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Microchannel synthesis technology for N-(n-Butyl)thiophosphoric triamide

A technology of n-butyl thiophosphoric triamide and synthesis technology, which is applied in the field of micro-channel synthesis technology of n-butyl thiophosphoric triamide, can solve the difficulty of separation and purification, serious back-mixing of materials and long reaction time and other problems, to achieve the effect of improving the total yield and purity, less three wastes, and short reaction time

Inactive Publication Date: 2015-02-25
ZHEJIANG AOFUTUO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using triethylamine or excess n-butylamine as an acid-binding agent has many by-products, and it is difficult to separate and purify, and most of these processes require separation in the middle, the reaction time is long, the material backmixing is serious, there are many impurities, and the energy consumption is high. , low yield, serious environmental pollution

Method used

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  • Microchannel synthesis technology for N-(n-Butyl)thiophosphoric triamide
  • Microchannel synthesis technology for N-(n-Butyl)thiophosphoric triamide

Examples

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Effect test

Embodiment 1

[0024] In this embodiment, 3.39kg (2.0mol) of phosphorus trichloride and 1.695kg of dichloromethane are mixed, and 1.465kg (2.0mol) of n-butylamine is added to 1.465kg of dichloromethane and injected into the Corning microchannel simultaneously with a plunger metering pump respectively. Reactor feed port, the other feed port injects 10% NaOH solution 8kg (2mol) with metering plunger pump, adjusts the back pressure valve to 0MPa, controls and adjusts the material entering speed, uses up above-mentioned three kinds of materials evenly at the same time, temperature control At 10 °C, the reaction time is 20 s. When the material enters the third plate, it is cooled to 15°C, and the fourth plate is fed with NH at 15°C 3 14.96kg (8.8mol), the material is received at the outlet, the material is separated from the gas and liquid, and the inorganic layer is separated at rest. After the organic layer is evaporated to part of the dichloromethane, it is cooled and crystallized, filtered to...

Embodiment 2

[0027] In this embodiment, 3.39kg (2.0mol) of phosphorus trichloride and 3.39kg of dichloromethane are mixed, and 1.465kg (2.0mol) of n-butylamine is added to 2.93kg of dichloromethane and injected into the Corning microchannel simultaneously with a plunger metering pump respectively. Reactor feed port, another feed port injects 10% NaOH solution 8kg (2.0mol) with metering plunger pump, adjusts the back pressure valve to be 0.25MPa, controls and regulates the feed rate of material, uses up above-mentioned three kinds of materials evenly simultaneously, The temperature was controlled at 50°C, and the reaction time was 25s. When the material enters the third plate, it is cooled to 15°C, and the fourth plate is fed with NH at 15°C3 14.96kg (8.8mol), the material is received at the outlet, the material is separated from the gas and liquid, and the inorganic layer is separated at rest. After the organic layer is evaporated to part of the dichloromethane, it is cooled and crystallize...

Embodiment 3

[0030] In this embodiment, 3.39kg (2.0mol) of phosphorus trichloride and 2.712kg of dichloromethane are mixed, and 1.465kg (2.0mol) of n-butylamine is added to 2.637kg of dichloromethane and injected into the Corning microchannel simultaneously with a plunger metering pump respectively. Reactor feed port, another feed port injects 10% NaOH solution 8kg (2.0mol) with metering plunger pump, adjusts the back pressure valve to be 0.5MPa, controls and regulates the feed rate of material, evenly uses up above-mentioned three kinds of materials simultaneously, The temperature was controlled at 25°C, and the reaction time was 30s. When the material enters the third plate, it is cooled to 15°C, and the fourth plate is fed with NH at 15°C 3 14.96kg (8.8mol), the material is received at the outlet, the material is separated by gas and liquid, and the inorganic layer is separated at rest. After the organic layer is evaporated to part of the dichloromethane, it is cooled and crystallized, ...

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Abstract

The invention discloses a microchannel synthesis technology for N-(n-Butyl)thiophosphoric triamide. The microchannel synthesis technology comprises the following steps: evenly mixing thiophosphoryl chloride and dichloromethane as well as n-butyl amine and dichloromethane, respectively injecting the two mixtures in a feed inlet of a Corning microchannel reactor simultaneously by a metering plunger pump, injecting 10% NaOH solution into another feed inlet through a metering plunger pump, regulating the value of a back pressure valve, controlling the reaction time of materials, evenly using up the three materials, reacting through four modules, receiving the materials at an outlet, performing gas-liquid separation to the materials, standing and separating an inorganic layer, evaporating a part of dichloromethane from an organic layer, cooling and crystalizing, and filtering to obtain NBPT products. The microchannel synthesis technology has the characteristics of being simple and convenient to operate, fewer in side products, low in energy consumption, high in yield, low in cost and suitable for continuous industrial production.

Description

technical field [0001] The invention relates to a microchannel synthesis process of n-butylthiophosphoric triamide. Background technique [0002] Nitrogen, phosphorus and potassium are the three most important elements in agricultural production, among which nitrogen is the most important. In the 1980s, with the widespread use of chemical fertilizers, grain production has generally increased. According to the estimates of the Food and Agriculture Organization of the United Nations, 55% of the increase in food production in developing countries comes from the role of chemical fertilizers. Urea is the most important nitrogen fertilizer, accounting for about 60%-70% of the total nitrogen fertilizer in my country, but the utilization rate of urea by crops is usually very low. In farmland, the utilization rate of urea is usually only 30%-35%. Urea is rapidly hydrolyzed into NH under the action of urease in soil 4 + , at this time, part of the gaseous NH 3 has escaped from t...

Claims

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Application Information

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IPC IPC(8): C07F9/22C05G3/90
CPCY02P20/10
Inventor 戴锋戴稼本戴舒天戴亦能
Owner ZHEJIANG AOFUTUO CHEM
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