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A kind of method of refining isophthalonitrile

A technology of isophthalonitrile and distillation kettle, which is applied in the purification/separation of carboxylic acid nitrile, organic chemistry and other directions, can solve the problems of difficulty in obtaining, high price and high energy consumption, and achieves reduction of content, improvement of yield, and improvement of products. quality effect

Active Publication Date: 2019-04-05
SHANGHAI XIAOMING DETECTION TECH SERVICE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic solvent used in this patent is mainly m-methylbenzonitrile, which is difficult to obtain and expensive
The process requires the use of a rectification column and a flash evaporator, and relatively high energy consumption

Method used

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  • A kind of method of refining isophthalonitrile
  • A kind of method of refining isophthalonitrile
  • A kind of method of refining isophthalonitrile

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A kind of method that is used for isophthalonitrile refining, its technological process is as figure 1 As shown, the isophthalonitrile crude product obtained by thin-wall trapping or water spray trapping is used as raw material, and the solid powdery raw material is added in still 1, and the heating of the still adopts heat transfer oil. The crude phthalonitrile is slowly melted from solid to liquid. After the temperature of the kettle is raised to 180°C, the vacuum is turned on, and the vacuum degree is raised to above 0.08MPa, and stirring is started. Continue heating until the temperature of the kettle reaches 210°C, and the product begins to evaporate, and the vacuum degree is increased to above 0.095MPa. When the temperature of the top of the kettle is raised to 250°C, turn off the vacuum, stop feeding the heat transfer oil, and cool down the distillation kettle. Regularly open the valve at the bottom of the still to discharge the distillation residue in the still....

Embodiment 2

[0028] A method for refining isophthalonitrile, using the crude isophthalonitrile obtained by thin-wall capture as a raw material, and introducing the solid powdery raw material into a still. In this embodiment, the still adopts a still-type The reactor is heated by heat conduction oil, and the temperature in the kettle is controlled at 170°C. The crude product is slowly melted from solid to liquid. After it is completely melted, the vacuum is turned on and the stirring is turned on, and the vacuum degree is increased to above 0.085MPa. Continue to heat until the temperature of the still reaches 206°C, and the product begins to evaporate, and the vacuum degree is increased to above 0.095MPa, continue to heat up, and stop when the temperature of the top of the still is 250°C, the raw materials are stirred in the still by propulsion, and the liquid in the still boils After that, isophthalonitrile turns into gas and is steamed out from the distillation tank. The distilled isophtha...

Embodiment 3

[0032] A method for refining isophthalonitrile, using the crude isophthalonitrile obtained by thin-wall capture as a raw material, and introducing the solid powdery raw material into a still. In this embodiment, the still adopts a still-type The reactor is heated by heat conduction oil, and the temperature in the kettle is controlled at 240°C. The crude product is slowly melted from solid to liquid. After it is completely melted, turn on the water flushing vacuum pump, control the vacuum degree of the reaction system to 0.08MPa, turn on stirring and continue to heat up, and distill Stop when the temperature at the top of the still is 260°C, the raw materials are stirred by anchor in the distillation kettle, after the liquid in the kettle boils, isophthalonitrile turns into gas and evaporates from the distillation kettle, and the distilled isophthalonitrile steam passes through the column The tubular heat exchanger is cooled to 180°C, and then introduced into the receiving kettl...

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Abstract

The invention relates to a method for refining isophthalonitrile. The method comprises the following steps: introducing an isophthalonitrile crude product raw material into a distillation kettle, cooling the distilled isophthalonitrile steam by a heat exchanger, introducing the isophthalonitrile into a receiving kettle, keeping the temperature, and finally, slicing by a slicer to obtain the refined isophthalonitrile finished product. Compared with the prior art, the method provided by the invention can enhance the isophthalonitrile content in the product and lower the meta-cyanobenzamide content, thereby reducing the hexachlorobenzene content in the chlorothalonil product and lowering the residue mass in the melter in the chlorothalonil production device.

Description

technical field [0001] The invention relates to the field of pesticide refining, in particular to a method for refining isophthalonitrile. Background technique [0002] Isophthalonitrile (IPN) is an important organic raw material for organic synthesis. Tetrachloroisophthalonitrile synthesized by chlorination is an efficient and low-toxic fungicide; m-xylylenediamine obtained by hydrogenation is a superior performance It is an excellent epoxy resin curing agent, and it is also a raw material for polyurethane resin and nylon resin. [0003] At present, the most important method of synthesizing isophthalonitrile is to obtain m-xylene with ammonia and oxygen under the action of catalyst through ammoxidation reaction. In the 1950s, Japan’s Showa Denko developed the production technology for the synthesis of isophthalonitrile in a fixed-bed ammoxidation of m-xylene. In the 1970s, Japan’s Mitsubishi Gas Co., Ltd. and the US Badger Company jointly developed a fine-particle catalyst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/34C07C255/51
CPCC07C253/34C07C255/51
Inventor 李强王海波田玫丽胡清禚文峰谢思勉田晓宏
Owner SHANGHAI XIAOMING DETECTION TECH SERVICE CO LTD
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