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Efficient synthetic method for N-methyl MF resin solution

A technology of methylformamide and a synthesis method, which is applied in the field of efficient synthesis of N-methylformamide, can solve the problems of large catalyst usage, increased preparation cost and the like, and achieves the effects of high activity, cost saving and good stability

Inactive Publication Date: 2018-11-27
SUZHOU GAIDE FINE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is simple, continuous production, and low cost of raw material consumption. The composite catalyst used is a mixture of copper oxide, zinc oxide, aluminum oxide, phosphorus pentoxide, and sodium oxide, but the amount of catalyst used in the reaction process is relatively large, effectively increasing preparation cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The efficient synthetic method of N-methylformamide comprises the following steps:

[0027] (1) Mix zinc nitrate, iron nitrate, and aluminum acetate into deionized water, stir until the solid dissolves, and prepare a mixed solution; wherein, the mass ratio of zinc nitrate, iron nitrate, and aluminum acetate is 1:1:1;

[0028] (2) Stir in the ethylenediaminetetraacetic acid and ethanol solution until the solid dissolves to obtain an ethylenediaminetetraacetic acid solution with a mass concentration of 5%;

[0029] (3) Add ethylenediaminetetraacetic acid solution dropwise to the mixed solution prepared in step (1). After the dropwise addition, raise the temperature to 80-90°C, reflux for 30 minutes while stirring, cool to room temperature, and then pour into the mixed solution Drop ammonia water for precipitation for 1 hour, filter, wash the precipitate with deionized water and absolute ethanol in turn, and dry to obtain a catalyst precursor; wherein, the mass ratio of et...

Embodiment 2

[0034] The efficient synthetic method of N-methylformamide comprises the following steps:

[0035] (1) Mix zinc nitrate, iron nitrate, and aluminum acetate into deionized water, stir until the solid dissolves, and prepare a mixed solution; wherein, the mass ratio of zinc nitrate, iron nitrate, and aluminum acetate is 5:1:2;

[0036] (2) Stir in the ethylenediaminetetraacetic acid and ethanol solution until the solid dissolves to obtain an ethylenediaminetetraacetic acid solution with a mass concentration of 10%;

[0037] (3) Add ethylenediaminetetraacetic acid solution dropwise to the mixed solution prepared in step (1). After the dropwise addition, raise the temperature to 80-90°C, reflux for 50 minutes while stirring, cool to room temperature, and then add Add ammonia water to precipitate for 6 hours, filter, wash the precipitate with deionized water and absolute ethanol in turn, and dry to obtain a catalyst precursor; wherein, the mass ratio of ethylenediaminetetraacetic ac...

Embodiment 3

[0042] The efficient synthetic method of N-methylformamide comprises the following steps:

[0043] (1) Zinc nitrate, ferric nitrate, and aluminum acetate are mixed and added into deionized water, stirred until the solid is dissolved, and a mixed solution is obtained; wherein, the mass ratio of zinc nitrate, ferric nitrate, and aluminum acetate is 2:1:1;

[0044] (2) Stir in the ethylenediaminetetraacetic acid and ethanol solution until the solid dissolves to obtain an ethylenediaminetetraacetic acid solution with a mass concentration of 6%;

[0045] (3) Add ethylenediaminetetraacetic acid solution dropwise to the mixed solution prepared in step (1). After the dropwise addition, heat up to 80-90°C, reflux for 35 minutes while stirring, cool to room temperature, and then pour into the mixed solution Add ammonia water to precipitate for 2 hours, filter, wash the precipitate with deionized water and absolute ethanol in turn, and dry to obtain a catalyst precursor; wherein, the mas...

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PUM

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Abstract

The invention discloses an efficient synthetic method for an N-methyl MF resin solution. The method comprises the following steps: firstly, preparing a catalyst precursor by means of a co-precipitating method; adding EDTA in the preparation process, wherein the growth speed of a precipitate is controlled effectively; then sintering the catalyst precursor to prepare catalyst powder; activating andmodifying the catalyst powder with N-isopropyl acrylamide and triethylene tetramine to prepare a catalyst; then carrying out dehydrogenizing catalytic treatment on methanol under catalysis of the catalyst to prepare methyl formate; and then reacting with methylamine to prepare a target product N-methyl formamide. The method is simple to operate, the adopted catalyst is high in catalytic activity,and the prepared target product is high in purity and high in yield.

Description

Technical field: [0001] The invention relates to the field of organic synthesis, in particular to an efficient synthesis method of N-methylformamide. Background technique: [0002] N-Methylformamide, a colorless transparent liquid, miscible with water and ethanol, has an ammonia smell, boiling point: 198-199°C (101.1kPa), it is mainly used as a raw material for organic synthesis, and is often used in the synthesis of medicines. The preparation method of N-methylformamide mainly contains following several kinds at present: (1) methylamine method is made by the reaction of methylamine and carbon monoxide. (2) The methyl formate method is obtained by reacting methyl formate and methylamine. Add ethyl formate to the reactor, add methylamine aqueous solution under cooling, and reflux at 40°C. Then stand for 3d, and recover ethanol under reduced pressure to obtain the crude product. Then the finished product is obtained by vacuum distillation. (3) Add calcium chloride to the mi...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/03B01J23/80
CPCB01J23/002B01J23/80B01J2523/00C07C67/00C07C231/02B01J2523/27B01J2523/31B01J2523/842C07C233/03C07C69/06
Inventor 李晓明
Owner SUZHOU GAIDE FINE MATERIALS CO LTD
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