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Preparation method of acetoxime methyl ether

A technology of acetone oxime methyl ether and acetone oxime, which is applied in the field of preparation of acetone oxime methyl ether, to achieve the effects of reducing cost and energy consumption, increasing yield, and mild reaction conditions

Active Publication Date: 2021-09-24
ZHEJIANG JINHUA NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there is no method for industrialized production of acetoxime methyl ether. How to produce acetone oxime methyl ether efficiently and at low cost is a problem that the industry is more concerned about at present.

Method used

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  • Preparation method of acetoxime methyl ether
  • Preparation method of acetoxime methyl ether
  • Preparation method of acetoxime methyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of preparation method of acetone oxime methyl ether, its scheme is:

[0029] Add 80kg of acetone oxime, 60kg of sodium hydroxide, 1kg of phase transfer catalyst and 600kg of toluene into the reactor, control the temperature at 40°C, mix and stir for 10min, then control the reaction temperature at 50°C, then start to feed 120kg of monochloromethane into the reactor, The control is completed within 30 minutes; then the heat preservation reaction is carried out for 10 minutes; after the reaction is completed, the crude solid sodium chloride is separated, the filtrate is pumped to the evaporator, heated to about 60°C with steam, and the acetone oxime methyl ether in the filtrate is evaporated The condenser condenses and flows into the crude product tank, and then the obtained acetone oxime methyl ether crude product is circulated and heated through the ether tower reboiler, and a small amount of water is condensed through the ether rectification tower condenser and fl...

Embodiment 2

[0037] A kind of preparation method of acetone oxime methyl ether, its scheme is:

[0038]Add 120kg of acetone oxime, 9kg of sodium hydroxide, 3kg of phase transfer catalyst and 700kg of toluene into the reactor, control the temperature at 50°C, mix and stir for 30min, then control the reaction temperature at 60°C, then start to feed 180kg of monochloromethane into the reactor, The control is completed within 40 minutes; then the heat preservation reaction is carried out for 20 minutes; after the reaction is completed, the crude solid sodium chloride is separated, the filtrate is pumped to the evaporator, heated to about 70°C with steam, and the acetone oxime methyl ether in the filtrate is evaporated The condenser condenses and flows into the crude product tank, and then the obtained acetone oxime methyl ether crude product is circulated and heated through the ether tower reboiler, and a small amount of water is condensed through the ether rectification tower condenser and flo...

Embodiment 3

[0046] A kind of preparation method of acetone oxime methyl ether, its scheme is:

[0047] Add 180kg of acetone oxime, 120kg of sodium hydroxide, 5kg of phase transfer catalyst and 800kg of toluene into the reactor, control the temperature at 60°C, mix and stir for 60min and then control the reaction temperature at 70°C, then start to feed 220kg of methylene chloride into the reactor, The control is completed within 60 minutes; then the heat preservation reaction is carried out for 30 minutes; after the reaction is completed, the crude solid sodium chloride is separated, the filtrate is pumped to the evaporator, heated to about 80°C with steam, and the acetone oxime methyl ether in the filtrate is evaporated The condenser condenses and flows into the crude product tank, and then the obtained acetone oxime methyl ether crude product is circulated and heated through the ether tower reboiler, and a small amount of water is condensed through the ether rectification tower condenser ...

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Abstract

The invention relates to the field of chemical engineering, in particular to a preparation method of acetoxime methyl ether, which comprises the following steps: performing etherification reaction on acetoxime, methane chloride and sodium hydroxide under the action of a phase transfer catalyst to generate acetoxime methyl ether, and rectifying to obtain the finished product of acetoxime methyl ether. The reaction conditions are mild, the operation is simple, the synthesis is easy, the byproduct acetone can be recycled, and the cost and the energy consumption can be reduced; under the action of the heteropolyacid salt phase transfer catalyst, the etherification reaction can solve the problem of compatibility during the organic-inorganic two-phase reaction and improve the reaction efficiency and yield, and meanwhile, the catalyst also has an etherification catalysis effect and is beneficial to forward movement of the reaction and increase of the yield of the product; compared with the prior art, the reaction yield is higher, the material utilization rate is large, and the preparation method of the acetoxime methyl ether has an industrial prospect.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of acetone oxime methyl ether. Background technique [0002] Oxime ether derivatives are a class of compounds with excellent biological activity, not only widely used in medicine, but also an important class of active compounds in pesticides. Acetone oxime methyl ether is a promising pharmaceutical intermediate. [0003] CN106083644A relates to 1-phenyl-2-alicyclic ketoxime ethers represented by chemical structural formulas Ia, Ib, IIa and IIb and their pesticide-acceptable salts: in the formula, R is selected from: C1~C4 straight-chain alkyl Or C3~C4 branched chain alkyl; n is selected from: 1, 2, 3 or 4; X1~X4 is selected from: hydrogen, methyl, ethyl, fluorine, chlorine, bromine, iodine; R1 is selected from: hydrogen, methyl Base, ethyl, C3~C7 straight chain alkyl and branched chain alkyl, C2~C5 alkenyl, C2~C5 chloroalkenyl or C2~C5 alkynyl; Y1, Y5 are s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/12C07C251/54B01J31/24C08F226/06C08F8/42
CPCC07C249/12B01J31/24C08F226/02C08F8/42B01J2531/64C07C251/54C08F226/06Y02P20/584
Inventor 周黎旸周强茅志清段仲刚徐碧涛张军良
Owner ZHEJIANG JINHUA NEW MATERIALS
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