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Preparation process of electronic-grade potassium hydroxide

A potassium hydroxide and preparation technology, applied in the direction of alkali metal oxides/hydroxides, inorganic chemistry, alkali metal compounds, etc., can solve the problems of unfavorable purification, low energy efficiency, slow production efficiency, etc., to improve the adsorption range, Improved adsorption capacity and high selectivity

Pending Publication Date: 2021-09-28
JIANGYIN RUNMA ELECTRONICS MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, in the production of electronic grade potassium hydroxide, potassium hydroxide is generally prepared into potassium hydroxide solution first, and then heavy metals and sodium ions are removed by ion exchange or cooling and crystallization, but this method has slow production efficiency, low energy efficiency and high purification effect. Not ideal, the resulting potassium hydroxide concentration of heavy metal ions is still high
[0004] Chinese patent CN106904637A discloses a high-activity potassium hydroxide purification process, which is dissolved in ionized water, acetone crystallization is added dropwise at 5°C, centrifuged under nitrogen protection, the filter cake is filtered out and then dried under reduced pressure under nitrogen protection to obtain high-purity Potassium hydroxide suitable for ITO development needs, this method is only aimed at the purity and fineness of potassium hydroxide, and does not involve the removal of metal cations
The crystallization efficiency of the potassium chloride crystal prepared in this method is low, and the purity requirement of the introduced hydrogen chloride gas or hydrogen chloride aqueous solution is higher, otherwise more impurity ions will be introduced, which is not conducive to purification, and then affects the purity of subsequent potassium hydroxide

Method used

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  • Preparation process of electronic-grade potassium hydroxide

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Experimental program
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Effect test

Embodiment 1

[0029] A preparation process for electronic grade potassium hydroxide, comprising the following steps carried out successively and continuously:

[0030] (1) Dissolve food-grade potassium chloride to form a 300g / L aqueous solution (60°C), and then pass through the adsorption tower filled with aminocarboxylic acid chelating resin, and then the adsorption tower filled with iminodiacetic acid chelating resin (D751) Absorption tower adsorption, adsorption tower flow rate 15m 3 / h, the replacement time is 0.5h, and then purified by P507 extraction resin, the purification time is 0.5h, to obtain a high-purity potassium chloride solution.

[0031] (2) Concentrate and crystallize high-purity potassium chloride solution at 110°C to obtain potassium chloride crystals.

[0032] (3) Dissolve potassium chloride crystals in high-purity water to prepare a 300g / L potassium chloride solution, which is electrolyzed by a bipolar membrane electrodialysis system composed of a bipolar membrane and...

Embodiment 2

[0036] A preparation process for electronic grade potassium hydroxide, comprising the following steps carried out successively and continuously:

[0037] (1) Dissolve food-grade potassium chloride to form a 350g / L aqueous solution (70°C), and then pass through the adsorption tower filled with aminocarboxylic acid chelating resin, and then filled with fluorinated modified iminodiacetic acid chelating The adsorption tower of the resin is adsorbed, and the flow rate of the adsorption tower is 15m 3 / h, the replacement time is 0.5h, and then purified by P507 extraction resin, the purification time is 0.5h, to obtain a high-purity potassium chloride solution.

[0038] (2) Concentrate and crystallize high-purity potassium chloride solution at 110°C to obtain potassium chloride crystals.

[0039] (3) Dissolve potassium chloride crystals in high-purity water to prepare a 300g / L potassium chloride solution, which is electrolyzed by a bipolar membrane electrodialysis system to obtain a...

Embodiment 3

[0043] A preparation process for electronic grade potassium hydroxide, comprising the following steps carried out successively and continuously:

[0044] (1) Dissolve food-grade potassium chloride to form a 350g / L aqueous solution (65°C), and then pass through the adsorption tower filled with aminocarboxylic acid chelating resin, and then filled with fluorinated modified iminodiacetic acid chelating The adsorption tower of the resin is adsorbed, and the flow rate of the adsorption tower is 15m 3 / h, the replacement time is 0.5h, and then purified by P507 extraction resin, the purification time is 0.5h, to obtain a high-purity potassium chloride solution.

[0045] (2) The absorbed potassium chloride solution was concentrated and crystallized at 110°C to obtain potassium chloride crystals.

[0046] (3) Dissolve potassium chloride crystals in high-purity water to prepare a 400g / L potassium chloride solution, which is electrolyzed by a bipolar membrane electrodialysis system to ob...

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Abstract

The invention relates to a preparation process of electronic-grade potassium hydroxide, which comprises the following successive and continuous steps: sequentially passing a potassium chloride aqueous solution through a first chelating resin and a second chelating resin at a constant flow rate for adsorption to obtain a potassium chloride high-purity solution, then conducting concentrating to obtain potassium chloride crystals, adding pure water into the potassium chloride crystals for dissolving, after dissolving, conducting treating by a bipolar membrane electrodialysis system to obtain a low-concentration potassium hydroxide solution, and finally conducting heating and concentrating to obtain the electronic-grade potassium hydroxide. According to the preparation process of the electronic-grade potassium hydroxide, metal cations Fe<2+>, Ca<2+>, Mg<2+>, Ni<2+> and Zn<2+> are less than or equal to 100ppb, Na<+> is less than or equal to 50ppm, the preparation process is simple and easy to operate, and the high-concentration and high-purity electronic-grade potassium hydroxide can be continuously produced on a large scale.

Description

technical field [0001] The invention belongs to the technical field of chemical preparations, and in particular relates to a preparation process of electronic grade potassium hydroxide. Background technique [0002] Potassium hydroxide is the main raw material for stripping liquid and developer in photovoltaic, panel, semiconductor and other electronic industries. The purity of potassium hydroxide has a great influence on the quality of later-stage products. Industrial grade potassium hydroxide can no longer meet the requirements. Therefore, it is necessary to purify industrial grade potassium hydroxide to improve its quality. [0003] At present, in the production of electronic grade potassium hydroxide, potassium hydroxide is generally prepared into potassium hydroxide solution first, and then heavy metals and sodium ions are removed by ion exchange or cooling and crystallization, but this method has slow production efficiency, low energy efficiency and high purification e...

Claims

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Application Information

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IPC IPC(8): C01D3/16C01D1/42
CPCC01D3/16C01D1/42C01P2006/80
Inventor 戈烨铭何珂汤晓春
Owner JIANGYIN RUNMA ELECTRONICS MATERIAL
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