Method for preparing high-purity tetrabutyl ammonium hydroxide by continuous electrolysis

A technology of tetrabutylammonium hydroxide and tetrabutylammonium bromide is applied in the electrolysis process, electrolysis components, electrolysis organic production and other directions, which can solve the problems that the purification process cannot be continuously produced in small batches and the concentration of bromide ions is high, so as to improve the current Efficiency and product conversion, energy reduction, membrane cost savings

Inactive Publication Date: 2015-01-14
赵文洲
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for continuous electrolytic preparation of high-purity tetrabutylammonium hydroxide, effectively overcome the shortcoming of high bromide ion concentration in the product obtained by the existing tetrabutylammoni

Method used

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  • Method for preparing high-purity tetrabutyl ammonium hydroxide by continuous electrolysis

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Experimental program
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Effect test

Embodiment 1

[0036] Add 35% tetrabutylammonium bromide aqueous solution into the salt chamber 3, control the flow rate to 2000h / L, connect the direct current 12, control the temperature of each chamber to 60°C, and control the current density to be constant at 600 A / m 2 , Obtaining the tetrabutylammonium hydroxide aqueous solution that finished product content is 5%. Its bromide ion concentration is 33ppm; the current efficiency is 43%.

Embodiment 2

[0038] Add 35% tetrabutylammonium bromide aqueous solution into the salt chamber 3, control the flow rate to 1000 h / L, connect the direct current 12, control the temperature of each chamber at 50 °C, and control the current density at 600 A / m 2 , Obtaining the tetrabutylammonium hydroxide aqueous solution that finished product content is 15%. Its bromide ion concentration is 29 ppm; current efficiency is 39%.

Embodiment 3

[0040] Add 35% tetrabutylammonium bromide aqueous solution into the salt chamber 3, control the flow rate to 1000 h / L, connect the direct current 12, control the temperature of each chamber to 30 °C, and control the current density to be constant at 600 A / m 2 , Obtaining the tetrabutylammonium hydroxide aqueous solution that finished product content is 15%. Its bromide ion concentration is 25 ppm; current efficiency is 32%.

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Abstract

The invention relates to a method for preparing high-purity tetrabutyl ammonium hydroxide by continuous electrolysis, particularly relates to a method for preparing high-purity tetrabutyl ammonium hydroxide by using tetrabutyl ammonium bromide as a raw material and adopting a three-compartment bipolar membrane electrodialysis device, and belongs to the field of organic chemistry. The method is characterized by comprising the following step: by adopting the three-compartment bipolar membrane electrodialysis device, continuously preparing 5-20% tetrabutyl ammonium hydroxide by using a 15-35% tetrabutyl ammonium bromide aqueous solution as a raw material under the condition that the reaction temperature is 30-60 DEG C, the current density is 200-600A/m<2> and the flow rate of the raw materials is 500-2000L/h, wherein the concentration of bromine ions in the prepared tetrabutyl ammonium hydroxide is less than 100ppm. According to the method provided by the invention, the materials in the compartments are relatively constant in concentration, the temperature is relatively constant, an ionic membrane is not easy to swell or shrink, the membrane cost is saved, the current efficiency and the product conversion ratio are improved and the energy consumption is reduced, and moreover, the product quality is further improved. The method is suitable for industrial safe production on a large scale, clean in production process and free of discharge of wastewater and solid wastes.

Description

technical field [0001] The invention relates to a method for continuously electrolytically preparing high-purity tetrabutylammonium hydroxide, in particular to a method for continuously preparing high-purity tetrabutylammonium hydroxide by using a three-compartment bipolar membrane electrodialysis device, and belongs to the field of organic chemistry. 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, and polarographic analysis reagents. 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 tetr...

Claims

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Application Information

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IPC IPC(8): C25B3/00
Inventor 赵文洲
Owner 赵文洲
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