Method for industrially producing crotonic acid by adopting microchannel reactor

A micro-channel reactor, a technology for industrial production, applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of carboxylate salts, etc. Process development and other issues, to achieve the effect of reducing production steps, avoiding a large number of emissions, and shortening the reaction time

A micro-channel reactor, a technology for industrial production, applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of carboxylate salts, etc. Process development and other issues, to achieve the effect of reducing production steps, avoiding a large number of emissions, and shortening the reaction time

CN114560765AActive Publication Date: 2022-05-31广西金源生物化工实业有限公司
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  • Method for industrially producing crotonic acid by adopting microchannel reactor
  • Method for industrially producing crotonic acid by adopting microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] A kind of method adopting microchannel reactor industrial production crotonic acid, carries out according to the following steps:

[0050] S1. Material oxidation process: Cobalt acetate, activated alumina, and iron phosphomolybdate are used in a weight ratio of 1:1:1 to form a composite catalyst, and the initiators are selected from acetonitrile, dimethylformamide, and dimethylacetamide in a weight ratio of 1 :1:2 composite initiator. The gaseous oxidant is passed into the silicon carbide ceramic plate microchannel reactor, the gaseous oxidant is oxygen+air, ​​and the consumption of the gaseous oxidant (according to O 2 The molar weight of the form) is 25±2% of the mass of crotonaldehyde. When the pressure in the silicon carbide ceramic plate microchannel reactor reaches 1.6MPa, the crotonaldehyde, catalyst, and initiator (weight ratio 1:0.015:0.15) are mixed and pre- After heating to 30~35°C, inject it into the microchannel reactor through a metering pump, the materia...

Embodiment 2

[0057] A kind of method adopting microchannel reactor industrial production crotonic acid, carries out according to the following steps:

[0058] S1. Material oxidation process: Cobalt acetate, activated alumina, and iron phosphomolybdate are used in a weight ratio of 1:1:1 to form a composite catalyst, and the initiators are selected from acetonitrile, dimethylformamide, and dimethylacetamide in a weight ratio of 1 :1:2 composite initiator. The gaseous oxidant (air + oxygen) is passed into the silicon carbide ceramic plate microchannel reactor, and the amount of oxygen oxidant (according to O 2 The molar weight of the form) is 30±2% of the mass of crotonaldehyde. When the pressure in the silicon carbide ceramic plate microchannel reactor reaches 0.8MPa, mix and preheat the crotonaldehyde, catalyst, and initiator (weight ratio 1:0.01:0.30) After reaching 30~35°C, it is injected into the microchannel reactor through a metering pump, the material flow rate is 900±10ml / min, the ...

Embodiment 3

[0065] A kind of method adopting microchannel reactor industrial production crotonic acid, carries out according to the following steps:

[0066] S1. Material oxidation process: Cobalt acetate, activated alumina, and iron phosphomolybdate are used in a weight ratio of 1:1:1 to form a composite catalyst, and the initiators are selected from acetonitrile, dimethylformamide, and dimethylacetamide in a weight ratio of 1 :1:2 composite initiator. The gaseous oxidant (air + oxygen) is passed into the silicon carbide ceramic plate microchannel reactor, and the amount of the gaseous oxidant (according to O 2 The molar weight of the form) is 35±2% of the mass of crotonaldehyde. When the internal pressure of the silicon carbide ceramic plate microchannel reactor reaches 1.8MPa, the crotonaldehyde, catalyst, and initiator (weight ratio 1:0.015:0.20) are mixed and pre- After heating, it is injected into the microchannel reactor through a metering pump, the material flow rate is 1000±10ml...

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Abstract

The invention discloses a method for industrially producing crotonic acid by adopting a microchannel reactor, and relates to the technical field of chemical production of crotonic acid. A silicon carbide ceramic plate type micro-channel reactor is adopted, crotonaldehyde, a catalyst and an initiator are mixed and preheated according to a certain proportion, meanwhile, a gaseous oxidizing agent is introduced into the reactor, when the pressure in the reactor reaches 0.6-2.0 MPa, the mixed solution is injected into the micro-channel reactor through a metering pump for a reaction, the retention time of the materials is 8-30 min, and then the crotonaldehyde is obtained. The crotonic acid finished product can be obtained through the processes of material oxidation, crude product crystallization, crude product fine washing, fine product crystallization, drying granulation, catalyst regeneration and the like, the one-time yield of the product can reach 60%, and the mechanical application yield can reach 95%. The method has the advantages of good mass transfer and heat transfer effects, short oxidation reaction time, high product yield, high safety degree, few process steps, recyclable catalyst, low production cost, recyclable raw materials in each step, high reaction speed, low wastewater energy consumption and the like.

Description

technical field [0001] The invention relates to the technical field of chemical production of crotonic acid, in particular to a method for industrially producing crotonic acid using a microchannel reactor. Background technique [0002] Crotonic acid is an important chemical intermediate, which is widely used in many fields such as medicine, pesticides, dyes, spices, photosensitive chemicals, polymer catalysts, and biodiesel additives. [0003] The existing crotonic acid preparation methods are mainly divided into two types: non-catalytic oxidation production and catalytic oxidation production. (1) Non-catalytic oxidation production: the patent texts of Publication Nos. CN1396148 and CN101979371A respectively disclose the method of preparing crotonic acid without any catalyst oxidation. Using the data of the examples in the patent document of Publication No. CN1396148, it is found that the utilization rate of crotonaldehyde is only About 20±2%. (2) Catalytic oxidation produ...

Claims

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Application Information

Patent Timeline
31 May 2022
Publication
CN114560765A
IPC
C07C51/235; C07C51/42; C07C51/43; C07C51/47; C07C57/08; B01J21/04; B01J27/19; B01J31/04; B01J31/28; B01J31/40
CPC
C07C51/235; C07C51/42; C07C51/43; C07C51/47; B01J31/04; B01J31/28; B01J31/4053; B01J27/19
Inventors
程克; 黄晓磊