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Method for continuously synthesizing N-butylthiophosphoric triamide by microreactors

A technology of n-butyl thiophosphoric triamide and microreactor, applied in the field of chemical technology, can solve the problems of difficulty in separation and purification, long reaction time, many by-products, etc., and achieves shortened production cycle, short processing flow, The effect of less by-products

Inactive Publication Date: 2018-05-29
NORTH HUAJIN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But above-mentioned two kinds of methods all adopt triethylamine or excessive n-butylamine as acid-binding agent, there are many by-products, separation and purification have certain difficulty, and most of these processes need to be separated in the middle, the reaction time is long, and material back-mixing is serious, Many impurities, high energy consumption, low yield, serious environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of microreactor method continuously synthesizes the device of n-butyl thiophosphoric triamide, comprises the following steps:

[0021] (1) Fully mix n-butylamine and dichloromethane, as the first component, fully mix phosphorus trichloride and dichloromethane, as the second component, mix the first component and the second component Feed advection pump into the membrane dispersion microreactor for reaction, and at the same time feed ammonia gas through the gas distributor, the metal sintered membrane pore diameter of the membrane dispersion microreactor is 5 μm, the reaction residence time is 20s, and the reaction temperature is 23°C. Obtain N-thiophosphoryl dichloride ammonium chloride;

[0022] (2) The above-mentioned product is passed into the tubular microreactor, and ammonia gas is continuously introduced through the gas distributor to react at the same time. The pipe diameter of the tubular microreactor is 10mm, the length of the pipe is 5m, the residence t...

Embodiment 2

[0025] A kind of microreactor method continuously synthesizes the device of n-butyl thiophosphoric triamide, comprises the following steps:

[0026] (1) Fully mix n-butylamine and dichloromethane, as the first component, fully mix phosphorus trichloride and dichloromethane, as the second component, mix the first component and the second component The feed advection pump is fed into the membrane dispersion microreactor for reaction, and ammonia gas is introduced through the gas distributor at the same time. The metal sintered membrane pore size of the membrane dispersion microreactor is 8μm, the reaction residence time is 18s, and the reaction temperature is 23°C. Obtain N-thiophosphoryl dichloride ammonium chloride;

[0027] (2) The above-mentioned product is passed into the tubular microreactor, and ammonia gas is continuously introduced through the gas distributor to react at the same time. The pipe diameter of the tubular microreactor is 10mm, the length of the pipe is 5m, ...

Embodiment 3

[0030] A kind of microreactor method continuously synthesizes the device of n-butyl thiophosphoric triamide, comprises the following steps:

[0031] (1) Fully mix n-butylamine and chloroform, as the first component, fully mix the phosphorus trichloride and chloroform, as the second component, pass the first component and the second component through the feed advection The pump is input into the membrane dispersion microreactor for reaction, and ammonia gas is introduced through the gas distributor at the same time. The metal sintered membrane pore diameter of the membrane dispersion microreactor is 8 μm, the reaction residence time is 18s, and the reaction temperature is 23 ° C to obtain N-sulfur Phosphoryl dichloride ammonium chloride;

[0032] (2) The above-mentioned product is passed into the tubular microreactor, and ammonia gas is continuously introduced through the gas distributor to react at the same time. The pipe diameter of the tubular microreactor is 10mm, the lengt...

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Abstract

The invention discloses a method for preparing N-butylthiophosphoric triamide by continuous reaction in microreactors. The method comprises the following steps: uniformly mixing n-butylamine and triophosphoryl chloride with a solvent respectively at first, then adding a mixture into a membrane dispersion microreactor through a charging pump, dispersing the n-butylamine into a mixture solution of the triophosphoryl chloride in a micro-droplet form, performing reaction at certain temperature to obtain N-butylthiophosphoric dichloride, and simultaneously introducing ammonia as an acid binding agent of hydrogen chloride; delivering the reactant to a tubular microreactor, and continuously introducing ammonia into the reactor through a gas distributor to obtain the N-butylthiophosphoric triamideand ammonium chloride; finally collecting a product through a collection kettle, and executing operations of crystallization, filtering, drying and the like to obtain a product. The method has the advantages of short processing flow, mild reaction condition, simplicity for process operation, few byproducts, low energy consumption, high yield, low cost and the like, and is suitable for large-scaleindustrial production.

Description

technical field [0001] The invention belongs to the field of chemical process methods, and in particular relates to a method for continuously synthesizing N-n-butylthiophosphoric triamide using a microreactor. Background technique [0002] N-n-butylthiophosphoric triamide (NBPT) is a highly effective soil urease inhibitor, it has excellent urease inhibitory effect, can significantly reduce the decomposition of urea in the soil, and increase the nitrogen utilization rate of crops . Its inhibition mechanism is to compete for ligands and reduce urease activity. The nitrogen atom in the NBPT molecule forms a (N-Ni) ligand with the nickel atom in the urease, and the amino compound in the molecule can also be combined with the oxygen in the carbamate bridge. Atoms form a tridentate ligand, which is stronger than the monodentate ligand formed by urea and urease, thereby reducing the contact between urea and urease, slowing down the hydrolysis rate of urea, and improving the utiliz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/22B01J19/00
Inventor 魏丽娟王益波周川李耀波刘万胜赵欣麟罗闯佟小倩李秀兰李淑文罗颖范铁军于德峰王玉凤初小丽
Owner NORTH HUAJIN CHEM IND CO LTD
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