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Preparation method for tetra-alkyl ammonium hydroxide and application

A technology of tetraalkylammonium halide and ammonium hydroxide, which is applied in the preparation of amino compounds, organic compounds, and hydrogen atoms replaced by amino groups. It can solve the problems of high equipment requirements, cumbersome operation, and high energy consumption. Low cost, convenient operation and low energy consumption

Inactive Publication Date: 2010-10-27
JIANGSU YANGNONG CHEM GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: the temperature and pressure of the condensation reaction of trimethylamine and dimethyl carbonate in the first step of this method are relatively high, the requirements for equipment are relatively high, there is certain danger, and the yield of tetramethylammonium hydroxide is on the low side
These reaction processes for preparing tetraalkylammonium halides are all carried out in the presence of water. For the preparation of tetraalkylammonium hydroxide by ion exchange method in the next step, it cannot be directly carried out and must be removed. The operation is cumbersome and can be performed. consumes a lot

Method used

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  • Preparation method for tetra-alkyl ammonium hydroxide and application
  • Preparation method for tetra-alkyl ammonium hydroxide and application
  • Preparation method for tetra-alkyl ammonium hydroxide and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Operation step 1:

[0039] Add 529.56g of trimethylamine methanol solution containing 26.65% of trimethylamine into a 1L reactor, start to feed in methyl chloride gas under stirring, keep the temperature of the reaction solution at 30-35°C, ventilate for about 4 hours, stop ventilating, and the weight of the reaction solution increases About 143.1 g, pH=7. After the reaction, the reaction solution was heated and refluxed for 0.5h, the methyl chloride was absorbed by methanol, and the temperature was lowered to obtain a tetramethylammonium chloride methanol solution, weighing 647.78g. The content of tetramethylammonium chloride (TMACl) was determined to be 40.26%, and the yield was ≥ 99.5%.

[0040] Operation step 2:

[0041] Add 91.88g KOH (1.575mol) to 1L reactor and dissolve in 230g anhydrous methanol, add 391.65g (1.44mol) of the above-mentioned TMACl methanol solution under stirring, and keep warm at 60-70°C for 2h. After the heat preservation is completed, cool ...

Embodiment 2

[0043] Operation step 1:

[0044] Add 588g of trimethylamine methanol solution containing 15% trimethylamine into a 1L reactor, and start to feed in methyl chloride gas under stirring, keep the temperature of the reaction liquid at 20-25°C, ventilate for about 5 hours, stop ventilating, and the weight of the reaction liquid increases by about 79.24g, pH=7. After the reaction, the reaction solution was heated and refluxed for 0.5h, the methyl chloride was absorbed with methanol, and the temperature was lowered to obtain tetramethylammonium chloride methanol solution, weighing 662.1g, and the measured tetramethylammonium chloride (TMACl) content was 24.48%, and the yield≥ 99%.

[0045] Operation step 2:

[0046] Add 68.97g KOH (1.17mol) in 1L reactor and dissolve in 240g anhydrous methanol, add 523.34g (1.17mol) of the above TMACl methanol solution under stirring, and keep warm at 30-35°C for 3h. After the heat preservation is completed, cool down to 20°C with water, desalt t...

Embodiment 3～4

[0048] Change raw material methyl bromide to replace methyl chloride, other conditions are identical with embodiment 1, 2, the results are shown in Table 1.

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Abstract

The invention discloses a preparation method for tetra-alkyl ammonium hydroxide. The preparation method is implemented by the following technical scheme: performing a reaction on trialkylamine and alkyl halide in a single organic solvent to obtain tetra-alkyl ammonium halide; performing ion exchange on the tetra-alkyl ammonium halide and an oxide or a hydroxide of an alkali metal or an alkaline earth metal in the presence of an organic solvent; and obtaining the aqueous solution of the tetra-alkyl ammonium hydroxide by after-treatment. The method has the advantages of convenient raw material source, low cost, simple preparation process, high halide ion-exchange rate and the like. The tetra-alkyl ammonium hydroxide prepared by adopting the method is particularly suitable to be used as a base catalyst, which is used for the condensation of nitrobenzene and aniline for generating 4-nitrodiphenylamine and / or 4-nitrosodiphenylamine and the reduction for generating 4-aminodiphenylamine by hydrogenating. Therefore, the conversion rate of the nitrobenzene is greater than or equal to 99.5 percent and the selectivity is up to over 92 percent.

Description

technical field [0001] The present invention relates to a kind of preparation method of quaternary ammonium base, more specifically, relate to a kind of method of preparation tetraalkylammonium hydroxide, and the application of the product prepared by adopting the method as the condensation catalyst of rubber antioxidant intermediate. Background technique [0002] 4-Aminodiphenylamine, also known as RT base, is mainly used in the production of p-phenylenediamine rubber antioxidants 4010NA, 4020, etc. The production of p-aminodiphenylamine by the aniline nitrobenzene method is a "green production process" successfully developed at home and abroad in the past 10 years, that is, nitrobenzene and aniline are condensed in the presence of an alkali catalyst to generate 4-nitrodiphenylamine and 4-nitroso base diphenylamine, and then hydrogenation reduction in the presence of a catalyst to obtain 4-aminodiphenylamine. For the alkali catalyst used in the condensation reaction, the p...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/68B01J31/02C07C211/56C07C209/02C07C211/55C07C209/36C07C209/38
Inventor 程晓曦史雪芳唐琴顾志强田宇张龙邵波季秋峰
Owner JIANGSU YANGNONG CHEM GROUP
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