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A kind of preparation method of chloropentafluorobenzene

The technology of chloropentafluorobenzene and pentafluorobenzene is applied in the field of preparation of chloropentafluorobenzene, can solve problems such as low activity, limited contact efficiency, increase equipment cost, etc., and achieve the effect of easy recovery and treatment

Active Publication Date: 2020-01-31
DALIAN QIKAI MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, chlorine gas is gaseous, and the contact efficiency with the reaction substrate is limited, and the activity of electrophilic substitution between chlorine gas and hydrogen on the benzene ring is not high, so it is difficult to react with the reaction substrate (pentafluorobenzene) at normal temperature and pressure. Chlorination reaction
At the same time, due to the strong corrosiveness of chlorine gas, it has high requirements on equipment, so the chlorination reaction of chlorine gas in a pressure vessel will greatly increase the cost of equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 30g of anhydrous ferric chloride, 1.5g of anhydrous manganese chloride, 1.5g of anhydrous copper chloride, and 3g of anhydrous zinc chloride into 150mL of ethanol, and stir until dissolved (with heat release). After the ethanol solution of ferric chloride is cooled to room temperature, put in 100mL of 20-40 mesh coconut shell activated carbon for soaking. After soaking for 20 hours, heat and evaporate ethanol. Take the residue in the kettle and sieve off the powder, which is the chlorination catalyst, which needs to be kept dry and sealed.

[0030] Prepare pentafluorobenzene-ethanol solution with a mass ratio of 99:1 between pentafluorobenzene and ethanol. Take 5mL of the chlorination catalyst prepared above and put it in a fixed-bed reactor, and fill the space above the catalyst in the reactor with 10-20 mesh quartz sand as a gasification chamber and a mixing chamber. Feed chlorine gas, control the flow rate to 100mL / min, heat to 180°C, and activate for 3 hours. ...

Embodiment 2

[0032] Calcinate 20-40 mesh activated alumina particles at 500°C for 5 hours, dry and seal them for use after cooling. Put 30g of anhydrous ferric chloride and 4.5g of anhydrous zinc chloride into 150mL of ethanol, and stir until dissolved (accompanied by exotherm). After the ferric chloride ethanol solution is cooled to room temperature, put 100mL 20-40 mesh activated alumina particles into it for soaking. After soaking for 20 hours, heat and evaporate ethanol. Take the residue in the kettle and sieve off the powder, which is the chlorination catalyst, which needs to be kept dry and sealed.

[0033] Pentafluorobenzene and ethanol are configured into a pentafluorobenzene-ethanol solution at a mass ratio of 99:5. Take 5mL of the chlorination catalyst prepared above and put it in a fixed-bed reactor, and fill the space above the catalyst in the reactor with 10-20 mesh quartz sand as a gasification chamber and a mixing chamber. Feed chlorine gas, control the flow rate to 100mL...

Embodiment 3

[0035] Put 30g of anhydrous ferric trichloride, 1g of anhydrous copper chloride, and 4.5g of anhydrous zinc chloride into 150mL of ethanol, and stir until dissolved (accompanied by heat generation). After the ethanol solution of ferric chloride is cooled to room temperature, it is put into 20-40 mesh coconut shell activated carbon with a heap volume of 100mL for soaking. After soaking for 20 hours, heat and evaporate ethanol. Take the residue in the kettle and sieve off the powder, which is the chlorination catalyst, which needs to be kept dry and sealed.

[0036] Prepare pentafluorobenzene-ethanol solution with a mass ratio of 99:1 between pentafluorobenzene and ethanol. Take 5mL of the chlorination catalyst prepared above and put it in a fixed-bed reactor, and fill the space above the catalyst in the reactor with 10-20 mesh quartz sand as a gasification chamber and a mixing chamber. Feed chlorine gas, control the flow rate to 100mL / min, heat to 180°C, and activate for 3 ho...

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Abstract

The invention relates to a chloropentafluorobenzene preparation method, and belongs to the field of chemical production processes. According to the chloropentafluorobenzene preparation method, mixed gas obtained by mixing chlorine with reaction gas contacts with a catalyst to perform chlorination reaction, and pentafluorobenzene and ethyl alcohol are mixed and then gasified to obtain the reaction gas. The catalyst is prepared by a method including the steps: dissolving anhydrous ferric chloride and auxiliaries in absolute ethyl alcohol to obtain solution; adding coconut shell activated carbon or activated alumina particles into the solution, soaking the coconut shell activated carbon or activated alumina particles, and drying solvents by distillation to obtain the catalyst. The auxiliaries are one or more of manganese chloride, copper chloride and zinc chloride. Compared with the prior art, the chloropentafluorobenzene preparation method has the remarkable advantages that yield is high, solvents are omitted, reaction is continuous, no solid waste and liquid waste are generated, and the method is greener and more environment-friendly as compared with other methods.

Description

technical field [0001] The invention relates to a preparation method of chlorinated pentafluorobenzene, which belongs to the field of chemical production technology. Background technique [0002] Chloropentafluorobenzene is usually a colorless transparent liquid with the molecular formula C 6 f 5 Cl, molecular weight 202.50, melting point 18.1°C, boiling point 122-123°C, density 1.64g / cm 3 , the refractive index is 1.424. As an important basic chemical raw material, it can be used as an important intermediate in the synthesis of various perfluorinated aromatic compounds such as hexafluorobenzene, and in the synthesis of various medicines, pesticides, liquid crystal materials and special polymers, and has very broad development prospects. [0003] The introduction of fluorine atoms into organic compounds, especially aromatic compounds, can often make them exhibit special biological and physiological activities. Therefore, a large number of fluorine-containing pesticides an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/12C07C25/13
CPCC07C17/12C07C25/13
Inventor 田瀚卿姜殿平张洪学张忠
Owner DALIAN QIKAI MEDICAL TECH
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