A method for removing impurity arsenic in electronic grade hydrochloric acid

An electronic grade, hydrochloric acid technology, applied in chemical instruments and methods, halogen/halogen acid, chlorine/hydrogen chloride purification, etc., can solve problems such as removal, unqualified products, and failure of arsenic ions, so as to ensure safety and stability, and stable product quality Effect

Active Publication Date: 2021-04-02
SUZHOU CRYSTAL CLEAR CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the arsenic ion in the impurity presents positive trivalent in hydrochloric acid, trivalent arsenic and chloride ion form arsenic trichloride, and the boiling point of arsenic trichloride is 130.2°C, which is very similar to the temperature of hydrochloric acid distillation, so arsenic ion cannot be used Removal by distillation, so that if only the impurity ions are removed by distillation, the product will be unqualified

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) the concentration of 1000kg is that the hydrochloric acid solution raw material of 35% is put into oxidation device, and add the chlorine gas that is 0.05% of hydrochloric acid solution raw material quality, utilize mechanical arm to carry out slow and uniform stirring then, stirring time is 30min, to hydrochloric acid The arsenic in the tank is oxidized; wherein, the oxidation device is an integrated container made of steel, the inner wall of the oxidation device is provided with a polymer lining, and the bottom has a polytetrafluoroethylene substrate;

[0029] (2)) After stirring, cover the sealing cover on the oxidation device to seal the solution after stirring, and then leave it for 3 hours. During the standing process, according to the pressure value of the online pressure detection device Adjust the air pressure at any time to ensure a stable air pressure;

[0030] (3) After standing still, the oxidation device is uncapped, and then in the solution, add respe...

Embodiment 2

[0036] (1) the concentration of 1000kg is that the hydrochloric acid solution raw material of 35% is put into oxidation device, and add the hydrogen peroxide solution that is 0.1% of hydrochloric acid solution raw material quality, utilize mechanical arm to carry out slow uniform stirring then, the stirring time is 40min, to oxidize arsenic in hydrochloric acid;

[0037] (2)) After stirring, cover the sealing cover on the oxidation device to seal the solution after stirring, and then leave it for 3 hours. During the standing process, according to the pressure value of the online pressure detection device Adjust the air pressure at any time to ensure a stable air pressure;

[0038] (3) After standing still, the oxidation device is uncapped, and then in the solution, add respectively twice the activated carbon adsorbent that is 4% of the concentrated hydrochloric acid solution quality of the raw material, and charge high-purity nitrogen to carry out pressurized adsorption, addin...

Embodiment 3

[0044] (1) the concentration of 1000kg is that 35% hydrochloric acid solution raw material is put into oxidation device, and add the hypochlorous acid solution that is hydrochloric acid solution raw material quality 0.3%, utilize mechanical arm to carry out slow uniform stirring then, stirring time is 50min, to oxidize arsenic in hydrochloric acid;

[0045] (2)) After stirring, cover the sealing cover on the oxidation device to seal the solution after stirring, and then leave it for 3 hours. During the standing process, according to the pressure value of the online pressure detection device Adjust the air pressure at any time to ensure a stable air pressure;

[0046] (3) After standing still, the oxidation device is uncapped, then in the solution, add respectively twice the carbon molecular sieve adsorbent that is 5% of the raw material concentrated hydrochloric acid solution quality, and fill high-purity nitrogen to carry out pressurized adsorption, each time After adding th...

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Abstract

The invention discloses a method for removing an impurity arsenic in an electronic-grade hydrochloric acid. The method comprises the following steps: (1) putting the raw material of an concentrated hydrochloric acid into an oxidation device, then adding an oxidizing agent, stirring at a constant speed; (2) sealing the stirred solution, and then standing; (3) adding an adsorbent into the solution;(4) taking out the adsorbent, filtering the solution, enabling the filtered solution to enter an evaporation device; (5) distilling the solution at the high temperature through the evaporation device,and obtaining a hydrogen chloride gas; (6) arranging an absorbing groove in a distillation pipeline of the evaporation device to adsorb and filter the hydrogen chloride gas; (7) condensing the hydrogen chloride gas treated in the step (6), and obtaining the electronic-grade hydrochloric acid. The impurity arsenic in the hydrochloric acid is efficiently removed, no other impurity ions are broughtin the removal process, and the high-purity hydrochloric acid whose arsenic content reaches the standard is produced under the premise that the continuous stable production is guaranteed.

Description

technical field [0001] The invention relates to the technical field of preparation of ultrapure chemicals, in particular to a method for removing impurity arsenic in electronic grade hydrochloric acid. Background technique [0002] Ultra-clean and high-purity electronic chemicals are key integrated materials for VLSI manufacturing, and their purity and cleanliness have a very important impact on yield, electrical performance, and reliability. At present, the cutting-edge semiconductor technology has reached the level of 7-22 nanometers. Correspondingly, the requirements for the purity of electronic chemicals are also getting higher and higher. [0003] High-purity hydrochloric acid is one of the electronic chemicals used in the semiconductor manufacturing industry. It is mainly used in the standard RCA cleaning process of silicon wafers to remove and clean metal and organic impurities on the surface of silicon wafers. The purity of hydrochloric acid determines the amount of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/07
CPCC01B7/0712C01B7/0718
Inventor 赵俊男高小云傅华
Owner SUZHOU CRYSTAL CLEAR CHEMICAL CO LTD
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