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A kind of method for the dehydration of mixture of hexachlorobenzene and potassium fluoride

A technology of potassium fluoride and hexachlorobenzene, applied in organic chemistry, halogen substitution preparation, etc., can solve problems such as reactor corrosion, potential safety hazards, equipment damage, etc., and achieve the effects of reducing corrosion, complete dehydration, and simple process

Active Publication Date: 2015-09-16
衢州乾达科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Hexachlorobenzene and potassium fluoride are raw materials for the preparation of hexafluorobenzene, etc., and the preparation of hexafluorobenzene by using hexachlorobenzene and potassium fluoride needs to be carried out under high temperature and high pressure, and the deliquescence of potassium fluoride makes the reaction voxel There is a trace amount of water, and the existence of these trace amounts of water will cause serious corrosion of the reactor during the preparation of hexafluorobenzene, which will not only cause damage to the equipment, but also cause serious safety hazards. Therefore, remove hexachlorobenzene and fluorine before the reaction. The moisture in the potassium chloride mixture is extremely necessary

Method used

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  • A kind of method for the dehydration of mixture of hexachlorobenzene and potassium fluoride
  • A kind of method for the dehydration of mixture of hexachlorobenzene and potassium fluoride
  • A kind of method for the dehydration of mixture of hexachlorobenzene and potassium fluoride

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Effect test

Embodiment 1

[0021] Add 130 g of raw materials hexachlorobenzene, 260 g of active potassium fluoride, and 400 g of solvent dichloromethane into the reactor. After the addition is completed, the reactor is heated to 40-50° C., and the temperature is maintained for 30 hours. After opening the valve, the solvent Evaporate and condense for recovery. Measure solvent moisture data.

Embodiment 2

[0023] According to the operation steps of Example 1, keeping other things unchanged, benzene is used as the solvent, the temperature of the reactor is controlled to be 80-90° C., and the moisture content of the solvent is measured.

Embodiment 3

[0025] According to the operation steps of Example 1, keeping other things unchanged, toluene was used as the solvent, the temperature of the reactor was controlled to be 110-120° C., and the moisture content of the solvent was measured.

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Abstract

The invention relates to a method for dewatering a mixture of hexachlorobenzene and potassium fluoride. The method comprises the following steps of: (1) placing the hexachlorobenzene and potassium fluoride with moisture into a closed container; (2) adding dry solvent into the closed container containing the hexachlorobenzene and potassium fluoride with moisture; (3) heating the closed container containing the hexachlorobenzene, the potassium fluoride and the dry solvent until the solvent is boiled for 30 minutes, then evaporating the solvent, condensing to recover the solvent; (4) measuring moisture in the solvent recovered by condensation obtained from step (3), if the moisture in the solvent is larger than 50ppm, continuously dewatering, adding the recovered solvent after drying into the closed container again, and repeating processes of heating, solvent recovering and the like in the step (3) until the moisture in the solvent is less than 50ppm. The method is simple in process and complete in dewatering. By utilizing the method, safe operation of a fluorobenzene reactor is realized, and a processed material can be directly used for fluorobenzene reaction.

Description

technical field [0001] The invention relates to a method for dehydrating a mixture of hexachlorobenzene and potassium fluoride. Background technique [0002] Hexachlorobenzene, also known as hexachlorobenzene, CAS: 118-74-1, English name hexachlorobenzene, pure product is colorless fine needle or small plate crystal, industrial product is light yellow or light brown crystal, molecular formula C 6 Cl 6 , molecular weight 284.78, melting point 231°C, boiling point 309°C, density 2.044g / cm3, insoluble in water, limitedly soluble in most organic solvents such as heated ethanol and chloroform. [0003] Potassium fluoride, CAS: 7789-23-3, English name Potassium fluoride, colorless cubic crystal. Molecular formula KF, molecular weight 58.1, melting point 858°C, boiling point 1505°C, density 2.48g / cm3, deliquescent, easily soluble in water, slightly soluble in alcohol and acetone. [0004] Hexachlorobenzene and potassium fluoride are raw materials for the preparation of hexafluor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C25/13C07C17/20
Inventor 吴晓秉陈鸿福吴纬斌鲁帅
Owner 衢州乾达科技有限公司
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