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Continuous production process of N-normal-butyl thiophosphoryl triamide

A technology for n-butyl thiophosphoric triamide and production process is applied in the field of continuous production technology of urease inhibitor N-n-butyl thiophosphoric triamide, and can solve the problems of high cost, large pollution and complicated process and other problems, to achieve the effects of low production cost, less side reactions, and increased reaction temperature

Active Publication Date: 2014-01-22
江西吉翔医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the shortcomings of the existing N-n-butylthiophosphoric triamide preparation technology, such as complex process, high cost, and large pollution, the present invention provides a green craft

Method used

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  • Continuous production process of N-normal-butyl thiophosphoryl triamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Mix 10.20kg (60.18mol) of phosphorus trichloride and 30L of chlorobenzene to form component A, and mix 4.50kg (61.64mol) of n-butylamine and 11.40kg (61.62mol) of tri-n-butylamine and 30L of chlorobenzene to form component A. Part B. Transport components A and B to the Y-type jet mixer respectively, and enter the first tubular reactor after mixing. The reaction temperature is controlled at 35°C, and the residence time is 80s. After the reaction, the reaction liquid enters the preheated to 60°C In the pipeline, the preheated reaction solution enters the second tubular reactor, and 6.7kg of ammonia gas (394mol) is continuously introduced, and the reaction temperature is controlled to be 70°C, and the residence time is 1200s. After the reaction, the reaction solution is added to cold water to fully Stir and mix, enter the layered kettle, and let it stand for layering. The organic layer was washed once with water, chlorobenzene was recovered by vacuum distillation, the rec...

Embodiment 2

[0028] Mix 10.20kg (60.18mol) of phosphorus trichloride with 26L of o-dichlorobenzene to form component A, 4.46kg (61.09mol) of n-butylamine, 6.94kg (61.42mol) of N-ethylpiperidine and 30L of o-dichlorobenzene Chlorobenzene mixed evenly is component B. Transport components A and B to the Y-type jet mixer respectively, and enter the first tubular reactor after mixing. The reaction temperature is controlled at 40°C, and the residence time is 60s. After the reaction, the reaction liquid enters the preheated to 60°C In the pipeline, the preheated reaction solution enters the second tubular reactor, and 6.5kg of ammonia gas (382mol) is continuously introduced, and the reaction temperature is controlled to be 75°C, and the residence time is 900s. After the reaction is completed, the reaction solution is added to cold water to fully Stir and mix, enter the layered kettle, and let it stand for layering. The organic layer was washed once with water, and N-ethylpiperidine was recovered...

Embodiment 3

[0032] Mix 10.20kg (60.18mol) of phosphorus trichloride and 32L of diethyl carbonate to form component A, 4.35kg (59.59mol) of n-butylamine, 8.12kg (60.15mol) of N,N-dimethylbenzylamine and Mix 24L of diethyl carbonate evenly to form component B. Transport components A and B to the Y-type jet mixer respectively, and enter the first tubular reactor after mixing. The reaction temperature is controlled at 25°C, and the residence time is 180s. After the reaction, the reaction liquid enters the preheated to 60°C In the pipeline, the preheated reaction solution enters the second tubular reactor, continuously feeds 6.8kg of ammonia (400mol), controls the reaction temperature to be 70°C, and has a residence time of 1000s. After the reaction, the reaction solution is added to cold water to fully Stir and mix, enter the layered kettle, and let it stand for layering. The organic layer was washed once with water, diethyl carbonate was recovered by distillation under reduced pressure, the...

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Abstract

The invention discloses a continuous production process of N-normal-butyl thiophosphoryl triamide. Mixture of thiophosphoryl chloride and organic solvent and mixture of n-butyl amine, tertiary amine acid-binding agent and organic solvent are respectively input in a Y-type jet flow mixing device to be rapidly mixed, then the mixture enters a first tubular reactor and an amination reaction is conducted, an obtained reaction solution is pre-heated, and enters a second tubular reactor, ammonia gas is added, the amination reaction is conducted, and finally the N-normal-butyl thiophosphoryl triamide is obtained through separation and purification. According to the continuous production process of the N-normal-butyl thiophosphoryl triamide, proper solvent and acid-binding agent are selected, proper reaction temperature is selected, and therefore the purpose that the amination reaction is continuously conducted in a pipeline without added pressure is achieved. The continuous production process of the N-normal-butyl thiophosphoryl triamide has the advantages that production efficiency is high, reaction condition can be controlled easily, yield is high, quality is high, discharge amount of the three wastes is small, resources are sufficiently used, and the continuous production process of the N-normal-butyl thiophosphoryl triamide is suitable for large-scale industrialized production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a continuous production process of N-n-butylthiophosphoric triamide, a urease inhibitor. Background technique [0002] N-butylthiophosphoric triamide is one of the effective soil urease inhibitors in agriculture. It can be formulated with urea in a certain proportion to make compound fertilizers. On the one hand, it can inhibit the activity of urease in the soil and slow down the hydrolysis of urea. speed, thereby increasing the utilization rate of urea and enhancing fertilizer efficiency; on the other hand, it can also provide sulfur, phosphorus and other elements to play a better role in soil improvement. US Patent US 4530714, Chinese Patent CN 101370753, etc. all disclose the application of N-n-butylthiophosphoric triamide as a urease inhibitor in urea and urea-based compound fertilizers. Chinese patent CN 101505806 also discloses other uses of N-n-butylthiophosphori...

Claims

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Application Information

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IPC IPC(8): C07F9/22C01C1/16
Inventor 郑土才杨泽慧冯晓根聂孝文况庆雷郑建霖魏源王吉陈锋王吉
Owner 江西吉翔医药化工有限公司
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