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Method for one-step continuous hydrogenation synthesis of 1, 3-dimethyl-2-imidazolinone based on fixed bed microreactor

A micro-reactor, imidazolinone technology, applied in chemical instruments and methods, chemical/physical/physical-chemical processes, organic chemistry, etc., can solve the problems of hidden dangers of hydrogen safety, high equipment investment costs, and high process costs, and achieve The effect of reducing catalyst dosage, high safety and uniform liquid phase distribution

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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Problems solved by technology

[0003] The two-step hydrogenation reduction of 2-imidazolidinone to prepare DMI greatly improves the cleaning effect of production, but the cost of the traditional reactor process is high and there are safety hazards in the use of a large amount of hydrogen
The use of micro-packed bed continuous hydrogenation reductive amination can reduce production cost to a certain extent, improve production efficiency and safety, but the device is complicated and the equipment input cost is slightly higher

Method used

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  • Method for one-step continuous hydrogenation synthesis of 1, 3-dimethyl-2-imidazolinone based on fixed bed microreactor

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Effect test

Embodiment 1

[0027] A method for continuously synthesizing 1,3-dimethyl-2-imidazolidinone based on one-step method of fixed-bed microreactor hydrogenation, the steps are as follows:

[0028] (1) 2-imidazolidinone is mixed with a solvent, and the solvent is a mixture prepared by methanol and deionized water at a mass ratio of 1:2 to obtain a methanol-water solution of 2-imidazolidinone with a concentration of 5wt%, and then formaldehyde Add formaldehyde at a molar ratio of 2.5:1 to 2-imidazolidinone, and mix with hydrogen at the inlet micro-mixer (molar ratio of hydrogen to 2-imidazolidinone is 3:1) to form a gas-liquid mixed fluid;

[0029] (2) the gas-liquid mixed fluid of step (1) gained flows through the micro-packed bed that is filled with the bifunctional palladium / carbon catalyst of sulfuric acid modification, 140 ℃ of micro-packed bed reaction temperatures, residence time is 2min, pressure 3.5MPa, Carry out heterogeneous hydrogenation reductive amination reaction;

[0030] (3) The ...

Embodiment 2

[0032] A method for continuously synthesizing 1,3-dimethyl-2-imidazolidinone based on one-step method of fixed-bed microreactor hydrogenation, the steps are as follows:

[0033] (1) 2-imidazolidinone is mixed with a solvent, and the solvent is a mixture of methanol and deionized water according to a mass ratio of 1:9 to obtain a methanol-water solution of 2-imidazolidinone with a concentration of 10 wt%. Formaldehyde is added at a molar ratio of 3.2:1 to 2-imidazolidinone, and mixed with hydrogen at the inlet micro-mixer (the molar ratio of hydrogen to 2-imidazolidinone is 4:1) to form a gas-liquid mixed fluid;

[0034] (2) the gas-liquid mixed fluid of step (1) gained flows through the micro-packed bed of the bifunctional palladium / carbon catalyst that is loaded with phosphoric acid modification, and micro-packed bed reaction temperature 160 ℃, residence time is 1min, pressure 3.0MPa, Carry out heterogeneous hydrogenation reductive amination reaction;

[0035] (3) The gas-li...

Embodiment 3

[0037] A method for continuously synthesizing 1,3-dimethyl-2-imidazolidinone based on one-step method of fixed-bed microreactor hydrogenation, the steps are as follows:

[0038] (1) 2-imidazolidinone is mixed with a solvent, and the solvent is a mixture prepared by DMI and deionized water according to a mass ratio of 1:9 to obtain a DMI-water solution of 2-imidazolidinone with a concentration of 15wt%, and then formaldehyde Add formaldehyde at a molar ratio of 2.5:1 to 2-imidazolidinone, and mix with hydrogen at the inlet micro-mixer (molar ratio of hydrogen to 2-imidazolidinone is 3:1) to form a gas-liquid mixed fluid;

[0039] (2) The gas-liquid mixed fluid obtained in step (1) flows through the micro-packed bed filled with phosphoric acid-modified bifunctional palladium / alumina catalyst, the micro-packed bed reaction temperature is 150°C, the residence time is 5min, and the pressure is 2.5MPa , carry out heterogeneous hydrogenation reductive amination reaction;

[0040] (3...

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Abstract

The invention provides a method for one-step continuous hydrogenation synthesis of 1, 3-dimethyl-2-imidazolinone based on a fixed bed microreactor, and belongs to the technical field of chemical reaction engineering. The method comprises the following steps: firstly, mixing a substrate solution to be hydrogenated with formaldehyde to obtain a mixed solution, or adding homogeneous acid into the mixed solution, mixing with hydrogen in an inlet micromixer to obtain a gas-liquid mixed fluid, and then enabling the gas-liquid mixed fluid to pass through a micropacked bed filled with a catalyst to continuously finish a heterogeneous hydrogenation process by a one-step method. According to the method, efficient mixing and excellent mass and heat transfer performance of the microreactor are utilized, gas-liquid and liquid-solid mass transfer in the heterogeneous hydrogenation reaction process is enhanced, the heat transfer capacity of the reactor is improved, the volume of the reactor can be reduced, and the reaction yield is increased. The method can solve the problems of low production efficiency, poor product purity and high device risk in a hydrogenation kettle process, realizes continuous automatic operation of the process, and has the advantages of high yield, good safety and the like.

Description

technical field [0001] The invention relates to the technical field of chemical reaction engineering, in particular to a method for continuously synthesizing 1,3-dimethyl-2-imidazolidinone by one-step continuous hydrogenation in a fixed-bed microreactor. 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-imid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/32B01J19/00
CPCC07D233/32B01J19/0093Y02P20/584
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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