Preparation method of tetrachloro-terephthalonitrile with low hexachlorobenzene content

A technology of tetrachloroterephthalonitrile and terephthalonitrile, which is applied in the field of preparation of chemical intermediate tetrachloroterephthalonitrile, can solve the problems of unfavorable environmental protection, many intermediate products, and many wastes, and achieve The process and operation are practical, the steps are simple, and the chlorine flow is reasonable.

Inactive Publication Date: 2018-04-20
JIANGSU WEUNITE FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is a four-step reaction, which adopts batch production, and there are many reaction intermediate products. At the same time, a large amount of acid-containing wastewater is generated and a large amount of solvent is used in the preparation process, so there are many three wastes in the production process, which is not conducive to environmental protection.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Put the metered amount of terephthalonitrile into the vaporizer for vaporization. After the vaporization of isophthalonitrile, it is taken out of the vaporizer by nitrogen gas and mixed with chlorine gas, and then enters the fluidized bed and fixed bed equipped with special chlorination catalyst in turn. react. The molar ratio of the intake air is isophthalonitrile: nitrogen: chlorine = 1:6:4.2, the reaction temperature of the fluidized bed and the fixed bed are respectively controlled at 310°C and 342°C, and the pressure is 0.003MP. After the reaction, the reaction The mixed gas is sent to the receiver, and tetrachloroterephthalonitrile is obtained after condensing and drying, with a yield of 95.3%, a content of 99.2%, and HCB of 15.2ppm.

Embodiment 2

[0015] Put the measured amount of terephthalonitrile into the vaporizer for vaporization. After the terephthalonitrile is vaporized, it will be taken out of the vaporizer by nitrogen gas and mixed with chlorine gas, and then enter the fluidized bed and fixed bed equipped with special chlorination catalysts. react. The molar ratio of the intake air is isophthalonitrile: nitrogen: chlorine = 1:7:5, the reaction temperature of the fluidized bed and the fixed bed are respectively controlled at 320°C and 345°C, and the pressure is 0.004MP. After the reaction, the reaction The mixed gas is sent to the receiver, and tetrachloroterephthalonitrile is obtained after condensing and drying, with a yield of 96.2%, a content of 99.5%, and HCB of 12 ppm.

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PUM

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Abstract

The invention discloses a preparation method of tetrachloro-terephthalonitrile with low hexachlorobenzene content. The preparation method comprises the following steps: putting metered para-phthalonitrile into a vaporizer, performing vaporization, taking m-phthalonitrile out of the vaporizer along with nitrogen after vaporizing the m-phthalonitrile, mixing the m-phthalonitrile and chlorine duringmixing, and sequentially entering a fluidized bed and a fixed bed with special chlorination catalysts to perform reaction. The molar ratio of the gas inlet quantities of the para-phthalonitrile to thenitrogen to the chlorine is equal to 1:(6-7):(4-5), the reaction temperature of the fluidized bed and the reaction temperature of the fixed bed are controlled to be 300 to 320 DEG C and 340 to 350 DEG C correspondingly, the pressure is controlled to be 0.002 to 0.005 MPa, the reaction mixed gas is fed into a material receiver after the reaction, and condensation drying is conducted to obtain thetetrachloro-terephthalonitrile with low hexachlorobenzene content.

Description

technical field [0001] The invention belongs to the technical field of chemical production and relates to a preparation method of a chemical intermediate tetrachloroterephthalonitrile. Background technique [0002] Tetrafluoroterephthalonitrile is an important organic intermediate with a white powder appearance, which is further synthesized into tetrafluoroterephthalonitrile by fluorination, and tetrafluoroterephthalonitrile is an important fluorine-containing Aromatic chemical intermediates, widely used in the synthesis of medicines, pesticides, dyes and fluoropolymers. Using them to synthesize pesticides has strong selectivity, less usage, low toxicity to humans, and low residues. It has broad development prospects, high value, and good market prospects. Thereby tetrachloroterephthalonitrile as the raw material for producing tetrafluoroterephthalonitrile has received extensive attention for a long time. [0003] CN200610038423.8 discloses a kind of method of industrializ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/51
CPCC07C253/30C07C255/51
Inventor 蒙健张松林
Owner JIANGSU WEUNITE FINE CHEM CO LTD
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