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A kind of environmental protection processing method of hexachlorobenzene

An environmental protection treatment, hexachlorobenzene technology, applied in the direction of halogen substitution preparation, organic chemistry, etc., can solve the problems of short process route, difficult degradation, low yield, etc., achieve low reaction risk factor, avoid environmental pollution, and improve raw material conversion rate high effect

Active Publication Date: 2017-12-22
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hexachlorobenzene has a completely symmetrical structure, and has a large number of chlorine substitutions, high toxicity, and very difficult to degrade
According to the survey, at least 600 tons of hexachlorobenzene are produced in the domestic chemical production process every year, and the sealed hexachlorobenzene waste has the risk of leakage and diffusion, which poses a huge hidden danger to the safety of the surrounding ecological environment
Hexachlorobenzene is usually disposed of by simple incineration, which may produce dioxins during the incineration process, causing great harm to the environment
[0014] This method has a short process route and low cost of raw materials, but it also has low yield and serious coking in the reactor, which limits the industrial application
[0015] In summary, the existing synthetic methods of hexafluorobenzene and chloropentafluorobenzene have the disadvantages of low conversion rate, low yield, serious coking in the reactor, and being unfavorable for industrialized production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 200 g of hexachlorobenzene and 408 g of highly active potassium fluoride into a single reactor, and then add 2000 g of dried organic solvent tri-n-butylamine. After the addition, test the pressure of the single reactor for leak detection and nitrogen replacement. Then start stirring, and slowly raise the temperature to the reaction temperature of 280° C., and react at a constant temperature for 15 hours. The pressure of the single reactor rises to the reaction pressure of 2.0-3.0 Mpa. As the reaction progresses, the reaction pressure gradually increases. Stop heating after the reaction is over, lower the temperature to 130°C, open the valve of the single reactor, and steam the reaction products in the single reactor to condense and collect them to obtain hexafluorobenzene and chloropentafluorobenzene; then start vacuum distillation Collect incompletely fluorinated fluorochlorobenzene (dichlorotetrafluorobenzene, trichlorotrifluorobenzene, tetrachlorodifluorobenzene, ...

Embodiment 2

[0046] Add 200 g of hexachlorobenzene and 408 g of highly active potassium fluoride into a single reactor, and then add 2000 g of dried organic solvent tri-n-butylamine. After the addition, test the pressure of the single reactor for leak detection and nitrogen replacement. Then start stirring, and slowly raise the temperature to the reaction temperature of 200° C., and react at a constant temperature for 15 hours. The pressure of the single reactor rises to the reaction pressure of 2.0-3.0 Mpa. As the reaction progresses, the reaction pressure gradually increases. Stop heating after the reaction is over, lower the temperature to 130°C, open the valve of the single reactor, and steam the reaction products in the single reactor to condense and collect them to obtain hexafluorobenzene and chloropentafluorobenzene; then start vacuum distillation Collect incompletely fluorinated fluorochlorobenzene (dichlorotetrafluorobenzene, trichlorotrifluorobenzene, tetrachlorodifluorobenzene, ...

Embodiment 3

[0051] Add 200 g of hexachlorobenzene and 408 g of highly active potassium fluoride into a single reactor, and then add 2000 g of dried organic solvent tri-n-butylamine. After the addition, test the pressure of the single reactor for leak detection and nitrogen replacement. Then start stirring, and slowly raise the temperature to the reaction temperature of 230° C., and react at a constant temperature for 15 hours. The pressure of the single reactor rises to the reaction pressure of 2.0-3.0 Mpa. As the reaction progresses, the reaction pressure gradually increases. Stop heating after the reaction is over, lower the temperature to 130°C, open the valve of the single reactor, and steam the reaction products in the single reactor to condense and collect them to obtain hexafluorobenzene and chloropentafluorobenzene; then start vacuum distillation Collect incompletely fluorinated fluorochlorobenzene (dichlorotetrafluorobenzene, trichlorotrifluorobenzene, tetrachlorodifluorobenzene, ...

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Abstract

The invention discloses an environmentally friendly treatment method for hexachlorobenzene, which comprises the following steps: (1) putting hexachlorobenzene and an active potassium fluoride solution organic solvent into a single reactor; Perform pressure test, leak detection and nitrogen replacement in a single reactor; (3) raise the temperature of the single reactor to 200-300°C and increase the pressure to 2.0-3.0MPa; react at the reaction temperature and pressure for 10-15 hours; (4) put the The reaction product in the single reactor is steamed out and collected after condensation; (5) hexafluorobenzene and chloropentafluorobenzene of the rectification separation reaction product; (6) underpressure distillation collects the fluorochlorobenzene (by- product) and an organic solvent; then take out the potassium chloride residue in the single reactor, then re-add in the single reactor after drying the chlorofluorobenzene to continue using. The reaction condition is mild, the conversion rate and yield are high, and practical chemical intermediates can be obtained while reducing pollution, and the application prospect is broad.

Description

technical field [0001] The invention relates to a comprehensive utilization method of chemical by-products, in particular to an environmentally friendly treatment method for hexachlorobenzene. Background technique [0002] Hexachlorobenzene is one of the first batch of 12 controlled chemical substances in 3 categories announced by the United Nations Environment Program "Stockholm Convention on Persistent Organic Pollutants (PoPs), and the hazards to human health and environmental pollution are imminent. Hexachlorobenzene has a completely symmetrical structure, and has many chlorine substitutions, high toxicity, and very difficult to degrade. According to the survey, at least 600 tons of hexachlorobenzene are produced in the domestic chemical production process every year, and the sealed hexachlorobenzene waste has the risk of leakage and diffusion, which poses a huge hidden danger to the safety of the surrounding ecological environment. Hexachlorobenzene is usually disposed...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/20C07C25/13
Inventor 吴奕周强
Owner JUHUA GROUP TECH CENT
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