Method for producing 5-nitroguaiacol sodium salt by using micro-channel reaction device

A technology of microchannel reaction and sodium guaiacol, applied in chemical instruments and methods, preparation of nitro compounds, chemical/physical/physical-chemical reactors, etc., can solve the problems of harsh reaction conditions and low product yield, etc. To achieve the effect of short reaction time, improved reaction conversion rate, and controllable reaction temperature

Pending Publication Date: 2020-06-26
郑州郑氏化工产品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a method for producing 5-nitroguaiacol sodium using a microchannel reaction device to solve the problems of harsh reaction conditions and low product yield in the prior art

Method used

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  • Method for producing 5-nitroguaiacol sodium salt by using micro-channel reaction device
  • Method for producing 5-nitroguaiacol sodium salt by using micro-channel reaction device
  • Method for producing 5-nitroguaiacol sodium salt by using micro-channel reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Pump the guaiacol-acetic anhydride solution containing the acidic catalyst in the raw material kettle I into the microchannel reactor I for reaction, the mass ratio of guaiacol, acetic anhydride and phosphoric acid is 1:0.86:0.005, and the reaction condition is 120°C Keep at low temperature for 10 minutes to obtain acetylguaiacol solution. The acetylguaiacol solution was cooled to 48° C. for later use. The purity of acetylguaiacol was 99.7% as detected by liquid phase.

Embodiment 2-9

[0046] Adopt the raw material proportioning identical with embodiment 1, under certain temperature, keep for a period of time, get the acetylguaiacol solution that microchannel reactor 1 comes out and detect.

[0047] The reaction product purity of table 1 embodiment 2-9

[0048]

Embodiment 10-11

[0050] Using the same mass ratio of guaiacol, acetic anhydride and acidic catalyst as in Example 1, the same reaction temperature of 120°C and the same retention time of 10min, the difference is that in Example 10, phosphoric acid is changed to sulfuric acid. 11 Change phosphoric acid to trifluoroacetic acid.

[0051] The reaction product purity of table 2 embodiment 10-11

[0052] Example acid catalyst Acetylguaiacol Purity 10 sulfuric acid 98.5％ 11 Trifluoroacetate 99.5％

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Abstract

The invention discloses a method for continuously producing 5-nitroguaiacol sodium salt by using a micro-channel reaction device. The method comprises the following steps of: (1) pumping a guaiacol-acetic anhydride solution containing an acidic catalyst into a micro-channel reactor I for reaction to obtain an acetyl guaiacol solution; (2) respectively pumping the cooled acetyl guaiacol solution and a nitric acid-acetic acid mixed solution into a micro-channel reactor II simultaneously for reaction to obtain a 5-nitroacetyl guaiacol solution; (3) cooling the 5-nitroacetyl guaiacol solution, pouring the 5-nitroacetyl guaiacol solution into water for crystallization, performing filtering, and collecting filter residue to obtain a 5-nitroacetyl guaiacol wet product; and (4) adding the 5-nitroacetyl guaiacol wet product into a sodium hydroxide solution, carrying out heating reaction, at the end of the reaction, conducting cooling, crystallizing and filtering, collecting the filter residue,and performing drying to obtain the 5-nitroguaiacol sodium salt. According to the method, the utilization rate of acetic anhydride reaches 95% or above, the nitration reaction yield is increased to 90% or above, and the three-step yield of 5-nitroguaiacol sodium salt is 80% or above.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and technology, and specifically relates to a method for efficiently producing 5-nitroguaiacol sodium through a microchannel reaction device by using guaiacol, acetic anhydride, nitric acid and sodium hydroxide. Background technique [0002] 5-Nitroguaiacol sodium is the main active ingredient of a new plant production regulator, sodium nitrophenolate. It can quickly penetrate into plants, regulate and control the synthesis of nucleic acids, proteins and enzymes in plants, and promote the synthesis of cell protoplasm. Flow, increase cell viability, thereby promoting plant germination, rooting, growth, reproduction and fruiting, and has obvious effects on improving crop quality, increasing production and increasing income. Due to its low toxicity and high efficiency, it and its compound sodium nitrophenolate have been formulated and recommended by the Food and Agriculture Organization of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/37C07C201/08C07C205/43C07C67/08C07C69/157B01J19/00
CPCC07C201/12C07C201/08C07C67/08B01J19/0093C07C69/157C07C205/43C07C205/37
Inventor 许伟长郑先福郑昊刘志山
Owner 郑州郑氏化工产品有限公司
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