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Preparation method of methyl orthoaminobenzoate by means of microchannel reactor

A technology of methyl anthranilate and methyl anthranilate, which is applied in the field of preparing methyl anthranilate by using a microchannel reactor, can solve the problems of low purity and yield of methyl anthranilate, and achieves Good heat and mass transfer effect, no amplification effect, excellent repeatability

Inactive Publication Date: 2017-06-30
田振民 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main purpose of the present invention is to overcome the defects in the existing method for preparing methyl anthranilate, and provide a new method for preparing methyl anthranilate using a microchannel reactor to solve the problems of the prior art The purity and yield of methyl anthranilate are not high, so it is more suitable for practical use and has industrial utilization value

Method used

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  • Preparation method of methyl orthoaminobenzoate by means of microchannel reactor
  • Preparation method of methyl orthoaminobenzoate by means of microchannel reactor
  • Preparation method of methyl orthoaminobenzoate by means of microchannel reactor

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Effect test

Embodiment 1

[0041] Pump material storage tank A (phthalimide source solution) and material storage tank B (sodium hypochlorite solution) into the microchannel reactor at a volume ratio of 1:1.55. Among them, in material storage tank A (phthalimide source solution), the concentration of phthalimide is 2.3mol / L, the concentration of sodium hydroxide is 4.0mol / L, and the concentration of methanol is 11.0mol / L L. In the B material storage tank (sodium hypochlorite solution), the concentration of the sodium hypochlorite is 13%. The microchannel reactor is composed of MRX, MRH-II and MRH-I connected in series, and the phthalimide source liquid and sodium hypochlorite solution are pumped into the microchannel reactor. The residence time in the microchannel reactor was 30 seconds, and the reaction temperature was -5°C. The reaction solution from the microchannel reactor MRH I was detected, and the conversion rate was 100%, and the mass yield was 89.5%.

Embodiment 2

[0043] Pump material storage tank A (phthalimide source solution) and material storage tank B (sodium hypochlorite solution) into the microchannel reactor at a volume ratio of 1:1.55. Wherein in the A material storage tank (phthalimide source solution), the concentration of phthalimide is 2.3mol / L, the concentration of sodium hydroxide is 2.4mol / L, and the concentration of methanol is 10.5mol / L L. In the B material storage tank (sodium hypochlorite solution), the concentration of the sodium hypochlorite is 13%. The microchannel reactor is composed of MRX, MRH-II and MRH-I connected in series, and the phthalimide source solution and sodium hypochlorite solution are pumped into the microchannel reactor. The residence time in the microchannel reactor was 25 seconds, and the reaction temperature was -5°C. The reaction liquid from the microchannel reactor MRH I was detected, and the conversion rate was 100%, and the mass yield was 85.0%.

Embodiment 3

[0045] A material storage tank (phthalimide source solution) and B material storage tank (sodium hypochlorite solution) are pumped into the microchannel reactor according to a volume ratio of 1:1.55, wherein the A material storage tank (phthalimide amine source solution), the concentration of phthalimide is 4.0mol / L, the concentration of sodium hydroxide is 4.0mol / L, and the concentration of methanol is 11.0mol / L. In the B material storage tank (sodium hypochlorite solution), the concentration of the sodium hypochlorite is 15%. The microchannel reactor is composed of MRX, MRH-II and MRH-I connected in series, and the phthalimide source solution and sodium hypochlorite solution are pumped into the microchannel reactor. The residence time in the microchannel reactor was 23 seconds, and the reaction temperature was -5°C. The reaction liquid from the microchannel reactor MRH I was detected, and the conversion rate was 100%, and the mass yield was 84.3%.

[0046] Table 1 is the re...

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Abstract

The invention relates to a method of preparing methyl orthoaminobenzoate by means of a microchannel reactor. The method is characterized by comprising the following steps of: pumping a phthalimide source liquid and a sodium hypochlorite solution into a mixing module MRX of the microchannel reactor; and after mixed reaction, feeding the mixture into a reaction module MRH of the microchannel reactor again for Hofmann degradation reaction to obtain methyl orthoaminobenzoate, wherein the volume ratio of the phthalimide source liquid to the sodium hypochlorite solution is 1: (1.0-2.2). The method provided by the invention is short in reaction time, the prepared methyl orthoaminobenzoate product is high in purity and high in yield, the production cost is greatly lowered, and the production efficiency is increased.

Description

technical field [0001] The invention relates to a method for preparing methyl anthranilate, in particular to a method for preparing methyl anthranilate using a microchannel reactor. Background technique [0002] As an intermediate of dyes, medicines, pesticides, and spices, methyl anthranilate is widely used in the fields of medicine, pesticides, spice processing, and fine chemicals. It is widely found in natural plants such as lemon jasmine oil, ylang-ylang, gardenia, and tuberose oil. Therefore, with its high added value and wide application value. [0003] At present, the method for synthesizing methyl anthranilate is mainly o-nitrobenzoic acid reductive esterification method, or using anthranilic acid as raw material, it is obtained through salt formation, diazotization, reduction and cyclization. The document "Essence, Fragrance and Cosmetics"-2007, 03 proposed a kind of o-nitrobenzoic acid as raw material, synthesized methyl o-nitrobenzoate through esterification, th...

Claims

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Application Information

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IPC IPC(8): C07C227/04C07C229/56B01J19/00
CPCC07C227/04B01J19/0093C07C229/56
Inventor 田振民王继龙焦丽娟田子馨
Owner 田振民
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