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Chloropentafluorobenzene preparation method

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

Active Publication Date: 2017-09-22
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] 30 g of anhydrous iron trichloride, 1.5 g of anhydrous manganese chloride, 1.5 g of anhydrous copper chloride, and 3 g of anhydrous zinc chloride were put into 150 mL of ethanol and stirred until dissolved (with exotherm). After the ferric trichloride ethanol solution is cooled to room temperature, it is put into the pile volume of 100mL 20-40 mesh coconut shell activated carbon soaked. After soaking for 20 hours, the ethanol is evaporated by heating. Take the residue in the kettle and sift to remove the powder, which is the chlorination catalyst, which needs to be dried and sealed.

[0030] The pentafluorobenzene and ethanol are prepared into a pentafluorobenzene-ethanol solution at a mass ratio of 99:1. Take 5 mL of the chlorination catalyst prepared above and install 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. Add chlorine gas, control the flow rate to 100mL...

Embodiment 2

[0032] The 20-40 mesh activated alumina particles are calcined at 500° C. for 5 hours, and are dried and sealed for use after cooling. 30 g of anhydrous iron trichloride and 4.5 g of anhydrous zinc chloride were put into 150 mL of ethanol, and stirred until dissolved (with exotherm). After the ferric trichloride ethanol solution is cooled to room temperature, it is put into the pile volume of 100mL 20-40 mesh activated alumina particles soaked. After soaking for 20 hours, the ethanol is evaporated by heating. Take the residue in the kettle and sift to remove the powder, which is the chlorination catalyst, which needs to be dried and sealed.

[0033] The pentafluorobenzene and ethanol are prepared into a pentafluorobenzene-ethanol solution at a mass ratio of 99:5. Take 5 mL of the chlorination catalyst prepared above and install 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 chamb...

Embodiment 3

[0035] 30 g of anhydrous ferric chloride, 1 g of anhydrous copper chloride, and 4.5 g of anhydrous zinc chloride were put into 150 mL of ethanol, and stirred until dissolved (with exothermic heat). After the ferric trichloride ethanol solution is cooled to room temperature, it is put into the pile volume 100mL 20-40 mesh coconut shell activated carbon soaked. After soaking for 20 hours, the ethanol is evaporated by heating. Take the residue in the kettle and sift to remove the powder, which is the chlorination catalyst, which needs to be dried and sealed.

[0036] The pentafluorobenzene and ethanol are prepared into a pentafluorobenzene-ethanol solution at a mass ratio of 99:1. Take 5 mL of the chlorination catalyst prepared above and install 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. Add chlorine gas, control the flow rate to 100mL / min, heat to 180°C, and activate f...

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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] Chlorinated pentafluorobenzene is usually a colorless transparent liquid, 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. It is an important basic chemical raw material and can be used as an important intermediate for the synthesis of various perfluoroaromatic compounds such as hexafluorobenzene. It can synthesize a variety of medicines, pesticides, liquid crystal materials and special polymers, and has very broad development prospects. [0003] The introduction of fluorine atoms in organic compounds, especially aromatic compounds, can often cause them to exhibit special biological and physiological activities. Therefore, in recent years, a large number of fluorine-containing pesticide...

Claims

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Application Information

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Patent Type & Authority Applications(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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