A kind of preparation method of methyl three long-chain aliphatic ammonium carbonate

A hydrocarbyl ammonium carbonate, long-chain technology, applied in the preparation of organic carbonates, the preparation of amino compounds, the preparation of organic compounds, etc., can solve the problems of large consumption of acids and bases, complicated processes, impure products, etc., to reduce acidity. The effect of alkali consumption, expansion of application range and conversion rate improvement

Active Publication Date: 2019-06-28
CENT SOUTH UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

[0003] Aiming at the technical problems that the existing method for preparing methyl tri-long-chain aliphatic ammonium carbonate salts has impure products, complex processes, large consumption of acid and alkali, and high cost, the purpose of the present invention is to provide a high-yield A method for preparing high-purity methyl three long-chain aliphatic ammonium carbonate salts with high efficiency. Compared with the existing anion exchange transformation method, the method greatly simplifies the process steps, and can effectively remove bromide and iodine salt catalysts, improving the methyl three The purity of the long-chain aliphatic ammonium carbonate has expanded its application range. For example, the high-purity methyl tri-long-chain aliphatic ammonium carbonate is used in the alkaline extraction process of tungsten, molybdenum and vanadium in rare metal metallurgy, which can bring better application effect

Method used

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  • A kind of preparation method of methyl three long-chain aliphatic ammonium carbonate
  • A kind of preparation method of methyl three long-chain aliphatic ammonium carbonate
  • A kind of preparation method of methyl three long-chain aliphatic ammonium carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Measure 240mL N235, 240mL dimethyl carbonate, 120mL anhydrous methanol, weigh 25.0g (trioctylmethyl quaternary ammonium bromide) catalyst, add it to a 1L autoclave, heat up to 110°C, and react at 1.1-2.4MPa After 8 hours, after the reaction stopped, it was cooled, and the solvent and unreacted dimethyl carbonate were distilled off under reduced pressure. The conversion of N235 was 95.39%. Add the distilled tri-long-chain fatty alkyl quaternary ammonium ester into 400 mL of potassium hydroxide solution with a concentration of 2 mol / L under stirring, and react at 80°C for 9 hours, then let stand to separate the phases, separate the oil phase and the water phase, The oil phase is carbonate-type quaternary ammonium salt (containing water, which can be removed under reduced pressure), with a yield of 93.77%, and wherein the content of bromine element is 1.67%.

Embodiment 2

[0039] Measure 240mL trioctyl tertiary amine, 240mL dimethyl carbonate, 120mL anhydrous methanol, add 27.8g (trioctylmethyl quaternary ammonium bromide) catalyst, add it to a 1L autoclave, raise the temperature to 115 ° C, at 1.7 ~2.7MPa reacted for 6 hours, after the reaction stopped, cooled, and evaporated the solvent and unreacted dimethyl carbonate under reduced pressure. The conversion rate of trioctyl tertiary amine is 97.19%. Add the distilled trioctyl methyl quaternary ammonium ester to 400mL sulfuric acid solution with a concentration of 2mol / L under stirring, react at room temperature for half an hour, let stand to separate the phases, separate the oil phase and the water phase, and the oil phase is sulfuric acid The root type quaternary ammonium salt (containing water, which can be removed under reduced pressure) has a yield of 95.83%, and wherein the bromine content is 1.85%.

Embodiment 3

[0041] Measure 240mL trioctyl tertiary amine, 240mL dimethyl carbonate, 120mL anhydrous methanol, add 28.0g (trioctylmethyl quaternary ammonium iodide) catalyst, add it to a 1L autoclave, raise the temperature to 110°C, at 1.75 ~2.7MPa reacted for 6 hours, after the reaction stopped, cooled, and evaporated the solvent and unreacted dimethyl carbonate under reduced pressure. The conversion rate of trioctyl tertiary amine is 92.78%. Add the distilled trioctylmethyl quaternary ammonium ester to 300mL hydrochloric acid solution with a concentration of 3mol / L under stirring, react at room temperature for half an hour, let stand to separate the phases, separate the oil phase and the water phase, and the oil phase is three Octylmethylammonium chloride (water-containing, decompressed to remove water), its yield is 94.27%, wherein the iodine element content is 2.33%.

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Abstract

The invention discloses a preparation method of methyl tri-long-chain aliphatic group ammonium carbonate. The method comprises the following steps: performing quaternization reaction on tri-long-chain aliphatic group tertiary amine and dimethyl carbonate, thus obtaining a mixture containing methyl tri-long-chain aliphatic group mono-ester quaternary ammonium salt carbonate; performing reduced pressure distillation on the mixture to recycle dimethyl carbonate, placing the mixture into an alkaline solution for hydrolysis reaction, and performing oil-water separation on a hydrolysis reaction product, wherein an oil phase is the methyl tri-long-chain aliphatic group ammonium carbonate. According to the preparation method, the methyl tri-long-chain aliphatic group ammonium carbonate which is high in yield and high in purity can be obtained; furthermore, the preparation method has the characteristics of simple step and low cost; the high-purity methyl tri-long-chain aliphatic group ammonium carbonate can be further converted into a high-purity halide ion, sulfate ion and bicarbonate ion type quaternary ammonium salt derivative which can be widely applied to extractive metallurgy, and particularly to the extraction industry of oxygen-containing negative ions such as tungsten, molybdenum and vanadium.

Description

technical field [0001] The present invention relates to a kind of preparation method of methyl tri-long-chain aliphatic hydrocarbon ammonium carbonate salt, particularly a kind of methyl tri-long-chain aliphatic hydrocarbon-based monomethyl carbonate quaternary ammonium salt intermediate synthesized by bromide or iodine salt as a catalyst, and then The invention discloses a method for obtaining methyl tri-long-chain aliphatic ammonium carbonate salt by hydrolyzing an intermediate, which belongs to the fields of organic synthesis and fine chemical industry. Background technique [0002] Methyl three long-chain fatty alkyl quaternary ammonium salts are a very important class of organic chemicals. They are mainly used as bactericides, detergents, extractants and antistatic agents in petrochemicals, agricultural chemicals, medicine and hygiene, textiles, Hydrometallurgy and daily chemical industries, etc. The ammonizing agents of the cationic quaternary ammonium salt derivative...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/00C07C211/63
CPCC07C68/06C07C209/00C07C211/63C07C69/96
Inventor 曹佐英李嘉豪张贵清肖连生李青刚曾理关文娟李嘉
Owner CENT SOUTH UNIV
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