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Electronic-grade pyrazole aqueous solution and preparation method thereof

An aqueous solution and electronic-grade technology, which is applied in the field of electronic-grade pyrazole aqueous solution and its preparation, can solve the problems of high metal ion content that cannot meet the needs of silicon wafer cleaning and less research on purification and preparation processes, and achieve increased conductivity and simple process operation , low-cost effect

Pending Publication Date: 2021-04-13
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of metal ions in the currently commercially available pyrazole is too high to meet the requirements of the silicon wafer cleaning industry, and there are few studies on purification and preparation processes at home and abroad.

Method used

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  • Electronic-grade pyrazole aqueous solution and preparation method thereof
  • Electronic-grade pyrazole aqueous solution and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In the ultrapure electrolyzer (1) used, the cathode plate (9) is a titanium electrode (99.99% in purity), and the anode plate (7) is a platinum electrode (99.99% in purity); the cathode plate (9) and the anode plate (7) are The distance between them is 0.8 cm. The cationic exchange resin (11) used in the anode chamber (6) and the cathode chamber (8) is 001*7 type cationic exchange resin, and its particle size range is (0.315 ~ 1.25mm) ≥ 95%, wet bulk density 800 kg / m 3 , the packing density in the cathode chamber (8) is 80% of its wet bulk density, and the packing density in the anode chamber (6) is 85% of its wet bulk density. The raw material of the pyrazole aqueous solution used is an industrial grade pyrazole product, which is dissolved in water to obtain a pyrazole aqueous solution with a mass concentration of 10%.

[0039] First, add a specified amount of 001*7 cationic exchange resin (11) into the anode chamber (6) and cathode chamber (8), respectively, add Ul...

Embodiment 2

[0044] In the ultrapure electrolyzer (1) used, the cathode plate (9) is a platinum electrode (99.99% in purity), and the anode plate (7) is a titanium electrode (99.99% in purity); the cathode plate (9) and the anode plate (7) are The distance between them is 1.0 cm. The cationic exchange resin (11) used in the anode chamber (6) and the cathode chamber (8) is 2800H type cationic exchange resin, its particle size range is (0.315 ~ 1.25mm) ≥ 95%, and the wet bulk density is 810 kg / m 3 , the packing density in the cathode chamber (8) is 81% of its wet bulk density, and the packing density in the anode chamber (6) is 87% of its wet bulk density. The raw material of the pyrazole aqueous solution used is an industrial grade pyrazole product, which is dissolved in water to obtain a pyrazole aqueous solution with a mass concentration of 10%.

[0045] Firstly add specified amount of 2800H cationic exchange resin (11) into the anode chamber (6) and cathode chamber (8) Ultrapure hydro...

Embodiment 3

[0050] The cathode plate (9) in the ultrapure electrolyzer (1) used is a titanium-iridium alloy electrode (purity 99.99%), and the anode plate (7) is a platinum electrode (purity 99.99%); the cathode plate (9) and the anode plate (7 ) with a distance of 1.5 cm. The cationic exchange resin (11) used in the anode chamber (6) and the cathode chamber (8) is 2800H type cationic exchange resin, its particle size range is (0.45 ~ 1.25mm) ≥ 95%, and the wet bulk density is 780 kg / m 3 , the packing density in the cathode chamber (8) is 84% ​​of its wet bulk density, and the packing density in the anode chamber (6) is 89% of its wet bulk density. The raw material of the pyrazole aqueous solution used is an industrial grade pyrazole product, which is dissolved in water to obtain a pyrazole aqueous solution with a mass concentration of 20%.

[0051] Firstly add specified amount of 2800H cationic exchange resin (11) into the anode chamber (6) and cathode chamber (8) Ultrapure hydrochlor...

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Abstract

The invention relates to an electronic-grade pyrazole aqueous solution and a preparation method thereof. The content of metal ions such as Na<+>, Mg<2+>, K<+>, Ca<2+>, Cu<2+>, Zn<2+>, Ni<2+>, Cr<3+>, Al<3+> and Fe<3+> in the pyrazole aqueous solution is lower than 50 ppb, and the pyrazole content is larger than or equal to 10%. According to the method, the pyrazole aqueous solution is purified through a combined process of ionic membrane electrolysis and ion exchange resin, wherein the ion exchange resin is added into an ionic membrane electrolytic cell to enhance the conductivity of the solution and assist in removing metal ions. One part of metal ions in a pyrazole stock solution in an anode chamber are migrated to a cathode chamber from the anode chamber under the action of electric field force, the other part of ions are adsorbed by ion resin in the electrolytic cell, and finally the electronic-grade pyrazole aqueous solution is obtained in the anode chamber. The electronic-grade pyrazole aqueous solution can be used as a solvent of a chemical cleaning solution for microelectronic industries such as super-large-scale integrated circuits or screen displays.

Description

technical field [0001] The invention relates to the field of preparation of electronic grade reagents, in particular to an electronic grade pyrazole aqueous solution and a preparation method thereof. Background technique [0002] Pyrazole is a colorless or white acicular or prismatic crystalline organic cyclic compound. It is often used as a halogen-containing solvent, a stabilizer for lubricating oil, a chelating agent or an intermediate in organic synthesis. It occupies an important role in the research and development of medicine and pesticides. very important position. [0003] Electronic-grade pyrazole aqueous solution is an ultra-clean and high-purity reagent. Because it has a strong chelating effect on metal ions, it can be used as a cleaning agent in the microelectronics industry such as silicon wafer cleaning and substrate cleaning in the field of integrated circuits and electronic component processing. Chip wet cleaning, etc. The key to ultra-clean and high-purit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J47/12C25B3/05C25B3/09C25B9/19
CPCB01J47/12C25B3/00
Inventor 胡硕真张新胜金家昱王坦郭江楠程芸芸高思捷
Owner EAST CHINA UNIV OF SCI & TECH
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