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Method for production of quaternary ammonium hydroxide

A technology of quaternary ammonium base and halogenated quaternary ammonium salt, which is applied in chemical instruments and methods, electrolytic organic production, electrolytic components, etc., and can solve problems such as difficulty in completely isolating halogen gas and oxidation degradation of anion exchange membranes

Inactive Publication Date: 2010-03-24
TOKUYAMA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, although the life of the anion exchange membrane can be extended, the following problems still remain: it is difficult to completely isolate the halogen gas, and even a small amount of halogen gas generated at the electrode passes through the cation exchange membrane and contacts with the anion exchange membrane, causing anion Exchange membrane slowly oxidizes and deteriorates, etc.

Method used

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  • Method for production of quaternary ammonium hydroxide
  • Method for production of quaternary ammonium hydroxide
  • Method for production of quaternary ammonium hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0130] According to the following recipe, a paste mixture (polymerizable composition) for anion exchange membrane formation was prepared.

[0131] Recipe for the paste mixture:

[0132] 50 parts by weight of chloromethyl styrene

[0133] 50 parts by weight of styrene

[0134] 21.4 parts by weight of divinylbenzene

[0135] Di-tert-butyl peroxide (radical polymerization initiator) 7.14 parts by weight

[0136] Styrene-butadiene copolymer (base resin) 14.3 parts by weight

[0137] Next, a calendered high-density polyethylene net of the following specifications was prepared as a skeleton base material.

[0138] High-density polyethylene mesh:

[0139] Product name: NBC Industries ニツプ strong net

[0140] Thickness: 150μm

[0141] Mesh number: 200 per 1 square meter

[0142] The previously prepared paste mixture was coated on the above-mentioned skeleton substrate, followed by covering with a polyester film (peeling film), and then the paste mixture was polymerized to obt...

Embodiment 2

[0153]The anion exchange membrane A and cation exchange membrane C used in Example 1 were used except that figure 2 The setup shown has an effective membrane area of ​​2dm 2 The electrolysis was performed in the same manner as in Example 1 except in the electrolysis device. (The anion exchange membrane A is set so that the surface cross-linked layer is on the anode side.)

[0154] That is, in figure 2 0.5 equivalent of sulfuric acid circulates in the anode chamber 11 of the shown electrolysis device, circulates 0.5 equivalent of hydrochloric acid in the chamber 7 between the cation exchange membrane C and the anion exchange membrane A on the anode side, and circulates between the anion exchange membrane A and the cathode side Circulate 2.5 equivalents of tetramethylammonium chloride aqueous solution in the chamber (stock solution chamber 5) between the cation exchange membranes C, and circulate pure water in the cathode chamber 9, the current density is 30A / dm 2 , the tem...

Embodiment 3

[0157] An anion exchange membrane A was prepared in the same manner as in Example 1, except that the surface crosslinked layer was formed on one side of the original membrane by immersion in a 1.0-N dimethylamine aqueous solution for 3 hours.

[0158] The exchange capacity of the surface crosslinked layer at this time was 0.008 meq / g dry film. In addition, the ion-exchange capacity of the anion-exchange membrane A before electrolysis is 1.2meq / g dry membrane, the rupture strength of Mullen's formula is more than 1.0MPa, and the water permeability is 0ml / (m 2 ·hour·0.1MPa).

[0159] Except for using the above-mentioned anion exchange membrane A, the electrolytic operation was carried out continuously in exactly the same manner as in Example 2. As a result, after one year of continuous operation of the anion exchange membrane A, the ion exchange capacity was 1.0 meq / g dry membrane, Mullen The bursting strength of the formula is 0.9MPa, and the water permeability is 0ml / (m 2 ·h...

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Abstract

To provide a method in which the deterioration of an anion exchange membrane within a short period can be prevented effectively, and which can produce highly pure quaternary ammonium hydroxide steadily for a long period without the need of replacing the membrane with new one. ¢MEANS FOR SOLVING PROBLEMS! Disclosed is a method for producing quaternary ammonium hydroxide by arranging an anion exchange membrane and a cation exchange membrane between electrodes and supplying an aqueous solution of a halogenated quaternary ammonium salt to a stock solution chamber facing the side of a cathode of the anion exchange membrane to carry out the electrolysis. In the method, a membrane comprising a base layer (31) and a surface layer (33) formed on one surface of the base layer (31) and having a highcrosslinking density is used as the anion exchange membrane, and the anion exchange membrane is so arranged that the surface layer is positioned on the side of an anode (1) to carry out the electrolysis.

Description

technical field [0001] The present invention relates to a process for the preparation of quaternary ammonium bases by electrolysis using ion exchange membranes. Background technique [0002] Quaternary ammonium bases represented by tetramethylammonium hydroxide are used in the execution and analysis of various chemical reactions as phase transfer catalysts, standard solutions of bases in non-aqueous titration, and organic alkaline agents. compound of. In addition, recently, in the manufacture of integrated circuits (ICs) and large scale integrations (LSIs), they are widely used as processing agents for the manufacture of semiconductor substrates, development of resists, and the like. [0003] As such a quaternary ammonium base, a high-purity substance with few impurities is required, and the demand for a high-purity quaternary ammonium base is high especially when it is used in a semiconductor manufacturing process. This is because semiconductor devices have become signifi...

Claims

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Application Information

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IPC IPC(8): C25B3/00B01D61/44C25B13/08
CPCB01D61/44C25B1/26C25B9/00C25B9/19C25B15/02C25B15/08
Inventor 川田聪志岸野刚之森本裕之岩本久彦
Owner TOKUYAMA CORP
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