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Preparation method for electronic grade tetramethylammonium hydroxide on industrial scale

A technology of tetramethyl ammonium hydroxide and tetramethyl ammonium bicarbonate, applied in electrolysis process, electrolysis components, electrolysis organic production and other directions, can solve the problems of simplicity and no description of the electrolysis process, and achieves high current efficiency and operation. Conditionally stable effects

Inactive Publication Date: 2017-10-24
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disclosed content of the patent process is too simple, there is no description of the electrolysis process, how the catholyte and anolyte flow during the electrolysis process, and how the gas generated by electrolysis is discharged.

Method used

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  • Preparation method for electronic grade tetramethylammonium hydroxide on industrial scale
  • Preparation method for electronic grade tetramethylammonium hydroxide on industrial scale
  • Preparation method for electronic grade tetramethylammonium hydroxide on industrial scale

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Put the tetramethylammonium bicarbonate raw material with a concentration of 65.0% into the anode liquid circulation tank at a flow rate of 287.0kg / h, the concentration of the anode circulation liquid entering the electrolytic cell is 35.0%, and the flow rate of the anode circulation pump is 10.0m 3 / h, the temperature of the ion-exchange membrane electrolyzer is controlled at 50°C, the concentration of the cathodic circulating fluid is 25.8%, and the flow rate of the cathodic circulating pump is 15.0m 3 / h, the flow rate of high-purity water into the cathode circulation tank is 262kg / h, and the current density of the electrolyzer is 1.5kA / m 2 , the outlet concentration of the product TMAH is 25.8%, the flow rate is 487.8kg / h, the product is detected by ICP-MS, the content of each metal ion is less than 1ppb, and the CO in the product 3 2- and NO 3 - The content is less than 50ppb, and the product meets the quality requirements of electronic grade products.

Embodiment 2

[0043] Put the tetramethylammonium bicarbonate raw material with a concentration of 55.0% into the anode liquid circulation tank at a flow rate of 339.5kg / h, the concentration of the anode circulation liquid entering the electrolytic cell is 25.0%, and the flow rate of the anode circulation pump is 7.0m 3 / h, the temperature of the ion-exchange membrane electrolyzer is controlled at 70°C, the concentration of the cathodic circulating fluid is 26.5%, and the flow rate of the cathodic circulating pump is 9.0m 3 / h, the flow rate of high-purity water into the cathode circulation tank is 262kg / h, and the current density of the electrolyzer is 1.0kA / m 2, the outlet concentration of the product TMAH is 26.5%, the flow rate is 475.0kg / h, the product is detected by ICP-MS, the content of each metal ion is less than 1ppb, and the CO in the product 3 2- and NO 3 - The contents are 150 and 350ppb respectively, and the products do not meet the quality requirements of electronic grade p...

Embodiment 3

[0045] Put the tetramethylammonium bicarbonate raw material with a concentration of 59.3% into the anode liquid circulation tank at a flow rate of 315kg / h, the concentration of the anode circulation liquid entering the electrolytic cell is 28%, and the flow rate of the anode circulation pump is 7.0m 3 / h, the temperature of the ion-exchange membrane electrolyzer is controlled at 55°C, the concentration of the cathodic circulating fluid is 25.0%, and the flow rate of the cathodic circulating pump is 8.0m 3 / h, the flow rate of high-purity water into the cathode circulation tank is 262kg / h, and the current density of the electrolyzer is 0.8kA / m 2 , the outlet concentration of the product TMAH is 25.2%, the flow rate is 500kg / h, the product is detected by ICP-MS, and the content of each metal ion is less than 1ppb, and the CO in the product 3 2- and NO 3 - The content is less than 50ppb, and the product meets the quality requirements of electronic grade products.

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Abstract

The invention discloses a method for preparing electronic-grade tetramethylammonium hydroxide on an industrial scale. In the method, tetramethylammonium bicarbonate is used as a raw material, and two chambers plus an ion membrane are used for electrolytic preparation. The electrolytic cell is a combined electrolytic cell composed of multiple unit cells composed of two chambers and ion membranes in parallel. The electrolytic solution in the electrolytic cell is forced to circulate with a magnetic pump. , tank liquid collection pipe, gas-liquid separator, circulation tank, pump and cooler. In order to prevent the accumulation of impurity ions in the system, a bypass is set in the anode circulation pipeline, so that part of the anolyte passes through the anion and cation exchange resin beds in the bypass to remove impurity ions. The gas generated by the cathode and anode passes through the liquid-sealed tank and then is emptied or recycled for utilization. The invention has a short technological process, can carry out industrialized continuous production, has stable operating conditions in the production process, high current efficiency, and all incoming raw materials become products without discharging electrolytic residual liquid.

Description

technical field [0001] The technology relates to a method for continuously producing electronic-grade tetramethylammonium hydroxide, which belongs to the field of electrochemical organic synthesis. Background technique [0002] Tetramethylammonium hydroxide, also known as tetramethylammonium hydroxide (TMAH), has a molecular formula of (CH3)4NOH. It is the strongest organic base. TMAH is mainly used in the integrated circuit (IC) industry and liquid crystal display industry (FT -LCD), developer and etchant for optoelectronic industry, ultra-pure cleaning agent for integrated circuit chemical mechanical polishing (CMP) process. In the electronics industry, TMAH product quality indicators mainly include metal ion content and anion impurity content, requiring each metal ion content to be less than 1ppb (μg / kg), and each anion content to be less than CO 3 2- , NO 3 - , Cl - The content is lower than 50ppb. At present, the industrial preparation of electronic grade TMAH is ...

Claims

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Application Information

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IPC IPC(8): C25B3/00C25B15/08C25B9/00
CPCC25B3/00C25B9/00C25B15/08
Inventor 杨长生孙斐忠严超
Owner TIANJIN UNIV
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