Method for recycling methylamine hydrochloride

A technology of methylamine hydrochloride and methylcarbamoyl chloride, applied in the field of recycling of methylamine hydrochloride, can solve the problems of long reaction process, large consumption of phosgene, high reaction temperature, etc., to reduce energy consumption and Discharge of three wastes, simple process and high yield

Inactive Publication Date: 2010-11-24
HUNAN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has high reaction temperature, strict requirements on equipment materials, long reaction process and large consumption of phosgene

Method used

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  • Method for recycling methylamine hydrochloride
  • Method for recycling methylamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 67.5g (1.0mol) of methylamine hydrochloride, 500g (4.11mol) of chloroform, and 130g (1.31mol) of liquid phosgene into a 1000mL autoclave, stir and raise the temperature to 110°C, the pressure of the autoclave is 2.3MPa, and continue the reaction for 4h , down to room temperature after the reaction. The reaction liquid is filtered, and the weight percentage of methylcarbamoyl chloride in the filtrate is 12.5%. After the phosgene is removed by the dephosphorization tower, it enters the circulation system of the MIC production device. The filter residue is returned to the autoclave to enter the reaction process of the next batch of methylamine hydrochloride. The conversion rate of methylamine hydrochloride was 73%, and the yield was 91.8% (calculated as methylamine hydrochloride).

Embodiment 2

[0014] Add 67.5g (1.0mol) of methylamine hydrochloride, 500g (4.12mol) of chloroform, and 100g (1.01mol) of liquid phosgene into a 1000mL autoclave, stir and raise the temperature to 110°C, the pressure of the autoclave is 2.0MPa, and continue the reaction for 4h , down to room temperature after the reaction. The reaction liquid is filtered, and the weight percent of carbamoyl chloride in the filtrate is 12.2%, and the phosgene is removed by the degassing tower, and then enters the circulation system of the MIC production device. The filter residue is returned to the autoclave to enter the reaction process of the next batch of methylamine hydrochloride. The conversion rate of methylamine hydrochloride was 71.2%, and the yield was 90.5% (calculated as methylamine hydrochloride).

Embodiment 3

[0016] Add 67.5g (1.0mol) of methylamine hydrochloride, 500g (5.05mol) of 1,2-dichloroethane, 120g (1.21mol) of liquid phosgene into a 1000mL autoclave, stir and heat up to 85°C, and the pressure of the autoclave is 1.7 MPa continued to react for 5h, and the reaction was completed and dropped to room temperature. The reaction liquid is filtered, and the weight percentage of methylcarbamoyl chloride in the filtrate is 10.8%. After the phosgene is removed by the degassing tower, it enters the circulation system of the MIC production device. The filter residue is returned to the autoclave to enter the reaction process of the next batch of methylamine hydrochloride. The conversion rate of methylamine hydrochloride was 62.2%, and the yield was 93.5% (calculated as methylamine hydrochloride).

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Abstract

The invention discloses a method for recycling methylamine hydrochloride to prepare methylamino formyl chloride. The methylamino formyl chloride is prepared by adopting a high-pressure reaction, using an organic solvent as a reaction solvent, and reacting the methylamine hydrochloride with phosgene, wherein the yield in terms of the methylamine hydrochloride is more than or equal to 90.0 percent. The method for recycling the methylamine hydrochloride has a simple process and a mild reaction condition; the used solvent is suitable for industrialized requirements; and reaction solution is directly used without purification after filtration and phosgene removal, and the three-waste amount is greatly reduced.

Description

technical field [0001] The invention relates to a method for recycling methylamine hydrochloride, in particular to a method for recycling methylamine hydrochloride produced during the production of methyl isocyanate (MIC). Background technique [0002] Methylamine hydrochloride is the basic raw material for the synthesis of medicines, pesticides, dyes and other organic synthesis. Its molecular formula is: [0003] CH 3 NH 2 HCl [0004] The treatment method of the by-product methylamine hydrochloride waste residue or methylamine hydrochloride wastewater produced in industry generally has three kinds at present: 1, steam stripping or gaseous membrane method: the aqueous solution of methylamine hydrochloride is adjusted pH ≥ 11, makes The vast majority of ammonia or organic amine exists in a free state, and 99% or more of ammonia or organic amine can be removed in water to obtain a by-product of ammonia or organic amine aqueous solution concentrated 5-20 times by volume, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C271/04C07C269/06C07C263/10C07C265/04
Inventor 熊前政肖旭辉臧阳凌孔晓红李萍王燕阳勇强高洪建
Owner HUNAN CHEM RES INST
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