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Method for recovering dimethylamine from dimethylamine hydrochloride

A technology of dimethylamine hydrochloride and dimethylamine, which is applied in the field of recycling chemical and pharmaceutical raw materials, can solve the problems of high operation difficulty, high recycling cost, harsh reaction conditions, etc., achieve high efficiency, convenient operation, and solve environmental problems problem effect

Inactive Publication Date: 2013-07-03
DALIAN NETCHEM CHIRAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the dimethylamine hydrochloride produced in industrial production contains more impurities, it is difficult to obtain high-purity dimethylamine after treatment, the recovery cost is high, and the waste is difficult to handle, which leads to the recovery of dimethylamine hydrochloride from dimethylamine hydrochloride. Amines cannot be produced on a large scale
[0005] Existing methods for recovering dimethylamine from dimethylamine hydrochloride mostly use calcium oxide solids and dimethylamine hydrochloride solids to heat and react to recover dimethylamine. However, due to the harsh reaction conditions of this method, the operation is difficult and the The generated waste is difficult to deal with, which limits the widespread promotion of industrialization
[0006] For recovering high-purity dimethylamine from dimethylamine hydrochloride, and low-cost, low-risk, easy-to-operate method, there is no other report

Method used

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Examples

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Effect test

example 1

[0022] Add 80g (50%) dimethylamine hydrochloride solution and 30g toluene to a 500ml four-necked flask equipped with a mechanical stirrer, thermometer, reflux condenser, distillation condenser and receiving bottle, and add dropwise at 60~65°C 47g (42%) sodium hydroxide solution. The reflux condenser is fed with circulating water, the interior of the reflux condenser is filled with 5g of solid sodium hydroxide, the distillation condenser is fed with a cooling medium below -10°C, and the receiving bottle is cooled with a cooling medium below -5°C. After starting the stirring, the temperature was raised to 78°C, and kept at 78°C until no dimethylamine flowed out, and the reaction was completed. Collect about 20g of dimethylamine with a water content of <0.2%, and the yield is about 90%. After the reaction solution was separated, 56 g of water was distilled from the lower water layer at 95-110 °C, cooled to 30-35 °C and filtered to obtain 15 g of sodium chloride solid waste.

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Abstract

The invention discloses a method for recovering dimethylamine from dimethylamine hydrochloride, which comprises the following steps: the dimethylamine hydrochloride and sodium hydroxide aqueous solution are reacted through taking toluene as solvent; and dimethylamine is recovered and obtained through heating, rectification, and arefaction with solid sodium hydroxide. The recovering method provided by the invention has high efficiency, is convenient for operation, solves the problem of recovering and reusing the dimethylamine from the dimethylamine hydrochloride, can be used for effectively recovering high purity dimethylamine from the dimethylamine hydrochloride, solves the problem of environment protection in waste treatment as obtained waste sodium chloride can be easily treated, and is suitable for large scale industrial production.

Description

technical field [0001] The invention relates to a method for recovering chemical and pharmaceutical raw materials, in particular to a method for recovering dimethylamine from dimethylamine hydrochloride. Background technique [0002] Dimethylamine is a gas at room temperature and has an ammonia-like odor. It is mainly used as a rubber vulcanization accelerator, leather dehairing agent, medicine, pesticide, textile industry solvent, dye, explosive, propellant and dimethylhydrazine, N,N - Raw materials for organic intermediates such as dimethylformamide. Dimethylamine is an important intermediate of pesticides, and can be used to prepare fungicides thiram, thiram, thiram zinc, thiram nickel, thiram arsenic, tuzet, pyrimol; insecticides piricarb, dimehypo, Monosultap, feticide, and cyprofen; herbicides chlorotoluron, isoproturon, hexazinone, fluuron, etc. [0003] Dimethylamine hydrochloride is mainly used as a catalyst in acetylation analysis, and also used in organic synt...

Claims

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Application Information

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IPC IPC(8): C07C211/04C07C209/68C07C209/86
Inventor 国宏伟张乙吴星娥李峰王治峰
Owner DALIAN NETCHEM CHIRAL TECH
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