Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Continuous preparation method and preparation device of N-n-butyl thiophosphoric triamide

A technology of n-butyl thiophosphoric triamide and n-butyl dichlorothiophosphoric amide, which is applied in the field of continuous preparation methods and preparation devices of N-n-butyl thiophosphoric triamide, and can solve the problem of unsuitable Industrialized production, long reaction time, and high production cost have the effect of shortening production cycle, improving process safety, and facilitating recycling and application.

Active Publication Date: 2020-04-03
武威金仓生物科技有限公司
View PDF15 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of long reaction time, high production cost, unsuitability for industrialized production, and potential environmental protection hazards in the existing N-n-butylthiophosphoric triamide synthesis technology, the present invention proposes an N-n-butyl thiophosphoric triamide synthesis technology. Continuous preparation method and preparation device of phosphoric acid triamide

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Continuous preparation method and preparation device of N-n-butyl thiophosphoric triamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Under the protection of nitrogen, add 120kg (708.3mol, 1eq) phosphorus trichloride and 1000kg toluene in batching kettle 1, obtain the toluene solution of phosphorus trichloride after mixing uniformly. With two calibrated first liquid metering pumps 4 respectively, phosphorus trichloride toluene solution and 57kg (779mol, 1.1eq) n-butylamine are injected in the microchannel reactor 5, wherein, the progress of phosphorus trichloride toluene solution The sampling speed is 37ml / min, and the sampling speed of n-butylamine is 2.56ml / min. The mixed reaction liquid enters the microchannel reactor 5 with an inner diameter of 5 mm and a total length of 3 m at a speed of 1.8 m / min. The temperature of the microchannel reactor is controlled to be 25° C. and the reaction residence time is 100 s. The obtained N-n-butyldichlorothiophosphoramide toluene solution is treated with anion exchange resin 7 and then enters storage tank 8 for direct use in the next step of reaction.

[0041]T...

Embodiment 2

[0045] Under the protection of nitrogen, add 120kg (708.3mol, 1eq) phosphorus trichloride and 1000kg toluene in batching kettle 1, obtain the toluene solution of phosphorus trichloride after mixing uniformly. With two calibrated first liquid metering pumps 4 respectively, phosphorus trichloride toluene solution and 57kg (779mol, 1.1eq) n-butylamine are injected in the microchannel reactor 5, wherein, the progress of phosphorus trichloride toluene solution The sampling speed is 37ml / min, and the sampling speed of n-butylamine is 2.56ml / min. The mixed reaction liquid enters the microchannel reactor 5 with an inner diameter of 5 mm and a total length of 3 m at a speed of 1.8 m / min. The temperature of the microchannel reactor is controlled to be 25° C. and the reaction residence time is 120 s. The obtained N-n-butyldichlorothiophosphoramide toluene solution is treated with anion exchange resin 7 and then enters storage tank 8 for direct use in the next step of reaction.

[0046] ...

Embodiment 3

[0049] Under the protection of nitrogen, add 120kg (708.3mol, 1eq) phosphorus trichloride and 1000kg toluene in batching kettle 1, obtain the toluene solution of phosphorus trichloride after mixing uniformly. With two calibrated first liquid metering pumps 4 respectively, phosphorus trichloride toluene solution and 57kg (779mol, 1.1eq) n-butylamine are injected in the microchannel reactor 5, wherein, the progress of phosphorus trichloride toluene solution The sampling speed is 37ml / min, and the sampling speed of n-butylamine is 2.56ml / min. The mixed reaction liquid enters the microchannel reactor 5 with an inner diameter of 5 mm and a total length of 3 m at a speed of 1.8 m / min. The temperature of the microchannel reactor is controlled to be 20° C. and the reaction residence time is 100 s. The obtained N-n-butyldichlorothiophosphoramide toluene solution is treated with anion exchange resin 7 and then enters storage tank 8 for direct use in the next step of reaction.

[0050] ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a continuous preparation method and a preparation device of N-n-butyl thiophosphoric triamide. The preparation method comprises the following steps: (1) adding a thiophosphoryl chloride toluene solution and n-butylamine into a micro-channel reactor for substitution reaction to obtain an N-n-butyl dichloro thioxophosphamide toluene solution, treating the N-n-butyl dichlorothioxophosphamide toluene solution with an anion exchange resin, and feeding the treated N-n-butyl dichloro thioxophosphamide toluene solution into a storage tank; (2) adding the solution in the storage tank and ammonia gas into a tubular reactor for reaction to obtain an N-n-butyl thiophosphoric triamide toluene solution; and (3) carrying out extraction washing, organic phase concentration recrystallization, separation and drying on the obtained solution to obtain the high-purity N-n-butyl thiophosphoric triamide. According to the continuous preparation method and the preparation device disclosed by the invention, the continuity of the production process of the N-n-butyl thiophosphoric triamide is realized, the defect of intermittent operation of a kettle type reactor is avoided, the process is simplified, the reaction selectivity is improved, and the purposes of clean production, shortening of the production period and reduction of the production cost are achieved.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a continuous preparation method and a preparation device of N-n-butylthiophosphoric triamide. Background technique [0002] N-n-butylthiophosphoric triamide is currently one of the most effective soil urease inhibitors. It has outstanding advantages such as high efficiency, non-toxicity, and no side effects. It is usually used as an effective component of compound fertilizers. [0003] CN101337976A has reported a kind of method of N-n-butyl thiophosphoric acid triamide, adopts phosphorus trichloride and n-butylamine to react and separates intermediate N-n-butyl dichlorothiophosphoric amide, through purified N- After reacting n-butyl dichlorothiophosphoramide with ammonia gas, N-n-butylthiophosphoric triamide can be obtained. However, the process is cumbersome, involves high temperature and low temperature reaction requirements, poor reaction selectivity, long production cycle, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07F9/22
CPCC07F9/224
Inventor 于亦忠高于王志浩国洪雷施裕华
Owner 武威金仓生物科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com