A method of producing electronic grade hydrofluoric acid

An electronic-grade hydrofluoric acid and hydrofluoric acid technology, applied in the direction of fluorine/hydrogen fluoride, etc., can solve the problems such as the difficulty of applying ultra-high-purity hydrofluoric acid, the inability to absorb hydrogen fluoride gas, and the incomplete separation of arsenic trifluoride, so as to increase the economy. Benefits and environmental benefits, reduced equipment and investment, and improved product purity

Active Publication Date: 2011-12-14
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the reaction of industrial anhydrous hydrofluoric acid and potassium permanganate is generally used, followed by direct distillation and purification to prepare electronic grade hydrofluoric acid, that is, high-purity hydrogen fluoride. The purity of hydrofluoric acid produced by this method is relatively low, especially hydrogen The separation of arsenic trifluoride in hydrofluoric acid is not complete, so the ultra-high-purity hydrofluoric acid produced by this method is difficult to apply in ultra-large-scale integrated circuits (microelectronics industry); at the same time, the process parameters are not easy to control in the production process
In addition, in the current preparation process of electronic grade hydrofluoric acid, because hydrogen fluoride gas cannot be completely absorbed, its tail gas emission is easy to cause pollution to the surrounding environment

Method used

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Embodiment 1

[0021] The method of the present invention specifically comprises the following steps: (1) crude distillation: the anhydrous hydrofluoric acid raw material of 350kg flows out from the storage bottle, adds the crude still of band heat exchanger, in the crude still, controls the crude still If the internal pressure is less than 0.2Mpa, add 5.25kg of potassium permanganate solution to make a large amount of sulfur dioxide and arsenic trifluoride contained in industrial anhydrous hydrofluoric acid form difficult-to-volatilize compounds; Hydrogen oxide, the gas distilled out at a temperature of 30-50°C in the crude distillation still rises continuously, passes through the crude distillation tower, and then enters the water condenser directly installed on the top of the tower, and repeatedly condenses, refluxes, and vaporizes, and the gas, The two phases of the liquid are in close contact repeatedly in the water condenser and the upper part of the crude distillation tower, and the te...

Embodiment 2

[0023] The method of the present invention specifically comprises the following steps: (1) crude distillation: the anhydrous hydrofluoric acid raw material of 250kg flows out from the storage bottle, adds the crude still of band heat exchanger, in the crude still, controls the crude still Internal pressure is less than 0.2Mpa, add 2.5kg (NH4) 2S2O8, make a large amount of sulfur dioxide and arsenic trifluoride contained in industrial anhydrous hydrofluoric acid generate the compound that is difficult to volatilize; Then add 5kg weight percent and be 30% peroxide Hydrogen, the gas distilled out at a temperature of 30-50°C in the crude still rises continuously, passes through the crude distillation tower, and then enters the water condenser directly installed on the top of the tower, and repeatedly condenses, refluxes, and vaporizes. The two phases are repeatedly and closely contacted in the water condenser and the upper part of the crude distillation tower, and the temperature o...

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Abstract

The invention relates to a method for producing electronic-grade hydrofluoric acid, which specifically comprises the following steps: (1) after preheating the measured anhydrous hydrofluoric acid raw material, carry out crude distillation to remove low-boiling substances; After crude distillation, the hydrofluoric acid discharged from the outlet of the condenser is absorbed with ultrapure water, and the absorption is 48-49% aqueous hydrofluoric acid solution; Boiling distiller distillation, hydrogen fluoride liquid gasification to generate ultra-pure electronic grade hydrofluoric acid gas, condensed into 48 ~ 49% aqueous hydrofluoric acid solution, high boiling point substances and heavy metals remain at the bottom of the sub-boiling distiller; (4 ) The semi-finished product of hydrofluoric acid from the sub-boiling distiller of fluoroplastics is filtered through the second stage and finally made into 48% ultra-high-purity hydrofluoric acid finished product through automatic filling. The method of the present invention makes full use of the different boiling points of anhydrous hydrofluoric acid and impurities in anhydrous hydrofluoric acid, and removes different impurities, especially silicon, at different temperatures, so that the impurity content of the obtained ultra-high-purity hydrofluoric acid is reduced to lowest.

Description

technical field [0001] The invention relates to a method for producing electronic-grade hydrofluoric acid, in particular to a method for producing electronic-grade hydrofluoric acid with anhydrous hydrofluoric acid as the main raw material. Background technique [0002] Electronic grade hydrofluoric acid (Hydrofuloric acid, electronic grade) is also called high-purity hydrofluoric acid. Molecular formula HF, molecular weight 20.006. As one of the key basic chemical materials for the manufacture of integrated circuits (IC), electronic grade hydrofluoric acid is mainly used for chip cleaning and corrosion. very important influence. With the rapid development of electronics, information, and communication industries, the requirements for the purity and impurities of reagent hydrofluoric acid are getting higher and higher, and the demand has also increased sharply. The general electronic pure hydrofluoric acid is far from meeting the harshness of the market. The preparation o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/19
Inventor 侯红军刘海霞杨华春于贺华薛旭金陈宏伟韩建军刘海庆尚钟声方志超
Owner DO FLUORIDE CHEM CO LTD
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