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Preparation method of high-purity hydrogen bromide

A hydrogen bromide, high-purity technology, applied in directions such as hydrogen bromide, bromine/hydrogen bromide, etc., can solve problems such as leakage, and achieve the effects of reducing easy explosion, high product stability, and easy large-scale production

Active Publication Date: 2021-09-17
绿菱电子材料(天津)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Bromine is used when it is produced and used, which solves the risk of leakage during the bromine feeding process, and at the same time saves the storage, transportation and waste packaging of bromine.

Method used

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  • Preparation method of high-purity hydrogen bromide
  • Preparation method of high-purity hydrogen bromide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Step S1: prepare a 40% sodium bromide solution in an environment protected by nitrogen gas.

[0045] S2 step: purging all containers after cleaning and drying with nitrogen, under nitrogen protection atmosphere, add 2.5kg sodium bromide solution in the bromine generator, at this moment, under the condition of stirring, the control reactor temperature is 15 °C, the amount of chlorine gas introduced was 3L / min, and the reaction time was 1.5h.

[0046] Step S3: Slowly increase the temperature of the bromine generator, the temperature is controlled at 65° C., the pressure is 0.03 MPa, the bromine is evaporated, and the moisture in the bromine is removed through a drying tower.

[0047] Step S4: the bromine flow after drying is controlled at 1m 3 / h into a fixed bed preheated at 340°C and filled with catalyst, and the amount of hydrogen introduced at this time is 1.5m 3 / h to prepare crude hydrogen bromide.

[0048] Step S5: the crude hydrogen bromide is cooled by cooling...

Embodiment 2

[0051] Step S1: prepare a 35% sodium bromide solution in an environment protected by nitrogen gas.

[0052] S2 step: purging all the containers after cleaning and drying with nitrogen, under nitrogen protection atmosphere, add 2.5kg sodium bromide solution in the bromine generator, at this moment, under the condition of stirring, control the reactor temperature to be 25 ℃, the amount of chlorine gas introduced is 2.5L / min, and the reaction time is 2h.

[0053] Step S3: Slowly increase the temperature of the bromine generator, the temperature is controlled at 60° C., the pressure is 0.03 MPa, the bromine is evaporated, and the moisture in the bromine is removed through a drying tower.

[0054] Step S4: the bromine flow after drying is controlled at 1m 3 / h into a fixed bed preheated at 340°C and filled with catalyst, and the amount of hydrogen introduced at this time is 1.5m 3 / h to prepare crude hydrogen bromide.

[0055] Step S5: the crude hydrogen bromide is cooled by coo...

Embodiment 3

[0058] Step S1: prepare a 50% lithium bromide solution in an environment protected by nitrogen gas.

[0059] Step S2: purging all the containers after washing and drying with nitrogen, and adding 2.5 kg of lithium bromide solution to the bromine generator under nitrogen protection atmosphere, at this time, under the condition of stirring, the temperature of the reactor is controlled to be 20 ° C, The amount of chlorine gas introduced was 2.8L / min, and the reaction time was 3h.

[0060] Step S3: Slowly increase the temperature of the bromine generator, the temperature is controlled at 60° C., the pressure is 0.03 MPa, the bromine is evaporated, and the moisture in the bromine is removed through a drying tower.

[0061] Step S4: the bromine flow after drying is controlled at 1m 3 / h enters the fixed bed preheated at 360°C and filled with catalyst, and the amount of hydrogen introduced at this time is 2m 3 / h to prepare crude hydrogen bromide.

[0062] Step S5: the crude hydro...

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Abstract

The invention provides a preparation method of high-purity hydrogen bromide, and relates to the field of preparation of inorganic compounds. The preparation method mainly comprises the following steps: under the protection of inert gas, introducing chlorine into a metal bromide solution to prepare a mixture of bromine and metal chloride; and slowly raising the temperature, blowing out bromine, dehydrating the blown bromine through an adsorption tower, feeding the dehydrated bromine into a fixed bed filled with a catalyst, simultaneously introducing hydrogen into the fixed bed for reaction to prepare a hydrogen bromide crude product, condensing, adsorbing and dehydrating the hydrogen bromide crude product, and then, rectifying through a two-stage rectifying tower to prepare the high-purity hydrogen bromide. Chlorine and metal bromide are adopted as raw materials, and the raw materials are convenient and easy to obtain; bromine is generated in the reaction process and then reacts with hydrogen, so that the problems of bromine storage and transportation, waste packaging material treatment and the like are solved. Meanwhile, the method is simple and stable in reaction, easy to operate and control and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic compounds, in particular to a preparation method of high-purity hydrogen bromide. Background technique [0002] High-purity electronic grade HBr is mainly used for polysilicon etching in the manufacturing process of 8-inch and 12-inch chips, and is one of the core gases in advanced chip manufacturing processes. In addition, due to its ability to act as a catalyst or reactant, hydrogen bromide is used by the semiconductor industry as one of the candidate etching gases for processing large trench structures in the future less than 7nm process. High-purity electronic-grade hydrogen bromide special gas has unique etching and deposition characteristics, and it is difficult to be replaced by other special gases in the short term. It has become the "bottleneck" of the current advanced process materials for integrated circuits. [0003] The raw material hydrogen bromide used for high-purity electr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B7/09
CPCC01B7/093
Inventor 王维佳张杰杨振建舒冬永李广新穆迪
Owner 绿菱电子材料(天津)有限公司
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