A clean production process for preparing n-n-butylthiophosphoric triamide

Abstract

The invention relates to a clean production process for preparing N-n-butyl thiophosphoric triamide, which mainly includes substitution, ammoniation, temperature return, filtration, desolventization and product purification processes, and N-n-butyl thiophosphoric triamide The organic solvent and ammonia produced in the production process of amide have been recycled, and ammonium chloride is a kind of chemical fertilizer raw material, which can be used in the production of chemical fertilizer. The process of the invention reduces production cost and reduces environmental pollution, and is a clean production process of N-n-butylthiophosphoric triamide with high yield, excellent product quality and no pollution.

Description

field of invention [0001] The invention relates to a clean production process for preparing N-n-butylthiophosphoric triamide, in particular to an industrialized clean production process for N-n-butylthiophosphoric triamide. Background technique [0002] N-n-butylthiophosphoric triamide is a highly effective urokinase inhibitor. 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 conversion of urea to release amine nitrogen is very fast. Before the crops can absorb it, they will be lost as ammonium nitrogen volatilization. Part of the ammonium nitrogen 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-n-butyl thiophosphoric triamid...

AI Technical Summary

Problems solved by technology

Using triethylamine alone as the acid-binding agent, the triethylamine hydrochloride generated has very little solubility in organic solvents, and the solution supersaturation is large, which makes the nucleation rate too fast, produces a large number of tiny crystals, and the crystals are difficult to grow up, and It is easy to produce crystal scale, and the fine crystal particles and crystal scale are easy to form agglomerates, which increases the difficulty of separation

[0005] WO2010045895, CN101337976, CN101525348, etc. disclose the reaction of alkyl primary amines with phosphorothion trichloride to obtain hydrocarbyl aminothiophosphoryl dichloride, and then feed ammonia gas to obtain hydrocarbyl thiophosphoryl triamide. No other Acid-binding agent, the raw material hydrocarbyl primary amine acts as an acid-binding agent and a reactant, which increases the amount of raw materials used, and there are many by-products, which cause certain difficulties in the separation and purification of the final product

[0006] CN101981040 discloses a method for preparing triamides from ammonia and amino dichloride. Although it is mentioned that liquid ammonia or ammonia gas can be used as a reactant, a special reactor is required in this method to ensure that the reaction is carried out in a non-backmixing manner , and it is necessary to ensure that the dichloride concentration is below a certain range, so the cost is high, which limits the large-scale industrial production of this method

[0007] At present, there are still shortcomings such as low production efficiency, long reaction time, high cost, serious waste, and difficult separation in various processes for producing N-n-butylthiophosphoric triamide. The clean production process of phosphoric acid triamide is easy to purify, reduces production cost, reduces environmental pollution, and has important industrial value

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