example 1 conditioned response;

[0043] The obtained mixed gas is pressurized to a pressure of 0.25 MPa, followed by the first-stage condensation separation and the second-stage condensation separation, wherein the condensation temperature of the first-stage separation is controlled at -25°C, and the condensation temperature of the second-stage separation is controlled at -25°C. At -125° C.; after secondary condensation, boron trifluoride liquid is obtained; a sample is detected by gas...

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Abstract

The invention discloses a preparation method of boron trifluoride and boron trifluoride mixed gas, which comprises the following steps: reacting diborane with fluorine-containing mixed gas in a fluorination reactor to generate a mixture containing hydrogen fluoride, boron trifluoride and inert gas; the fluorine-containing mixed gas is mixed gas of fluorine gas and inert gas, the inert gas is one or a mixture of more than two of nitrogen gas, helium gas and neon gas, and the mass percentage of diborane in the mixture of diborane and fluorine-containing mixed gas is 0-3.3% or 45.6-100%; and condensing and separating the mixture generated by the reaction to obtain boron trifluoride. According to the method, the reaction conversion efficiency is high, complete conversion of diborane can be achieved, meanwhile, by-products are few, purity is high, impurity gas is little, the generated by-product HF can be returned to the procedure of preparing fluorine through electrolysis, and ordered circulation of materials is achieved.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a preparation method of boron trifluoride and a boron trifluoride mixed gas. Background technique [0002] Boron trifluoride is widely used in high-tech fields, especially high-purity boron trifluoride has high added value and significant economic benefits. It is a high-purity gas standard substance that is widely used in the market to meet the urgent needs of petrochemical production and scientific research. At present, the preparation methods of boron trifluoride include wet method and dry method. However, the wet method has the disadvantages of low boron trifluoride yield (up to less than 90%) and many gas impurities. Compared with the dry method, the product purity can be greatly improved, but there are still some impurity gases such as silicon tetrafluoride. In addition, the fluorine content of conventional boron trifluoride gas is a fixed value (F / B atomic ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/06
CPCC01B35/061
Inventor 杨建明石坚吕剑惠丰梅苏宁李佳霖张前袁俊余秦伟肖川
Owner XIAN MODERN CHEM RES INST
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