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Refining process of high-purity pentafluorophenol

A pentafluorophenol and high-purity technology is applied in the refining process field of pentafluorophenol, which can solve the problems of small pollution, high yield, low energy consumption, etc., and achieve the effects of stable quality and good appearance and color.

Inactive Publication Date: 2016-12-07
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a refining process for high-purity pentafluorophenol. The process scheme combines the characteristics of industrial production of pentafluorophenol, and combines the traditional decolorization extraction process, fluoride removal and sedimentation process with molecular refining. The combination of distillation process effectively solves the quality problem of pentafluorophenol products. The purity, impurity content, dissolved residue, moisture and other indicators of refined pentafluorophenol products can all meet the quality standards of liquid crystal intermediates and pharmaceutical intermediates. The products The appearance and color are good, and the color will not change after long-term storage. The process is simple and easy, and compared with traditional processes, it has lower energy consumption, higher yield and less pollution. It is used for the purification of crude pentafluorophenol and the post-treatment process of industrial production of pentafluorophenol , has been maturely applied in actual industrial production

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  • Refining process of high-purity pentafluorophenol
  • Refining process of high-purity pentafluorophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 10kg of crude pentafluorophenol into a 50L custom-made extraction kettle with a built-in polytetrafluoroethylene coating, add 20L of dichloromethane and stir to dissolve, cool down the temperature of the extraction kettle to 5°C, and use a metering pump to pump 10% dilute hydrochloric acid solution from the acid storage tank Pump into the extraction kettle, stop when the pH reaches 4.5, keep the temperature in the kettle not exceeding 10°C, then add 1kg activated 4A molecular sieve, 260g vitamin C, 120g hydroquinone in sequence, stir for 4 hours, filter and then add 1.5kg activated carbon Carry out decolorization treatment for 2 hours, and then filter again; the filtrate is transferred to a defluoridation settler, and 18g of mixed flocculant (the mass ratio of activated alumina to polyaluminum chloride is 1:1.5) is added for 2 hours, and the mixture is pumped into a centrifuge for centrifugation, and the filtrate Filter through the ultrafiltration membrane again, get...

Embodiment 2

[0029] After filtering the pentafluorophenol mixture (without post-treatment) prepared by 1-halogenated pentafluorobenzene through basic catalysis and hydrolysis reaction, the filtrate was passed into the extraction kettle, and treated with reference to the method described in Example 1 to obtain pentafluorophenol The phenol product is detected by gas chromatography, the content is 99.81%, the simple impurity content is 0.08%, the fluorine loss is 0.01%, the melting point is 34-36°C, and the yield is 81.2%.

[0030] In summary, the pentafluorophenol product obtained by this process has good appearance and color, stable quality, high purity, and low energy consumption. The product quality can meet the quality requirements of liquid crystal intermediates and pharmaceutical intermediates.

[0031] The high-purity pentafluorophenol product obtained by adopting the technical scheme of the present invention can especially meet its quality requirements as a fluorine-containing liquid ...

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Abstract

The invention relates to a refining process of high-purity pentafluorophenol. The refining process comprises the following steps: (1) a decoloration process: dissolving rough pentafluorophenol into an organic solvent, regulating the pH value of the solution to be faintly acid, adding a molecular sieve, activated carbon, an antioxidant and a polymerization inhibitor, adequately stirring, and filtering; (2) a defluorination sedimentation process: introducing filtrate into defluorination flocculation equipment, adding an inorganic aluminum coagulant, carrying out stirring flocculation, pumping the filtrate into a rapid settling device, and filtering the filtrate by virtue of an ultrafiltration membrane to remove fluorine ions and a trace amount of heavy metal impurities until the concentration of the fluorine ions in the solution is less than 3mg / kg; and (3) a molecular rectifying process: introducing the solution into second-level file scraping type molecular rectifying equipment, and carrying out decompressed low-temperature rectifying to remove low-boiling components and high-boiling components, so as to obtain a high-purity pentafluorophenol product. Compared with the existing conventional process, the refining process has the advantages that the separation effect is excellent, and the product quality can be remarkably improved. The refining process is suitable for industrial production.

Description

technical field [0001] The invention relates to a chemical and pharmaceutical intermediate, in particular to a refining process of pentafluorophenol used for the purification of crude pentafluorophenol and the post-treatment of the industrial production of pentafluorophenol. Background technique [0002] As an important chemical intermediate, pentafluorophenol is widely used in liquid crystal, medicine and other fields. Due to the special properties of fluorine atoms such as electronic effect, simulation effect, barrier effect and permeation effect, fluorine-containing liquid crystal monomer materials often use fluorine atoms or fluorine-containing groups as polar end groups, which have low viscosity, high resistivity, and responsiveness. With the advantages of fast speed and high dielectric constant, pentafluorophenol is widely used in fluorine-containing liquid crystal intermediate materials. The purity, impurity content, fluorine loss, solvent residue, moisture content a...

Claims

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Application Information

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IPC IPC(8): C07C37/88C07C37/74C07C37/82C07C37/68C07C39/27
Inventor 窦杰杨俊伟扈广法王燕李程碑杭磊李浩
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND