Preparation method to recycle pyribenzoxim byproduct dicyclohexylurea

A technology of dicyclohexylurea and saflufenacil, which is applied in the field of agrochemicals, can solve problems affecting the continuous production of saflufenacil, inconsistencies in green manufacturing, and potential safety hazards, and achieve safe and green industrial production and waste utilization , the effect of reducing emissions

Inactive Publication Date: 2018-12-25
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The above-mentioned methods all have safety hazards, or use phosphorus pentoxide or phosphorus oxychloride as raw materials, or produce hydrogen sulfide gas with the smell of rotten eggs in the process, all of which have serious safety problems, seriously pollute the environment, and are not compatible with green manufacturing. match
[0004] Our research group invented a method for preparing saf

Method used

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  • Preparation method to recycle pyribenzoxim byproduct dicyclohexylurea
  • Preparation method to recycle pyribenzoxim byproduct dicyclohexylurea

Examples

Experimental program
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Embodiment 1

[0025] Put the by-product DCU (170g) and the catalyst 1-phenyl-3-methyl-phosphole-1-oxide (3.4g) into a 1000mL reactor, heat to 150°C for reaction, and react at 150°C After 12 hours, cool to 80°C to react, filter to recover the catalyst, distill the filtrate under reduced pressure, collect fractions at 125-130°C (6mmHg), and cool to obtain white solid DCC with a yield of 84.4% and a purity of 98.3%.

Embodiment 2

[0027] Put the by-product DCU (170g) and the catalyst 1-phenyl-3-methyl-phosphole-1-oxide (1.7g) into a 1000mL reactor, heat to 160°C for reaction, and react at 160°C 8h, cooled to 70°C for reaction, recovered the catalyst by filtration, distilled the filtrate under reduced pressure, collected fractions at 125-130°C (6mmHg), and cooled to obtain white solid DCC with a yield of 88.2% and a purity of 98.1%.

Embodiment 3

[0029] Put the by-product DCU (170g) into a 1000mL reactor, recover the catalyst 1-phenyl-3-ethyl-phosphole-1-oxide (2.1g), heat to 140°C for reaction, and react at about 140°C React for 18 hours, cool to 60°C to react, filter to recover the catalyst, distill the filtrate under reduced pressure, collect fractions at 135-140°C (8mmHg), and cool to obtain white solid DCC with a yield of 85.1% and a purity of 98.4%.

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Abstract

The invention discloses a preparation method to recycle pyribenzoxim byproduct dicyclohexylurea and belongs to the field of agricultural chemistry. The byproduct N,N'-dicyclohexylurea is used as a rawmaterial; N,N'-dicyclohexylurea and organic phosphorus catalyst are heated to 140-160 for reacting; the temperature is then lowered to 60-80 DEG C for reacting; after reacting, the catalyst is recycled by filtering, and filtrate is distilled under reduced pressure; distillate at 125-140 DEG C (6-8 mmHg) is collected and cooled to obtain white solid, N,N'-dicyclohexylcarbodiimide; the highest yield reaches 88.2%, and purity reaches 98.4%. The preparation method is efficient, environmentally friendly, sustainable, and suitable for industrial production; the preparation method has the advantagesof good energy efficiency, low consumption, lower pollutant emission and the like, allows a preparation technique of recycling byproducts of pyribenzoxim production process to be implemented, and meets the green manufacturing principle.

Description

technical field [0001] The invention relates to a method for preparing dicyclohexylcarbodiimide (DCC) by recovering and applying the by-product N,N'-dicyclohexylurea (DCU) produced in the production process of pyrimidin saflufenacil, in particular to a method utilizing The method for preparing DCC by using DCU as a raw material belongs to the field of agricultural chemistry. Background technique [0002] DCC (Dicyclohexylcarbodiimide), that is, N, N'-dicyclohexylcarbodiimide, is a dehydrating agent commonly used in industries and laboratories to synthesize aldehydes, ketones, amino acids, acid anhydrides, esters and other compounds, and is widely used in medicine and pesticides , materials and other fine chemical industries. With the rapid development of modern agriculture, the market demand for DCC is more and more strong. Zhang Guangyou and others reported the method of using dicyclohexyl thiourea method to synthesize DCC, that is, reacting cyclohexylamine and carbon dis...

Claims

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Application Information

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IPC IPC(8): C07C267/00
CPCC07C267/00C07C2601/14Y02P20/584
Inventor 徐德锋徐祥建
Owner CHANGZHOU UNIV
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