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Method for continuous hydrogenation synthesis of 1, 3-dimethyl-2-imidazole based on serial microreactors

A technology of microreactor and dimethyl, which is applied in the field of chemical reaction, can solve the problems of low production efficiency, low product purity, high production cost, etc., and achieve the effects of prolonging service life, high mass transfer efficiency and strong heat transfer ability

Pending Publication Date: 2022-04-26
河北康壮环保科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Traditional reactor-type hydrogenation has problems such as low production efficiency, low purity of the prepared product, and high production cost.

Method used

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  • Method for continuous hydrogenation synthesis of 1, 3-dimethyl-2-imidazole based on serial microreactors

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for continuously hydrogenating 1,3-dimethyl 2-imidazole based on series microreactors, the steps are as follows:

[0029] (1) Formaldehyde and 2-imidazolidinone are mixed according to the molar ratio of 2.5:1, dissolved in a solvent with a mass ratio of methanol to water of 1:2, and prepared into a methanol-water solution of 2-imidazolidinone with a concentration of 5 wt%. ;

[0030] (2) The methanol-water solution of 2-imidazolidinone in step (1) is passed through the micro-packed bed 1 with sulfonic acid group ion exchange resin, reacted for 5min at 70°C under the condition of a pressure of 3.0MPa, and carried out non- Homogeneous hydrogenation reduction reaction to prepare imine intermediate solution;

[0031] (3) The imine intermediate solution prepared in step (2) is mixed with hydrogen at the inlet micro-mixer according to a molar ratio of 2.5:1 to form a gas-liquid mixed fluid;

[0032] (4) The gas-liquid mixed fluid obtained in step (3) is passed thro...

Embodiment 2

[0035] A method for continuously hydrogenating 1,3-dimethyl 2-imidazole based on series microreactors, the steps are as follows:

[0036] (1) Formaldehyde and 2-imidazolidinone are mixed according to the molar ratio of 3.2:1, dissolved in a solvent with a mass ratio of methanol to water of 1:5, and prepared into a methanol-water solution of 2-imidazolidinone with a concentration of 10 wt%. ;

[0037] (2) The methanol-water solution of 2-imidazolidinone in step (1) is passed through the micro-packed bed 1 with carboxylic acid-based ion exchange resin, and reacted for 10 minutes at 80 ° C under the condition of 3.5 MPa, and carried out non-toxic Homogeneous hydrogenation reduction reaction to prepare imine intermediate solution;

[0038] (3) The imine intermediate solution prepared in step (2) is mixed with hydrogen in the inlet micro-mixer according to a molar ratio of 3:1 to form a gas-liquid mixed fluid;

[0039] (4) The gas-liquid mixed fluid obtained in step (3) is passed...

Embodiment 3

[0042] A method for continuously hydrogenating 1,3-dimethyl 2-imidazole based on series microreactors, the steps are as follows:

[0043] (1) Formaldehyde and 2-imidazolidinone are mixed according to the molar ratio of 2.5:1, dissolved in a solvent with a mass ratio of methanol to water of 1:10, and prepared into a methanol-water solution of 2-imidazolidinone with a concentration of 5 wt%. ;

[0044] (2) the methanol-water solution of the 2-imidazolidinone of step (1) is passed through packing with solid acid catalyst H 2 SO 4 The micro-packed bed 1 of / C reacted for 5 minutes at 80°C and a pressure of 3.0 MPa, and carried out a heterogeneous hydrogenation reduction reaction to prepare an imine intermediate solution;

[0045] (3) The imine intermediate solution prepared in step (2) is mixed with hydrogen in the inlet micro-mixer according to a molar ratio of 4:1 to form a gas-liquid mixed fluid;

[0046](4) The gas-liquid mixed fluid obtained in step (3) is passed through t...

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Abstract

The invention discloses a method for continuous hydrogenation synthesis of 1, 3-dimethyl-2-imidazole based on serial microreactors, and belongs to the technical field of chemical reactions. The method comprises the following steps: dissolving 2-imidazolidone and formaldehyde in a solvent according to a certain ratio to prepare a mixed solution with a certain concentration, mixing the mixed solution with a solid acid catalyst to prepare an imine intermediate solution, then mixing the imine intermediate solution with hydrogen to obtain a gas-liquid mixed fluid, carrying out hydrogenation reduction, and finally carrying out gas-liquid separation on the gas-liquid mixture to obtain the 2-imidazolidone. The purity of the product is higher than 97%. The microreactor is used for mixing efficiently and has excellent mass and heat transfer performance, so that the heat transfer capacity of the reactor is improved, the volume of the reactor can be remarkably reduced, and the reaction yield is improved. The method can solve the problems of low production efficiency, poor product purity, high device risk and the like in a hydrogenation kettle intermittent synthesis process, can realize continuous automatic operation of the process, directly reduces the industrial cost, and realizes safe and environment-friendly production.

Description

technical field [0001] The invention relates to the technical field of chemical reactions, in particular to a method for continuously hydrogenating 1,3-dimethyl 2-imidazole based on series microreactors. Background technique [0002] 1,3-Dimethyl-2 imidazolidinone (DMI) is a transparent and colorless polar aprotic solvent. Its excellent solubility can dissolve many polar organic and inorganic substances. It can be mixed with water in any proportion. Miscible. It has the characteristics of low toxicity, safety and stability. Widely used in petrochemical, pharmaceutical, electronic chip and other fields. The synthesis methods of DMI include carbon dioxide method, phosgene method, trichloroacetyl chloride method, urea method, and 2-imidazolidinone methylation method. At present, the industrial production of DMI mainly uses urea and ethylenediamine as raw materials to synthesize 2-imidazolidinone, and then N-methylates 2-imidazolidinone to obtain the product DMI. 2-Imidazoli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/32B01J19/00
CPCC07D233/32B01J19/0093B01J19/0046
Inventor 张吉松刘宁黄蒙蒙吴俊杰尹佳滨吴玉才
Owner 河北康壮环保科技股份有限公司
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