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Production process of p-toluenesulfonamide urea

A technology of toluenesulfonamide urea and p-toluenesulfonyl chloride, which is applied in the field of production process of p-toluenesulfonamide urea, can solve the problems of inconvenient automatic continuous production, complex synthesis process steps, large amount of organic solvent, etc., and achieve the convenience of automation Continuous production, good reduction effect, easy removal effect

Pending Publication Date: 2020-12-15
嘉兴市金利化工有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 1. The reaction efficiency is low, the degree of reaction is low, it is difficult to remove impurities, the yield is low, and the cost is high;
[0005] 2. The synthesis process steps are relatively complicated, the amount of organic solvent is large, the pollution is serious, and the safety is poor;
[0006] Therefore, it is not convenient for automatic continuous production

Method used

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  • Production process of p-toluenesulfonamide urea

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A p-toluenesulfonamido urea production process comprises the following steps:

[0035] S1. Put ammonium sulfite into the reaction kettle and dissolve it in 3 to 5 times of water; then add sodium hydroxide to dissolve the sodium hydroxide; then add p-toluenesulfonyl chloride to reduce p-toluenesulfonyl chloride to p-toluene Sulfinate, obtain p-toluene sulfinate aqueous solution;

[0036] S2. Add azodicarbonamide to the p-toluenesulfinate aqueous solution obtained in step S1 to react, and stop the reaction when no gas is released; cool down, filter, wash with water, and dry to obtain the target product p-toluenesulfonamide base urea;

[0037] The reaction temperature in the step S2 is 75-77°C.

[0038] Preferably, in step S1, the molar ratio of p-toluenesulfonyl chloride to ammonium sulfite is 1:1.25-1.35.

[0039] Preferably, in step S1, the molar ratio of p-toluenesulfonyl chloride to sodium hydroxide is 1:1.005-1.008.

[0040] Preferably, the reaction temperature i...

Embodiment 2

[0047] A p-toluenesulfonamido urea production process comprises the following steps:

[0048] S1. Put ammonium sulfite into the reaction kettle and dissolve it in 3 times of water; then add sodium hydroxide and dissolve the sodium hydroxide; then add p-toluenesulfonyl chloride to reduce p-toluenesulfonyl chloride to p-toluenesulfinic acid Acid salt, obtain p-toluene sulfinic acid salt aqueous solution;

[0049] S2. Add azodicarbonamide to the p-toluenesulfinate aqueous solution obtained in step S1 to react, and stop the reaction when no gas is released; cool down, filter, wash with water, and dry to obtain the target product p-toluenesulfonamide base urea;

[0050] The reaction temperature in the step S2 is 75°C.

[0051] In this embodiment, in step S1, the molar ratio of p-toluenesulfonyl chloride to ammonium sulfite is 1:1.25.

[0052] In this embodiment, in step S1, the molar ratio of p-toluenesulfonyl chloride to sodium hydroxide is 1:1.005.

[0053] In this embodiment...

Embodiment 3

[0060] A p-toluenesulfonamido urea production process comprises the following steps:

[0061] S1. Put ammonium sulfite into the reaction kettle and dissolve it in 5 times of water; then add sodium hydroxide and dissolve the sodium hydroxide; then add p-toluenesulfonyl chloride to reduce p-toluenesulfonyl chloride to p-toluenesulfinic acid Acid salt, obtain p-toluene sulfinic acid salt aqueous solution;

[0062] S2. Add azodicarbonamide to the p-toluenesulfinate aqueous solution obtained in step S1 to react, and stop the reaction when no gas is released; cool down, filter, wash with water, and dry to obtain the target product p-toluenesulfonamide base urea;

[0063] The reaction temperature in the step S2 is 77°C.

[0064] In this embodiment, in step S1, the molar ratio of p-toluenesulfonyl chloride to ammonium sulfite is 1:1.35.

[0065] In this embodiment, in step S1, the molar ratio of p-toluenesulfonyl chloride to sodium hydroxide is 1:1.008.

[0066] In this embodiment, ...

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Abstract

The invention discloses a production process of p-toluenesulfonamide urea, and the process comprises the following steps: S1, adding ammonium sulfite into a reaction kettle, dissolving the ammonium sulfite in 3-5 times of water, then adding sodium hydroxide and dissolving sodium hydroxide, adding p-toluenesulfonyl chloride, reducing p-toluenesulfonyl chloride into p-toluenesulfinate, and acquiringa p-toluenesulfinate aqueous solution; S2, adding azodicarbonamide into the p-toluenesulfinate aqueous solution obtained in the step S1, carrying out a reaction, and stopping the reaction when no gasis discharged; performing cooling, filtering, washing and drying to obtain the target product p-toluenesulfonamide urea. The production process of p-toluenesulfonamide urea is simple in steps and convenient for automatic continuous production; only water is used as a solvent, no organic solvent is used, and safety and environmental friendliness are achieved; the yield is high and reaches 95% or above, operation is easy, raw materials are easy to obtain, and the price is low; the process is a synthetic route suitable for large-scale automatic continuous production.

Description

technical field [0001] The invention relates to the field of chemical production technology, in particular to a production technology of p-toluenesulfonamidourea. Background technique [0002] P-toluenesulfonyl semicarbazide is a chemical substance with the molecular formula C8H11N3O3S. It is used as an additive for the foaming of polyvinyl chloride and other plastics and natural synthetic rubber. [0003] But, also there is following problem in the p-toluenesulfonamidourea production technique that is used at present: [0004] 1. The reaction efficiency is low, the degree of reaction is low, it is difficult to remove impurities, the yield is low, and the cost is high; [0005] 2. The synthesis process steps are relatively complicated, the amount of organic solvent is large, the pollution is serious, and the safety is poor; [0006] Therefore, it is not convenient for automatic continuous production. [0007] Based on the above situation, the present invention proposes a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/36C07C311/49C07C313/04
CPCC07C303/36C07C313/04C07C311/49
Inventor 朱建华李云霄李红
Owner 嘉兴市金利化工有限责任公司
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