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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: 2011-11-23
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 formulation, a paste mixture (polymerizable composition) for forming an anion exchange membrane was prepared.

[0131] The recipe of the paste mixture:

[0132] Chloromethylstyrene 50 parts by weight

[0133] Styrene 50 parts by weight

[0134] Divinylbenzene 21.4 parts by weight

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

[0138] High density polyethylene net:

[0139] Commodity name: NBC Industrial System Nipp Qiangli Net

[0140] Thickness: 150μm

[0141] Number of meshes: 200 per 1 square meter

[0142] The pre-prepared paste mixture is coated on the skeleton substrate, and then a polyester film (release film) is coated, and then the paste mixture is polymerized to obtain the original film of the anion exchang...

Embodiment 2

[0153] Use the anion exchange membrane A and cation exchange membrane C used in Example 1, except for installing figure 2 The effective membrane area of ​​the setup shown is 2dm 2 Except for the electrolysis device of, electrolysis was performed in the same manner as in Example 1. (The anion exchange membrane A is set so that the surface crosslinking layer is located on the anode side.)

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

Embodiment 3

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

[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 1.2 meq / g dry membrane, the rupture strength of the Mullen type is 1.0 MPa or more, and the water permeability is 0 ml / (m 2 ·Hour·0.1MPa).

[0159] Except for the use of the above-mentioned anion exchange membrane A, the electrolysis operation was continuously carried out in exactly the same manner as in Example 2. As a result, the ion exchange capacity of the anion exchange membrane A after 1 year of continuous operation was 1.0 meq / g dry membrane. The breaking strength of the formula is 0.9MPa, and the water permeability is 0ml / (m 2 ·Hour·0.1MPa). ...

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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 method for preparing a quaternary ammonium base by electrolysis using an ion exchange membrane. Background technique [0002] Quaternary ammonium bases represented by tetramethylammonium hydroxide are used as phase transfer catalysts, standard solutions of bases in non-aqueous titration, organic alkaline agents, etc., used in the implementation and analysis of various chemical reactions. compound of. In addition, recently, when manufacturing integrated circuits (ICs) or large-scale integrated circuits (LSIs), it has been widely used as a processing agent for manufacturing semiconductor substrates, developing resists, and the like. [0003] As such a quaternary ammonium base, a high-purity substance with few impurities is required. Especially when it is used in a semiconductor manufacturing process, the demand for a high-purity quaternary ammonium base is very high. This is because in recent years, semiconductor devices hav...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/00B01D61/44C25B13/08
CPCC25B1/26C25B9/00B01D61/44C25B9/19C25B15/02C25B15/08
Inventor 川田聪志岸野刚之森本裕之岩本久彦
Owner TOKUYAMA CORP
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