Synthesizing technology and device for improving nicosulfuron purity

A technology for the synthesis of nicosulfuron and nicosulfuron, which is applied in the field of synthesis technology and devices for improving the purity of nicosulfuron, can solve the problems of reducing the separation effect of the rectification tower, low yield content, long reaction time, etc., and achieve shortening Effect of reaction cycle, avoidance of environmental pollution, shortening of reaction time

Inactive Publication Date: 2018-03-06
JINGBO AGROCHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the route to synthesize nicosulfuron is mainly 3-[(N,N-dimethylcarbamoyl)-2-pyridyl]sulfonylcarbamate (referred to as urethane) and 4,6 dimethoxy Base-2-pyrimidinamine (referred to as pyrimidineamine) is condensed to remove a molecule of ethanol. In this method, rectification is used to separate ethanol, but the rectification time is generally between 20-40 hours and the reaction time is longer. The ethanol extracted from the top contains par...

Method used

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  • Synthesizing technology and device for improving nicosulfuron purity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the reactor, throw 120Kg (0.4Kmol) of urethane, 68.2Kg (0.44Kmol) of pyrimidinamine, and 900Kg of toluene. Throw 7.5kg (0.068Kmol) of calcium chloride in the calcium chloride storage tank, and throw 300Kg (3.26 Kmol) of toluene in the heating kettle. The reaction kettle and the heating kettle are heated at the same time, and the temperature of the reaction kettle is raised to boiling. The mixed steam of toluene and ethanol is condensed by the condenser and enters the calcium chloride storage tank to absorb ethanol. After that, the toluene enters the heating kettle to heat up and return to the reaction kettle. This operation is a continuous operation process. The content of ethanol in the toluene in the reaction kettle is lower than 0.0005% by sampling, the reaction is stopped, the temperature is lowered and centrifuged, and the product content after drying is 98.3%, and the yield is 98.4%.

Embodiment 2

[0017] In the reactor, throw 120Kg (0.4Kmol) of urethane, 68.2Kg (0.44Kmol) of pyrimidinamine, and 900Kg of toluene. Throw 7.9kg (0.072Kmol) of calcium chloride in the calcium chloride storage tank, and throw 300Kg (3.26 Kmol) of toluene in the heating kettle. The reaction kettle and the heating kettle are heated at the same time, and the temperature of the reaction kettle is raised to boiling. The mixed steam of toluene and ethanol is condensed by the condenser and enters the calcium chloride storage tank to absorb ethanol. After that, the toluene enters the heating kettle to heat up and return to the reaction kettle. This operation is a continuous operation process. The content of ethanol in the toluene in the reaction kettle is lower than 0.0005% by sampling, the reaction is stopped, the temperature is lowered and centrifuged, and the product content after drying is 98.4%, and the yield is 98.3%.

Embodiment 3

[0019] In the reactor, throw 120Kg (0.4Kmol) of urethane, 68.2Kg (0.44Kmol) of pyrimidinamine, and 900Kg of toluene. Throw 8.8Kg (0.08Kmol) of calcium chloride in the calcium chloride storage tank, and throw 300Kg (3.26 Kmol) of toluene in the heating kettle. The reaction kettle and the heating kettle are heated at the same time, and the temperature of the reaction kettle is raised to boiling. The mixed steam of toluene and ethanol is condensed by the condenser and enters the calcium chloride storage tank to absorb ethanol. After that, the toluene enters the heating kettle to heat up and return to the reaction kettle. This operation is a continuous operation process. The content of ethanol in the toluene in the reaction kettle is sampled to detect 0.0005%, the reaction is stopped, the temperature is lowered and centrifuged, and the product content after drying is 98.2%, and the yield is 98.3%.

[0020] In the process control of the above examples, compared with the existing co...

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Abstract

The invention relates to a synthesizing technology and device for improving nicosulfuron purity. The technology is characterized in that 3-[(N,N-dimethylaminocarbonyl)-2-pyridyl] sulfonylcarbamate, 4,6-dimethoxy-2-pyrilamine and methylbenzene are heated to condense; mixed steam of methylbenzene treated as a solvent in the reaction and ethyl alcohol produced in the condensation enters a condenser;the mixed solution of condensed methylbenzene and ethyl alcohol enters an absorbent storing tank; methylbenzene absorbed through the ethyl alcohol is heated through an absorbent, and then the methylbenzene is added to a reaction kettle; the reaction is stopped when the content of the ethyl alcohol in the mixed steam produced by the reaction kettle is less than 0.0005%; the mixed solution in the reaction is cooled and centrifuged to obtain nicosulfuron. According to the technology, the ethyl alcohol produced in the reaction can be quickly and effectively removed, and the reaction is promoted to forwards perform, thus the purity and the yield of nicosulfuron can be improved; and moreover, the methylbenzene treated as the solvent and taken out through the ethyl alcohol is recycled, so that more energy is saved; and the reaction cycle is greatly reduced through the design, and as a result, the production efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of pesticide compound synthesis, in particular to a synthesis process and device for improving the purity of nicosulfuron. Background technique [0002] The chemical formula of nicosulfuron is 2-(4,6-dimethylpyrimidin-2-pyrimidinylcarbamatesulfonyl)-N,N-dimethylnicotinamide, which is a new generation of broad Spectrum, high efficiency, low concentration, low residue and high selectivity herbicide. At present, the route to synthesize nicosulfuron is mainly 3-[(N,N-dimethylcarbamoyl)-2-pyridyl]sulfonylcarbamate (referred to as urethane) and 4,6 dimethoxy Base-2-pyrimidinamine (referred to as pyrimidineamine) is condensed to remove a molecule of ethanol. In this method, rectification is used to separate ethanol, but the rectification time is generally between 20-40 hours and the reaction time is longer. The ethanol extracted from the top contains part of the toluene solvent, so it is necessary to add an equal...

Claims

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Application Information

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IPC IPC(8): C07D401/12
CPCC07D401/12
Inventor 董燕戴荣华成道泉韦能春王建刚
Owner JINGBO AGROCHEM TECH CO LTD
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