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Method for preparing tetrabutylammonium hydroxide aqueous solution by anion exchange

A technology of tetrabutylammonium hydroxide and tetrabutylammonium bromide, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problem of slow exchange speed of ion membrane method, high equipment cost and energy consumption cost , low exchange efficiency and other problems, to achieve the effect of improving economic and social benefits, low equipment requirements, and high safety

Active Publication Date: 2017-10-27
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through comparison, it can be found that impurity ions are difficult to remove in the silver oxide method, electrolysis method and potassium hydroxide method, and the separation of raw materials and products is difficult, and the equipment cost and production cost are high; The cost is high; the exchange rate of the ion membrane method is slow and the exchange efficiency is low, which cannot meet the requirements of industrial production to obtain a large number of products; the ion exchange method of strong basic anion exchange resin and tetrabutylammonium bromide is cheap and has low requirements for equipment. Simple process and strong operability
At present, the production of tetrabutylammonium hydroxide in my country mainly adopts the membrane electrolysis method. Although this method has high product purity, it consumes a lot of energy.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0018] [Example 1] Anion exchange resin pretreatment method

[0019] Select 201*4 strong basic anion exchange resin, and its pretreatment method is divided into five steps, specifically:

[0020] (1) With 2 times the resin volume, the temperature T 0 Treat the resin at 50°C with a mass concentration of 1% NaCl aqueous solution, and wash with deionized water until the output is a colorless solution.

[0021] (2) Continue to process the above-mentioned resin with 3 times the volume of the resin, and a NaOH aqueous solution with a mass concentration of 0.5%, and wash with deionized water until the liquid is neutral (pH is 7).

[0022] (3) Continue to treat the resin with 0.5 times the resin volume and 0.5% sodium sulfite aqueous solution, and wash it with deionized water until the effluent is neutral (pH is 7).

[0023] (4) Treat the above-mentioned resin with 2 times the resin volume and 5% HCl aqueous solution, and wash with water until the effluent is neutral (pH is 7).

[...

example 2

[0025] [Example 2] Anion exchange resin pretreatment method

[0026] Choose 201*7 strong basic anion exchange resin, and its pretreatment method is divided into five steps, specifically:

[0027] (1) With 3 times the resin volume, the temperature T 0 Treat the resin at 20°C with a mass concentration of 15% NaCl aqueous solution, and wash with deionized water until the output is a colorless solution.

[0028] (2) Continue to process the above-mentioned resin with 2 times the volume of the resin and a NaOH aqueous solution with a mass concentration of 1%, and wash it with deionized water until the effluent is neutral.

[0029] (3) Continue to process the above-mentioned resin with 1 times the volume of the resin, EDTA with a mass concentration of 1%, and wash with deionized water until the effluent is neutral.

[0030] (4) Treat the resin with 10% HCl solution of 1 times the volume of the resin, and wash with water until the effluent is neutral.

[0031] (5) with temperature ...

example 3

[0032] [Example 3] Anion exchange resin pretreatment method

[0033] Select D290 type strongly basic anion exchange resin, and its pretreatment method is divided into five steps, specifically:

[0034] (1) With 2 times the resin volume, the temperature T 0 Treat the resin with 8% NaCl aqueous solution at 30°C, and wash with deionized water until the output is a colorless solution.

[0035] (2) Continue to process the above-mentioned resin with 2 times the volume of the resin and a NaOH aqueous solution with a mass concentration of 5%, and wash it with deionized water until the effluent is neutral.

[0036] (3) Continue to treat the above-mentioned resin with 0.7 times the resin volume and a mass concentration of 4% tartaric acid, and wash it with deionized water until the effluent is neutral.

[0037] (4) Treat the above resin with 1% HCl solution of 2 times the volume of the resin, and wash with water until the effluent is neutral.

[0038] (5) with temperature T 1 30°C, ...

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PUM

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Abstract

The present invention relates to a kind of method for preparing tetrabutyl ammonium hydroxide aqueous solution by anion exchange, firstly strong basic anion exchange resin is filled in the ion exchange column with external circulation device, is completely converted into OH-type through pretreatment; Then, adjust The flow rate is to pass the tetrabutylammonium bromide aqueous solution into the exchange column for exchange reaction with the resin. At the same time, the exchange reaction temperature is adjusted through the external circulation, and the tetrabutylammonium hydroxide aqueous solution is obtained after the reaction. The invention breaks through the technology of preparing tetrabutylammonium hydroxide aqueous solution with a mass concentration of 25% to 30% by the anion resin exchange method. The resin can be reused after being regenerated and revived. Compared with the electrolysis method, the production cost is greatly reduced, the energy consumption is small, and there is no pollution. A green, low-carbon, environmentally friendly and economical preparation method.

Description

technical field [0001] The invention relates to a method for preparing tetrabutylammonium hydroxide aqueous solution by anion exchange. Background technique [0002] Tetrabutylammonium hydroxide (TBAOH) is an organic strong base, commonly used as chromatographic analysis agent, electronic industry detergent, phase transfer catalyst, surfactant, templating agent, 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. As a chromatographic analysis agent, tetrabutylammonium hydroxide is widely used in industry and scientific research fields. Its ammonium salt, namely tetrabutylammonium salt, has the characteristics of high efficiency and low toxicity, and is often used as a fungicide, and is widely used in medicine, health and other industries. The production method of this product mainly co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/63C07C209/00
Inventor 孔岩林伟
Owner NANJING TECH UNIV
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