Method for preparing tetrabutylammonium hydroxide by taking tetrabutylammonium sulfate as raw material

A technology of tetrabutylammonium hydroxide and tetrabutylammonium sulfate, applied in electrolysis process, electrolysis components, electrolysis organic production and other directions, can solve the problems of low purity of tetrabutylammonium hydroxide, difficult to meet the requirements of microelectronics industry, etc. Process safety and low energy consumption

Inactive Publication Date: 2018-09-04
XINXIANG CHEM FIBER
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  • Abstract
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Problems solved by technology

The patent with the publication number CN102030665A discloses a method for preparing tetrabutylammonium hydroxide by chemical method. The purity of tetrabutylammonium hydroxide prepared by this method is not high, and there are a large number of anions (mainly bromide ions), which is difficult to reach microelectronics. industry requirements

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  • Method for preparing tetrabutylammonium hydroxide by taking tetrabutylammonium sulfate as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Will contain 30g / L of (TBA) 2 SO 4 The solution is subjected to three-compartment bipolar membrane electrodialysis. The equipment adopts Japanese bipolar membrane, Japanese cation exchange membrane and German anion exchange membrane. The polar liquid is 0.3mol / L sulfuric acid solution, and the current density of the electrolysis process is 200A / m 2 , the flow rate of the feed liquid chamber is 0.25L / h, electrodialysis is 3.5h, the conductivity of the solution in the feed liquid chamber is 1.3ms at the end, and the conductivity of the solution in the lye chamber is 3.7ms, generating 0.098mol of tetrabutylammonium hydroxide, tetrabutylammonium hydroxide The recovery rate of ammonium was 76.5%.

Embodiment 2

[0018] Will contain 70g / L of (TBA) 2 SO 4 The solution is subjected to three-compartment bipolar membrane electrodialysis. The equipment adopts German bipolar membrane, Japanese cation exchange membrane and Japanese anion exchange membrane. The polar liquid is 0.3mol / L sulfuric acid solution. The current density of the electrolysis process is 400A / m 2 , the flow rate of the feed liquid chamber is 0.3L / h, electrodialysis is 2.8h, the conductivity of the solution in the feed liquid chamber is 3.6ms at the end, and the conductivity of the solution in the lye chamber is 8.2ms, generating 0.26mol of tetrabutylammonium hydroxide, tetrabutylammonium hydroxide The recovery rate of ammonium was 84.2%.

Embodiment 3

[0020] Will contain 200g / L of (TBA) 2 SO 4 The solution is subjected to three-compartment bipolar membrane electrodialysis. The equipment adopts Japanese bipolar membrane, Japanese cation exchange membrane and Japanese anion exchange membrane. The polar liquid is 0.3mol / L sulfuric acid solution, and the current density of the electrolysis process is 600A / m 2 , the feed liquid chamber flow rate is 0.35L / h, electroosmosis. The recovery rate of ammonium was 82.9%.

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Abstract

The invention discloses a method for preparing tetrabutylammonium hydroxide by taking tetrabutylammonium sulfate as a raw material, and belongs to the technical field of preparation of tetrabutylammonium hydroxide by bipolar membrane electroosmosis. According to the technical scheme, the method for preparing the tetrabutylammonium hydroxide by taking the tetrabutylammonium sulfate as the raw material comprises the following step: carrying out bipolar membrane electroosmosis on a tetrabutylammonium sulfate solution in a three-compartment electroosmosis device. The three-compartment electroosmosis device comprises polar liquor chambers and an electroosmosis compartment, the polar liquor chambers are arranged on two sides of the three-compartment electroosmosis device, the electroosmosis compartment is sandwiched between the polar liquor chambers on the two sides, has a three-compartment structure, and is formed by unit groups of an acid liquor chamber, a material liquor chamber and an alkali liquor chamber in an arranged manner, the unit groups of the acid liquor chamber, the material liquor chamber and the alkali liquor chamber are formed by a bipolar membrane, an anion exchange membrane, a cation exchange membrane and another bipolar membrane which are arranged alternately at intervals, a tetrabutyl ammonium hydroxide solution is obtained from the alkali liquor chamber, and asulfuric acid solution is obtained from the acid liquor chamber. The three-compartment bipolar membrane electroosmosis process has the characteristics that the production process is safe, harmful gasis not generated, and energy consumption is low.

Description

technical field [0001] The invention belongs to the technical field of preparing tetrabutylammonium hydroxide by bipolar membrane electrodialysis, and in particular relates to a method for preparing tetrabutylammonium hydroxide by using tetrabutylammonium sulfate as a raw material. Background technique [0002] Tetrabutylammonium hydroxide (TBAOH) is an organic quaternary ammonium strong base. Tetrabutylammonium hydroxide is often used as organic synthesis reagents, surfactants, phase transfer catalysts, cleaning reagents in the electronics industry, polarographic analysis reagents, etc. Among them, high-purity tetrabutylammonium hydroxide is mainly used for chip cleaning and corrosion. Its purity Cleanliness and cleanliness have a very important impact on the yield, electrical performance and reliability of integrated circuits. Due to its unique effect, high-purity tetrabutylammonium hydroxide will replace tetramethylammonium hydroxide and tetraethylammonium hydroxide, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00C25B1/22
CPCC25B3/00C25B1/22
Inventor 乔浩才刘东奇曹俊友苏海霞杨军杰
Owner XINXIANG CHEM FIBER
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