Method for recovering tetrabutylammonium hydroxide by electrolysis of tetrabutylammonium sulfate solution

A technology of tetrabutylammonium hydroxide and tetrabutylammonium sulfate, applied in chemical instruments and methods, sulfur compounds, sulfur trioxide/sulfuric acid, etc., can solve the problems of increased recycling costs, waste of resources, pollution, etc., to reduce content, Effect of improving purity and improving recovery rate

Inactive Publication Date: 2018-08-31
XINXIANG CHEM FIBER
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Problems solved by technology

The patent with publication number CN104278288A discloses a method for preparing high-purity tetrabutylammonium hydroxide by continuous electrolysis. This method directly uses the three-compartment bipolar membrane electrodialysis process to cause the migration of tetrabutylammonium ions, which is easy to cause the polar liquid chamber , Acid solution chamber pollution reduces the recovery rate of tetrabutylammonium hydroxide, which to a certain extent causes the improvement of recovery cost and the waste of resources

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  • Method for recovering tetrabutylammonium hydroxide by electrolysis of tetrabutylammonium sulfate solution

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Experimental program
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Effect test

Embodiment 1

[0018] Will contain 30g / L of (TBA) 2 SO 4 The solution is subjected to four-compartment bipolar membrane electrodialysis with an intermediate liquid chamber. The equipment uses Japanese bipolar membranes, Japanese cation exchange membranes and German anion exchange membranes. The intermediate liquid chamber is 0.05mol / L sulfuric acid solution. The current of the electrolysis process The density is 200A / m 2 , the flow rate of the feed liquid chamber is 0.2L / h, and the electrodialysis is 1.5h. At the end, the conductivity of the solution in the feed liquid chamber is 835μs, and the conductivity of the solution in the lye chamber is 7.3ms, generating 0.15mol of tetrabutylammonium hydroxide, tetrabutylammonium hydroxide The recovery rate>99%, the purity reaches 98.9%, is concentrated to the mass fraction and is that the sulfate ion content is lower than 1500ppm in the tetrabutyl ammonium hydroxide solution of 40%.

Embodiment 2

[0020] Will contain 70g / L of (TBA) 2 SO 4 The solution is subjected to four-compartment bipolar membrane electrodialysis with an intermediate liquid chamber. The equipment uses Japanese bipolar membranes, Japanese cation exchange membranes and German anion exchange membranes. The intermediate liquid chamber is 0.1mol / L sulfuric acid solution. The current of the electrolysis process The density is 200A / m 2 , the feed liquid chamber flow rate is 0.2L / h, electrodialysis 3h, the conductivity of the solution in the feed liquid chamber is 1068μs at the end, and the conductivity of the solution in the lye chamber is 11.2ms, generating 0.38mol of tetrabutylammonium hydroxide, tetrabutylammonium hydroxide The recovery rate>99%, the purity reaches 98.2%, and the content of sulfate ion in the tetrabutylammonium hydroxide solution concentrated to 40% by mass fraction is lower than 2800ppm.

Embodiment 3

[0022] Will contain 200g / L of (TBA) 2 SO 4 The solution is subjected to four-compartment bipolar membrane electrodialysis with an intermediate liquid chamber. The equipment uses Japanese bipolar membranes, Japanese cation exchange membranes and German anion exchange membranes. The intermediate liquid chamber is 0.1mol / L sulfuric acid solution. The current of the electrolysis process The density is 200A / m 2 , the flow rate of the feed liquid chamber is 0.2L / h, electrodialysis is 8.5h, 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 32.5ms, generating 0.93mol of tetrabutylammonium hydroxide, tetrabutylammonium hydroxide The recovery rate of ammonium is more than 99%, and the purity reaches 98.6%. The sulfate ion content in the tetrabutylammonium hydroxide solution concentrated to a mass fraction of 40% is lower than 4500ppm.

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Abstract

The invention discloses a method for recovering tetrabutylammonium hydroxide by electrolysis of a tetrabutylammonium sulfate solution, and belongs to the technical field of recovery of tetrabutylammonium hydroxide by bipolar membrane electrodialysis. According to the key points of the technical scheme, the tetrabutylammonium sulfate solution is subjected to bipolar membrane electrodialysis in a four-compartment electrodialysis device with an intermediate liquid chamber, and the four-compartment electrodialysis device with the intermediate liquid chamber comprises polar liquid chambers at bothsides and an electrodialysis compartment sandwiched between the polar liquid chambers at two sides, and the electrodialysis compartment is of a four-compartment structure and is composed of the intermediate liquid chamber, an acid liquid chamber, a material liquid chamber and an alkaline liquid chamber which are formed by alternately and separately arraying a bipolar membrane, a cationic exchangemembrane, an anionic exchange membrane, a cationic exchange membrane and a bipolar membrane; a tetrabutylammonium hydroxide solution is obtained in the alkaline liquid chamber, and a sulfuric acid solution is obtained in the acid liquid chamber. The method can remarkably improve the purity and the recovery rate of the recovered product tetrabutylammonium hydroxide.

Description

technical field [0001] The invention belongs to the technical field of recovering tetrabutylammonium hydroxide by bipolar membrane electrodialysis, and in particular relates to a method for recovering tetrabutylammonium hydroxide by electrolyzing tetrabutylammonium sulfate solution. 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, and its purity 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 as the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/00C07C209/84C07C211/63C01B17/90B01D61/44B01D61/48
CPCB01D61/445B01D61/48C01B17/90C01B17/904C07C209/00C07C209/84C07C211/63
Inventor 乔浩才刘东奇曹俊友苏海霞杨军杰
Owner XINXIANG CHEM FIBER
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