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Method for producing 1, 3-dimethyl -2-imidazolinone

An imidazolinone and production method technology, applied in the field of synthesis 1, can solve the problems of low product purity, low product yield, high raw material cost, etc., and achieve the effects of wide sources, high conversion rate, and less three wastes

Inactive Publication Date: 2005-05-18
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current 1,3-dimethyl-2-imidazolinone production synthesis method has one-step method and two-step method, but no matter which synthetic route, there are obvious defects in production: the product yield is low (≤ 80%), or the product purity is not high (≤98%), or the raw material cost is too high

Method used

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  • Method for producing 1, 3-dimethyl -2-imidazolinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 305Kg of ethylenediamine, 391Kg of urea, and 549Kg of water into a 3000-liter reactor, stir and dissolve, react at 100-160°C for 15 hours, cool, crystallize, filter, and wash the filter cake with water three times to obtain 2- The imidazolinone crude product is 432Kg.

[0020] Add 344Kg of 2-imidazolinone, 1800Kg of 80% formic acid, and 1300Kg of 36% formaldehyde in a 5000-liter reactor, stir and dissolve, and react at 120°C for 16 hours, steam the unreacted formaldehyde, Formic acid and water, add cuprous chloride 50Kg, triethylamine 13Kg, stir and react at 120°C for 6 hours; cool to room temperature, filter, take the filtrate, distill, collect the fraction above 100°C, add anhydrous calcium chloride , stirred, and filtered; 375Kg of 1,3-dimethyl-2-imidazolidinone was obtained. After analysis, the product content was 99.51%, and the moisture content was 0.10%.

Embodiment 2

[0022] Add 305Kg of ethylenediamine, 391Kg of urea, and 275Kg of water into a 3,000-liter reactor, stir and dissolve, react at 100-160°C for 15 hours, cool, crystallize, filter, and wash the filter cake with water three times to obtain 2- The imidazolinone crude product is 512Kg.

[0023] Add 344Kg of 2-imidazolinone, 1800Kg of 80% formic acid, and 1300Kg of 36% formaldehyde in a 5000-liter reactor, stir and dissolve, and react at 120°C for 16 hours, steam the unreacted formaldehyde, Formic acid and water, add cuprous chloride 50Kg, triethylamine 13Kg, stir and react at 120°C for 6 hours; cool to room temperature, filter, take the filtrate, distill, collect the fraction above 100°C, add anhydrous calcium chloride , stirred, and filtered; 295Kg of 1,3-dimethyl-2-imidazolidinone was obtained. After analysis, the product content was 97.58%, and the moisture content was 0.18%.

Embodiment 3

[0025] Add 305Kg of ethylenediamine, 391Kg of urea, and 840Kg of water into a 3000-liter reactor, stir and dissolve, react at 100-160°C for 15 hours, cool, crystallize, filter, and wash the filter cake with water three times to obtain 2- The imidazolinone crude product is 372Kg.

[0026] Add 344Kg of 2-imidazolinone, 1800Kg of 80% formic acid, and 1300Kg of 36% formaldehyde in a 5000-liter reactor, stir and dissolve, and react at 120°C for 16 hours, steam the unreacted formaldehyde, Formic acid and water, add cuprous chloride 50Kg, triethylamine 13Kg, stir and react at 120°C for 6 hours; cool to room temperature, filter, take the filtrate, distill, collect the fraction above 100°C, add anhydrous calcium chloride , stirred, and filtered; 370Kg of 1,3-dimethyl-2-imidazolidinone was obtained. After analysis, the product content was 99.48%, and the moisture content was 0.12%.

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Abstract

The production process of 1, 3-dimethyl-2-imidazolinone includes the following technological steps: synthesizing 2-imidazolinone with ethylene diamine and urea as material and water as solvent; and synthesizing 1, 3-dimethyl-2-imidazolinone with 2-imidazolinone, formaldehyde and formic acid as material. The present invention has the advantages of high yield, including the yield of 2-imidazolinone of 95 % and the yield of 1, 3-dimethyl-2-imidazolinone of 90 %, wide material source, low material cost, reuse of the solvent, and less waste.

Description

Technical field: [0001] The invention relates to a chemical synthesis method, mainly a production method for synthesizing 1,3-dimethyl-2-imidazolidinone with ethylenediamine, urea, formaldehyde (paraformaldehyde) and formic acid as raw materials. Background technique: [0002] 1,3-Dimethyl-2-imidazolidinone, also known as dimethylethylene urea, or DMI for short, is a polar solvent with high boiling point, high flash point, low melting point, extremely low toxicity, and extremely Low pollution and strong solubility, it has strong stability, resistant to strong acid, strong alkali, water, light and oxygen. As an organic solvent and chemical raw material, it is widely used in medicine, pesticides, dyes, liquid crystal materials and other fields. The current 1,3-dimethyl-2-imidazolinone production synthesis method has one-step method and two-step method, but no matter which synthetic route, there are obvious defects in production: the product yield is low (≤ 80%), or the produ...

Claims

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Application Information

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IPC IPC(8): C07D233/32
CPCY02P20/582
Inventor 胡健陈国建胡江瑜谢自强
Owner ZHEJIANG XINHUA CHEM
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