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Method for preparing long-chain alkyl ammonium hydroxide

A long-chain alkyl and ammonium hydroxide technology, which is applied in the preparation of amino compounds from amines, organic chemistry, electrolysis process, etc., can solve the problems of low purity, large amount of resin, serious environmental pollution, etc., and achieve surface activity, The effect of low equipment requirements and high product purity

Active Publication Date: 2013-09-04
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent CN1417201A uses quaternary ammonium salts to react with inorganic bases in organic solvents to obtain long-chain alkyl ammonium hydroxides. In this method, because inorganic bases have certain solubility in organic solvents, the solution of the target product inevitably contains certain A large amount of metal ions such as potassium and sodium, the purity of the product is not high
Chinese patent CN1428330A adopts anion exchange resin to prepare corresponding long-chain alkyl ammonium hydroxide by quaternary ammonium salt, and this method resin consumption is very large, and pretreatment and regeneration can consume a large amount of high-purity acid-base, produce a large amount of waste acid and waste alkali simultaneously, and cost is lower high
Chinese patent CN101680101A describes the preparation of long-chain alkyl ammonium hydroxide by electrolysis of halogenated quaternary ammonium salts. This method generates halogen gas during the electrolysis process, causing serious environmental pollution, and the generation of strong acidic solutions will corrode electrodes and electrolysis equipment.
Secondly, the product contains halide ions, which affects the purity of the product
For the synthesis of tetraalkyl ammonium methyl carbonate by dimethyl carbonate and tertiary amine reaction, the corresponding long-chain alkyl ammonium hydroxide that tetraalkyl methyl ammonium carbonate arrives after hydrolysis, electrolysis has no report

Method used

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  • Method for preparing long-chain alkyl ammonium hydroxide
  • Method for preparing long-chain alkyl ammonium hydroxide
  • Method for preparing long-chain alkyl ammonium hydroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: 110.2g of dodecyldimethyl tertiary amine, 190.7g of dimethyl carbonate and 15.2g of methanol were added to the reaction kettle, stirred and reacted at 120°C for 8h, after the reaction was completed, the mixture was distilled off under reduced pressure Methanol and dimethyl carbonate to obtain ammonium dodecyl methyl ammonium carbonate, weigh 20.7g ammonium dodecyl methyl ammonium carbonate and 103.7g water, add them to the flask, stir and react at 70°C for 3h, and obtain dodecyl trimethyl ammonium carbonate Methyl ammonium bicarbonate aqueous solution, dodecyl trimethyl ammonium bicarbonate is prepared into a solution with a concentration of 0.8mol / L, and added to the anode of a single-membrane two-chamber electrolytic cell equipped with a polystyrene sulfonic acid membrane cation exchange membrane In the chamber, the cathode chamber is filled with deionized water, the anode is a titanium electrode coated with ruthenium oxide, the cathode is a stainless steel ...

Embodiment 2

[0036] Example 2: 107.3g of didodecylmethyl tertiary amine, 70.3g of dimethyl carbonate and 27.3g of methanol were added to the reaction kettle, stirred and reacted at 140°C for 7h, after the reaction was completed, the mixture was distilled off under reduced pressure Methanol and dimethyl carbonate to obtain didodecyl ammonium methyl ammonium carbonate, weigh 19.5g didodecyl methyl ammonium carbonate and 138.3g water, add them to a flask, stir and react at 60°C for 5h, and obtain didodecyl ammonium methyl ammonium carbonate Alkyl dimethyl ammonium bicarbonate aqueous solution, didodecyl dimethyl ammonium bicarbonate is prepared into a solution with a concentration of 0.8mol / L, and added to a single-membrane two-chamber electrolysis chamber equipped with a perfluorosulfonic acid membrane cation exchange membrane In the anode chamber of the tank, add 0.02mol / L dodecyl dimethyl ammonium hydroxide solution to the cathode chamber, the anode is a titanium electrode coated with iridi...

Embodiment 3

[0037] Example 3: 105.6g of dodecyl dimethyl tertiary amine, 77.9g of dimethyl carbonate and 21.8g of methanol were added to the reaction kettle, stirred and reacted at 100°C for 20h, after the reaction was completed, it was removed by distillation under reduced pressure Methanol and dimethyl carbonate to obtain ammonium dodecyl methyl ammonium carbonate. Weigh 17.3g of ammonium dodecyl methyl ammonium carbonate and 156.0g of water, add them to a flask, stir and react at 30°C for 7h, and obtain dodecyl ammonium methyl ammonium carbonate. Aqueous solution of methyl ammonium bicarbonate, dodecyl trimethyl ammonium bicarbonate is prepared into a solution with a concentration of 0.55mol / L, and added to the anode chamber of a single-membrane two-chamber electrolyzer equipped with a perfluorocarboxylic acid cation exchange membrane , add 0.5mol / L dodecyltrimethylammonium hydroxide solution in the cathode chamber, the anode is a titanium electrode coated with ruthenium oxide, the cath...

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Abstract

The invention relates to a method for preparing long-chain alkyl ammonium hydroxide. The method comprises the following steps of: reacting tertiary amine with dimethyl carbonate to obtain long-chain alkyl methylamine carbonate; hydrolyzing the long-chain alkyl methylamine carbonate to obtain long-chain alkyl ammonium bicarbonate; and electrolyzing the long-chain alkyl ammonium bicarbonate to prepare the corresponding long-chain alkyl ammonium hydroxide with high purity. The method is pollution-free, low in cost and high in purity.

Description

technical field [0001] The invention belongs to a method for preparing alkyl ammonium hydroxide, in particular to a method for preparing long-chain alkyl ammonium hydroxide. technical background [0002] Tetraalkylammonium hydroxides are strong organic bases of equal strength to caustic. And long-chain alkyl ammonium hydroxide can be applied in many fields because it not only has strong alkalinity, but also has surface activity. Long-chain alkyl ammonium hydroxide refers to ammonium hydroxide with more than 10 carbon atoms. [0003] Chinese patent CN1417201A uses quaternary ammonium salts to react with inorganic bases in organic solvents to obtain long-chain alkyl ammonium hydroxides. In this method, because inorganic bases have certain solubility in organic solvents, the solution of the target product inevitably contains certain A large amount of metal ions such as potassium and sodium, the purity of the product is not high. Chinese patent CN1428330A adopts anion exchang...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00C07C211/63C07C209/68
Inventor 耿涛滕晓光李秋小姜亚洁
Owner CHINA RES INST OF DAILY CHEM IND
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