Method for producing N-butyl-phosphorothioic triamide n-(n-butyl)thiophosphoric triamide

A technology of n-butylthiophosphoric triamide and its production method, which is applied in the field of chemical fertilizer urease inhibitors, can solve the problems of non-compliance with environmental protection requirements, cumbersome operation steps, and large discharge of three wastes, and achieve low cost and high source of raw materials The effect of wide and no discharge of three wastes

Active Publication Date: 2009-08-12
NORTH HUAJIN CHEM IND GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The report of [Publication No. CN101337976A] uses excessive alkylamine as the acid-binding agent. During the whole process, it has been washed with water twice, extracted, and dried. The resulting product yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 1 mole of phosphorus trichloride and 4 moles of tetrahydrofuran into the reactor, start stirring (260 rpm), and then slowly add 1 mole of n-butylamine and 6 moles of triethylamine mixture, the temperature is controlled at- React at 15°C for 2 hours, then pass 2 moles of ammonia gas into the reactor, control the temperature at 0°C, and obtain a crude product after reacting for 7 hours. Then after centrifugal separation to remove the solid residue, the resulting liquid is subjected to vacuum distillation at 70° C., and finally the finished product N-n-butyl thiophosphoric triamide is obtained.

Embodiment 2

[0016] Add 1 mole of phosphorus trichloride and 8 moles of tetrahydrofuran to the reactor, start stirring (300 rpm), and then slowly add 1 mole of n-butylamine and 2 moles of triethylamine mixture, the temperature is controlled at- React at 10°C for 5 hours, then pass 5 moles of ammonia into the reactor, and the temperature is controlled at -15°C. After reacting for 5 hours, a crude product is obtained. After centrifugal separation to remove the solid residue, the resulting liquid is subjected to vacuum distillation at 80°C, and finally the finished product N-n-butyl thiophosphoric triamide is obtained.

Embodiment 3

[0018] Add 1 mole of phosphorous trichloride and 12 moles of tetrahydrofuran into the reactor, start stirring (350 rpm), and then slowly add 1.5 moles of n-butylamine and 5 moles of triethylamine mixture, the temperature is controlled at 0 ℃, react for 8 hours, then pass 8 moles of ammonia into the reactor, the temperature is controlled at 5 ℃, and react for 1 hour to obtain a crude product. After centrifugal separation to remove the solid residue, the resulting liquid is distilled under reduced pressure at 90° C., and finally the finished product N-n-butyl thiophosphoric triamide is obtained.

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PUM

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Abstract

The invention relates to a production method of N-normal-butyl thiophosphoryl triamine, comprising the following steps: dehydrating raw materials to control the water content to be within a required range, mixing phosphorus thiochloride with tetrahydrofuran, stirring the mixture, lowering the temperature, adding a mixture of n-butylamine, triethylamine and tetrahydrofuran in the mixture of the phosphorus thiochloride and the tetrahydrofuran by means of slow dripping, keeping a certain reaction temperature for 1-8h to obtain a white turbid liquid; leading ammonia gas into the a reaction system under the normal atmosphere, controlling the lead-in speed of ammonia gas, and keeping the temperature of the reaction system for 1-5h; centrifugating the reaction liquid to separate solid generated in the reaction system, distilling an obtained organic liquid in a decompression mode to remove most of the solvent and obtain a crude product, recrystallizing and refining the crude product to obtain a refined product with the purity higher than 99 percent. The invention has the advantages of wide raw material source, short process, simple operation, low cost, no three waste discharge, high economical benefit, applicability for industrial production, and the like.

Description

Technical field: [0001] The invention relates to a method for producing chemical fertilizer urease inhibitors, in particular to a method for producing N-butyl thiophosphoric triamide. Background technique: [0002] At present, domestic and foreign scholars' research on urease / nitrification inhibitors has focused on its inhibition of urea hydrolysis process and nitrification-denitrification process. From an agronomic sense, the beneficial effect of inhibitors is to ensure the effect of soil nitrogen on crops. Continue to supply and reduce its total loss. Studies have shown that the best inhibitory effects among inorganic compounds are silver salts and mercury salts. Among organic compounds, dihydric phenols and quinones, such as hydroquinone (HQ), catechol and p-benzoquinone, have the most inhibitory effects. In the past 10 years, domestic and foreign studies have shown that N-butyl thiophosphoric triamide is a highly effective urease inhibitor. N-Butylthiophosphoric triamide can ...

Claims

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Application Information

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IPC IPC(8): C07F9/22C05G3/08C05G3/90
Inventor 蓝云飞王益波范立成封文娟李耀波周秀芝刘万胜范铁军李淑文罗影李秀兰于德峰贺齐刘福德
Owner NORTH HUAJIN CHEM IND GRP
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