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Method for industrialized production of N-alkyl substituted phosphoric triamide

A phosphoric triamide and alkylamine technology, applied in chemical instruments and methods, phosphate fertilizers, agriculture, etc., can solve the problems of difficult product separation and harsh production process requirements, achieve a simple product refining process, reduce operational difficulties, The effect of high product purity

Inactive Publication Date: 2009-09-09
林文斌 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It mainly solves the technical problems existing in the existing synthesis methods, such as harsh production process requirements and difficult product separation due to the use of triethylamine as an acid-binding agent.

Method used

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  • Method for industrialized production of N-alkyl substituted phosphoric triamide
  • Method for industrialized production of N-alkyl substituted phosphoric triamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The production process in the No. 1 reactor:

[0021] Add 50Kg of PSCl in No. 1 reactor 3 , 384Kg CH 2 Cl 2 , stirred and cooled to 10°C, added dropwise 43.3Kg of n-butylamine, and controlled the rate of addition to keep the temperature of the reaction system at 10-12°C. After the dropwise addition was completed, the reaction system was heated under normal pressure and heated to reflux state, refluxed for 1 hour, cooled, added 50L of water to stir and extract, left to stand, the aqueous phase and the organic phase were separated, and the organic phase was dried by anhydrous sodium sulfate and then entered into 2 Standby in the No. reaction kettle.

[0022] The production process in the No. 2 reactor:

[0023] Under normal pressure, the reaction feed liquid in the No. 2 reactor was stirred and cooled to 10°C, 20.5Kg of ammonia gas was continuously introduced, the temperature of the reaction system was kept at 15-20°C, the stirring speed was 20rpm, and a large amount ...

Embodiment 2

[0031] The production process in the No. 1 reactor:

[0032] Add 50Kg of PSCl in No. 1 reactor 3 , 384Kg CH 2 Cl 2 , stirred and cooled to 10°C, added dropwise 62.7Kg of n-hexylamine, and controlled the rate of addition to keep the temperature of the reaction system at 10-12°C. After the dropwise addition is completed, the reaction system is heated under normal pressure and heated to reflux state, reflux reaction for 2 hours, cooled, added 50L of water to stir and extract, let stand, the water phase and the organic phase are separated, and the organic phase is dried by anhydrous calcium chloride and then enters Standby in No. 2 reactor.

[0033] The production process in the No. 2 reactor:

[0034] Under normal pressure, the reaction feed liquid in the No. 2 reactor was stirred and cooled to 10°C, 20.5Kg of ammonia gas was continuously introduced, the stirring speed was at 30rpm, the temperature of the reaction system was kept at 15-20°C, and a large amount of White NH 4...

Embodiment 3

[0042] The production process in the No. 1 reactor:

[0043] Add 50Kg of PSCl in No. 1 reactor 3 , 384Kg CH 2 Cl 2 , stirred and cooled to 10°C, added dropwise 45.3Kg of n-butylamine, and controlled the rate of addition to keep the temperature of the reaction system at 10-12°C. After the dropwise addition is completed, the reaction system is heated under normal pressure to reflux state, reflux reaction for 1 hour, cooled, add 50L of water to stir and extract, let stand, the water phase and the organic phase are separated, and the organic phase is dried by calcium oxide and enters the No. 2 reaction Reserve in the kettle.

[0044] The production process in the No. 2 reactor:

[0045] Under normal pressure, the reaction feed liquid in the No. 2 reactor was stirred and cooled to 10°C, 20.5Kg of ammonia gas was continuously introduced, the stirring speed was at 40rpm, the temperature of the reaction system was kept at 15-20°C, and a large amount of White NH 4 Cl solid. Ammo...

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Abstract

The invention relates to a preparation method of N-alkyl substituted phosphoric triamide, in particular to a method for industrialized production of the N-alkyl substituted phosphoric triamide. The preparation method mainly solves technical problems of the existing synthetic method such as severe production process requirements and great separation difficulty of products caused by taking triethylamine as an acid-binding agent and the like. The technical proposal of the invention is as follows: the method for industrialized production of the N-alkyl substituted phosphoric triamide comprises the following steps: allowing phosphorus chloride solution to react with excessive alkylamine, using up the excessive alkylamine as the acid-binding agent, and introducing ammonia gas to obtain the N-alkyl substituted phosphoric triamide. The N-alkyl substituted phosphoric triamide is an efficient urokinase inhibitor.

Description

technical field [0001] The invention relates to a preparation method of N-alkyl substituted phosphoric triamide, in particular to a method for industrialized production of N-alkyl substituted phosphoric triamide. Background technique [0002] N-Alkyl-substituted phosphoric triamides are highly effective urokinase inhibitors. At present, urea, which is the most widely used in the world, must be converted into ammonium carbamate through the enzymatic hydrolysis of urokinase in the soil, and absorbed by plants in the form of ammonium nitrogen. Due to the high activity of urokinase in the soil, the rate of converting urea to release ammonium nitrogen is very fast, and before the crops can absorb it, they will be volatilized and lost as ammonia nitrogen. Some of the ammonium nitrogen that is not absorbed by crops can also be converted into nitrate nitrogen, which will cause the deterioration of the atmosphere and soil environment through leaching and volatilization. N-alkyl sub...

Claims

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Application Information

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IPC IPC(8): C07F9/22C05B15/00
Inventor 林文斌高晓伟
Owner 林文斌
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