Continuous production method for N-NBPT

A technology of n-butyl thiophosphoric triamide and production method, which is applied in the field of continuous production of N-n-butyl thiophosphoric triamide, can solve the problems of low recovery rate, high odor of triethylamine and high production efficiency Low and other problems, to achieve the effect of mild reaction conditions, easy industrial production, and slow reaction speed

Inactive Publication Date: 2014-04-30
CANGZHOU JINCANG FINE CHEM CO LTD
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  • Abstract
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Problems solved by technology

However, this process also has the disadvantages of long reaction time, strong triethylamine odor, low recovery rate, difficulty in post-treatment separation and purification, cumbersome operation steps and the need for pressurization when passing ammonia.
Chinese patent CN101503424 discloses a method for preparing N-n-butylthiophosphoric triamide by one-pot method, which also uses tetrahydrofuran as a solvent, triethylamine as an acid-binding agent, and reacts with ammonia under normal pressure, but there is still a reaction time Long, centrifuged separation reaction by-products of solid ammonium chloride, tetrahydrofuran and triethylamine loss and other issues
Chinese patent CN101759717 also uses triethylamine as an acid-binding agent and chloroform as a solvent. After passing through the

Method used

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  • Continuous production method for N-NBPT

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Experimental program
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Effect test

Embodiment 1

[0031] (1) Add 225 grams (1.33 moles) of phosphorus trichloride and 1360 grams (16.0 moles) of dichloromethane into a four-necked flask, stir and cool to -5°C, add 100 grams (1.37 moles) of n-butylamine and 50 G (0.58 mol) of methylene chloride was mixed uniformly and alternately added dropwise with 100 g (1.32 mol) of concentrated ammonia water to the above solution, keeping at -5°C. After the addition is complete, keep it at -5°C for 2 hours and the reaction is over.

[0032] (2) The reaction solution obtained in step (1) is filtered and separated into layers, and the lower organic phase is reacted with 5.32 moles of ammonia gas at 10° C., the reaction is terminated when the pH is greater than 8.5, and centrifugal filtration is performed.

[0033] (3) Concentrate the obtained liquid phase to 40% for cooling and crystallization. The product after centrifugation is 152 grams, with a content of 97.2%. Then 152 grams of product was added to 300 grams of dichloromethane to dissolve a...

Embodiment 2

[0035] Add 450 grams (2.66 moles) of phosphorus trichloride and 1130 grams (13.3 moles) of dichloromethane to a four-necked flask, stir and cool to -10°C, mix 200 grams (2.74 moles) of n-butylamine and 1000 grams (11.7 moles) of n-butylamine. Mol) dichloromethane is mixed uniformly and added dropwise to the above solution with 210 grams (2.75 moles) of concentrated ammonia water at the same time, keeping it at 0°C, after the dropwise addition is complete, keep it at 5°C for 3 hours and the reaction is over.

[0036] (2) The reaction solution obtained in step (1) is filtered and separated into layers, and the lower organic phase is reacted with 10.2 moles of ammonia gas at 25°C, and the reaction is terminated when the pH is greater than 9, and centrifugal filtration is performed.

[0037] (3) Concentrate the obtained liquid phase to about 50% for cooling and crystallization. The product after centrifugation is 315 grams, with a content of 97.2%. Then add 315 grams of product to 600 ...

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Abstract

The invention relates to a production method for chemical fertilizer urease inhibitors, in particular to a continuous production method for N-NBPT. The continuous production method comprises the following steps: mixing thiophosphoryl chloride and dichloromethane for stirring; cooling; then dropwise adding a mixed solution of n-butylamine and dichloromethane, and acid bounded reaction agents simultaneously; preserving heat for 0.5-6 hours after dropwise adding to obtain a reaction solution, wherein the acid bounded reaction agents are ammonium hydroxides or ammonia gases; filtering and layering the obtained reaction solution; introducing the ammonia gases into the underlayer reaction solution for an ammonolysis reaction; centrifuging, filtering and concentrating the reaction solution obtained after the ammonolysis reaction; recrystallizing to obtain the product. According to the invention, other auxiliary raw materials are not needed except for raw materials used for producing the product; the continuous production method needs no purification in the tremendously optimized reaction process, has a mild reaction condition and no other by-products, and has the advantages of high production efficiency, mild reaction condition, high yield, good quality, less three wastes, fully utilized resources and the like.

Description

Technical field [0001] The invention relates to a method for producing a chemical fertilizer urease inhibitor, in particular to a method for continuous production of N-butyl thiophosphoric triamide. Background technique [0002] N-Butylthiophosphoric triamide is one of the effective soil urease inhibitors in agriculture, and it can be formulated with urea in a certain proportion of compound fertilizer. On the one hand, it can inhibit the activity of urease, slow down the hydrolysis rate of urea, make urea easily absorbed by plants, and greatly improve the utilization rate of urea. On the other hand, it can also provide phosphorus, sulfur, nitrogen and other elements to improve the soil. U.S. Patent No. 4,530,714, Chinese Patent No. CN101370753, etc. have reported the application of N-butyl thiophosphoric triamide as a urease inhibitor in urea and urea-based compound fertilizers. [0003] N-Butylthiophosphoric triamide mainly has the following synthetic methods: [0004] (1) Two-st...

Claims

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Application Information

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IPC IPC(8): C07F9/22
Inventor 王志浩于亦忠徐栋于亦涛李宗
Owner CANGZHOU JINCANG FINE CHEM CO LTD
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