Preparation method of hexafluorobenzene and chloropentafluorobenzene
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A technology of chloropentafluorobenzene and chloropentafluorobenzene, which is applied in the field of preparation of hexafluorobenzene and chloropentafluorobenzene, can solve the problems of unfavorable industrial production, coking of reactors, and low conversion rate, and achieve a process synthesis route Short, avoid coking, less loss effect
Active Publication Date: 2013-10-23
衢州乾达科技有限公司
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[0016] The object of the present invention is to provide a method aimed at the shortcomings of the existing synthetic methods of hexafluorobenzene and chloropentafluorobenzene that the conversion rate is low, the yield is low, the reactor is seriously co
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Embodiment 1
[0048] In the reactor, add raw material hexachlorobenzene 130g, active potassium fluoride 260g, and catalyst tetrakis (diethylamino) phosphonium bromide 1.3g, after dehydrating with dichloromethane, add dry benzonitrile 130g, after the addition is completed, put The reactor is heated up slowly to 580°C and kept at constant temperature for 30 hours. The reaction pressure is 8.0-8.2Mpa. Stop heating. When the temperature drops to 300°C, open the valve to evaporate the reactant and solvent together and condense for recovery. Record the productive rate data of reaction product and see Table 1:
[0049] Table I:
[0050] Example
C 6 f 6 ,%
C 6 f 5 C1,%
Other fluorochlorobenzenes, %
Other high boiling substances, %
1
31.6
30.3
33.3
4.8
[0051] Other fluorochlorobenzenes refer to: C 6 f 4 C1 2 、C 6 f 3 C1 3 、C 6 f 2 C1 4 、C 6 FC1 5 Wait.
[0052] Other high boilers refer to products other than fluorochlorobe...
Embodiment 2、3、4、5
[0054] According to the operation steps of Example 1, keeping other reaction conditions unchanged, respectively controlling the reaction temperature to 500°C, 550°C, 600°C, and 650°C, the yield data of the measured reaction products are shown in Table 2:
[0055] Table II:
[0056] Example
Embodiment 6、7、8
[0058] According to the operation steps of Example 1, keep other reaction conditions unchanged, respectively control the ratio of the mass of hexachlorobenzene and catalyst to 1:005, 1:0.015, 1:0.03, and measure the yield data of reaction products in Table 3:
[0059] Table three:
[0060] Example
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Abstract
The invention discloses a preparation method of hexafluorobenzene and chloropentafluorobenzene. The preparation method of hexafluorobenzene and chloropentafluorobenzene comprises the following steps of: (1) adding raw materials including hexafluorobenzene, active potassium fluoride and a catalyst into a reactor; (2) carrying out nitrogen displacement on the reactor and adding a solvent into the reactor; (3) heating the reactor and stopping heating after a reaction completes; (4) after cooling, switching on an air valve of the reactor, evaporating a reaction product and the solvent in the reactor, and condensing and recycling the reaction product and the solvent; (5) deacidifying the reaction product and the solvent condensed and recycled in the step (4) through an acid separator; (6) separating hexafluorobenzene and chloropentafluorobenzene from the deacidified reaction product and solvent in the step (5) through a rectifying method; and (7) after the reaction product and the solvent in the reactor are completely recycled, cooling the reactor, opening a reaction kettle, and taking out residues such as potassium chloride in the reaction kettle. The preparation method of hexafluorobenzene and chloropentafluorobenzene has the characteristics of convenience for process operation, mildness in reaction, safety and controllability, simplicity in post treatment procedure, less loss and high yield.
Description
technical field [0001] The invention relates to a preparation method of hexafluorobenzene and chloropentafluorobenzene. Background technique [0002] Hexafluorobenzene, also known as perfluorobenzene, CAS: 392-56-3, English name Perfluorobenzene, alias hexafluorobenzene, colorless and transparent liquid, molecular formula C 6 f 6 , molecular weight 186.05, melting point 3.7-4.1°C, boiling point 81-82°C, density 1.612g / cm 3 , Refractive index 1.376-1.378. [0003] Chloropentafluorobenzene, also known as pentafluorochlorobenzene, CAS: 344-07-0, English name chloropentafluorobenzene, colorless and 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. [0004] Hexafluorobenzene and chloropentafluorobenzene can be used as important intermediates in the synthesis of perfluorinated aromatic compounds to synthesize a variety of medicines, pesticides, liquid c...
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