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A kind of continuous production method of 1,3-dimethyl-2-imidazolinone

A technology of imidazolinone and production method, applied in 1 field, can solve problems such as no target product, achieve high selectivity, high activity, and prevent sintering effect

Active Publication Date: 2021-08-20
MAIQI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As an emerging green methylation reagent, dimethyl carbonate cannot methylate 2-milineone. From the boiling point of the distilled fraction, there is no formation of the target product

Method used

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  • A kind of continuous production method of 1,3-dimethyl-2-imidazolinone
  • A kind of continuous production method of 1,3-dimethyl-2-imidazolinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The continuous production method of 1,3-dimethyl-2-imidazolidinone of the present invention, the detailed steps of described continuous production method are as follows:

[0052] 1) Preparation of heterogeneous catalyst:

[0053] a. Dissolve nickel nitrate, ferric nitrate, zinc acetate and molybdenum nitrate in deionized water to prepare a solution A with a concentration of 0.8mol / L, stir well; heat up the prepared solution A to 65°C, and then Add a silica sol emulsion with a mass percentage of silica of 20%, and drop it at a temperature of 85°C within 30 minutes; then add a precipitant Na 2 CO 3 Stir to control the end point pH value to 9, move the obtained slurry to a microwave hydrothermal parallel synthesizer to react for 8 hours, filter, wash and bake the obtained reactants in sequence, and calcinate at 650°C for 4 hours after baking. Post-grinding to obtain precursor particles;

[0054] The molar ratio between the contents of Ni, Fe, Zn and Mo in the nickel nit...

Embodiment 2

[0064] The continuous production method of 1,3-dimethyl-2-imidazolidinone of the present invention, the detailed steps of described continuous production method are as follows:

[0065] 1) Preparation of heterogeneous catalyst:

[0066] a. Dissolve nickel nitrate, ferric nitrate, zinc acetate, cobalt nitrate and molybdenum nitrate in deionized water to prepare a solution A with a concentration of 1.0 mol / L, stir well; heat up the prepared solution A to 70 ℃, then add a silica sol emulsion with a mass percentage of silicon dioxide of 15%, and drop it at a temperature of 80 ℃ within 25 minutes; then add a precipitant NaHCO 3 Stirring is carried out to control the pH value at the end point to be 8, and the obtained slurry is transferred to a microwave hydrothermal parallel synthesizer to react for 7 hours, and the obtained reactants are sequentially filtered, washed and baked, and calcined at 750°C for 3 hours after baking. Post-grinding to obtain precursor particles;

[0067] ...

Embodiment 3

[0077] The continuous production method of 1,3-dimethyl-2-imidazolidinone of the present invention, the detailed steps of described continuous production method are as follows:

[0078] 1) Preparation of heterogeneous catalyst:

[0079] a. Dissolve nickel nitrate, ferric nitrate, zinc acetate and molybdenum nitrate in deionized water to prepare a solution A with a concentration of 0.5mol / L, and stir well; heat up the prepared solution A to 60°C, and then Add a silica sol emulsion with a mass percentage of silica of 25%, and drop it at a temperature of 90°C within 20 minutes; then add a precipitant K 2 CO 3 Stir to control the end point pH value to 8, move the obtained slurry to a microwave hydrothermal parallel synthesizer to react for 8 hours, filter, wash and bake the obtained reactants in sequence, and calcinate at 550°C for 4 hours after baking. Post-grinding to obtain precursor particles;

[0080] The molar ratio between the contents of Ni, Fe, Zn and Mo in the nickel ...

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Abstract

The invention discloses a continuous production method of 1,3-dimethyl-2-imidazolinone. First prepare the heterogeneous catalyst, pack the obtained heterogeneous catalyst in the reactor, then add ethylene glycol to carry out circular washing of the heterogeneous catalyst; then add ethylene glycol, mass percent concentration of 40% monomethylamine Aqueous solution and dimethyl carbonate carry out condensation, ring closure reaction, continuously transform into 1,3-dimethyl-2-imidazolinone crude liquid; The crude liquid is continuously purified by four-stage rectification tower or five-stage rectification tower to obtain qualified finished product 1,3-dimethyl-2-imidazolidinone. Utilizing the present invention to prepare 1,3-dimethyl-2-imidazolidinone, the product yield is high, the purity is high, and by-products are few, and the operation is simple, the reaction conditions are mild, and the process is clean, which is suitable for industrial continuous production of 1,3- Dimethyl-2-imidazolinone.

Description

[0001] 1. Technical field: [0002] The invention belongs to the technical field of organic synthesis, and in particular relates to a continuous production method of 1,3-dimethyl-2-imidazolidinone. [0003] 2. Background technology: [0004] 1,3-Dimethyl-2-imidazolidinone, abbreviated as DMI, is a transparent, colorless liquid. At the same time, it is also a kind of polar aprotic solvent. Its excellent solubility can dissolve many polar solvents. The organic and inorganic substances can be miscible with water in any proportion and hydrogen bonds are easier to form between water molecules and DMI. DMI has a half amount of 1300mg / kg (ED 50 ) and a 50% lethal dose (LD) of 2840mg / kg 50 ). So far, no relevant reports about its carcinogenicity have been found. It can replace the carcinogenic HMPA. The active substance of this solvent can reach the damaged part quickly and accurately, and it hardly irritates the skin and has no allergic reaction. It can be maintained for a long tim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/32B01J23/89B01J37/34B01J37/08B01J37/02B01J37/06B01D3/14
CPCB01D3/146B01J23/002B01J23/8993B01J37/0201B01J37/06B01J37/088B01J37/346B01J2523/00C07D233/32B01J2523/17B01J2523/27B01J2523/41B01J2523/54B01J2523/68B01J2523/821B01J2523/842B01J2523/847B01J2523/845B01J2523/31
Inventor 吴彦彬闫广学宋国全肖强杨理吴正岭梁斌杨素阁
Owner MAIQI CHEM CO LTD
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