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Pentafluorophenol preparation mehtod

A technology for pentafluorophenol and preparation steps, applied in the field of preparation of pentafluorophenol, can solve the problems of difficulty in meeting the requirements for preparing high-quality liquid crystal materials and medicines, difficulty in separation, high production cost, complicated refining process of pentafluorophenol, etc. Stable, avoid side reactions, reduce the effect of yield

Active Publication Date: 2017-08-04
衢州乾达科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The existing technology produces pentafluorophenol, adopts conventional post-processing purification technology, and the product generally has a high content of single impurity, which is difficult to meet the technical problems of preparing high-quality liquid crystal materials and pharmaceuticals. The refining process of pentafluorophenol is complicated, and the separation is difficult and production high cost

Method used

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  • Pentafluorophenol preparation mehtod

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Preparation of hydrolysis catalyst:

[0023] (1) Preparing the precursor: by weight, put 100 parts of sodium aluminate in an air atmosphere at 400 ° C for 3 hours; then add 3 parts of potassium fluoride, 0.03 parts of 10-(2,5-dihydroxyphenyl )-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide, 0.2 parts of 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene, 5 parts of anhydrous trichloride Iron, 20 parts of sodium metasilicate pentahydrate, stir evenly, control the stirring speed to 110r / min, then leave for 5h to obtain the precursor;

[0024] (2) Drying and calcination: move the precursor to an oven, dry it at 105°C for 14 hours, grind it, and finally bake it in an air atmosphere at 400°C for 4 hours to obtain a hydrolysis catalyst;

[0025] 2. Preparation of pentafluorophenol

[0026] In parts by weight, add 700 parts of water, 75 parts of sodium hydroxide, 7 parts of hydrolysis catalyst, 100 parts of hexafluorobenzene, 0.5 part of didodecyl secondary amine into the autocla...

Embodiment 2

[0030] 1. Preparation of hydrolysis catalyst:

[0031] (1) Preparation of the precursor: by weight, put 100 parts of sodium aluminate in an air atmosphere at 200°C for 6 hours; then add 1 part of potassium fluoride, 0.01 part of 10-(2,5-dihydroxyphenyl )-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide, 0.1 part of 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene, 1 part of anhydrous trichloride Iron, 10 parts of sodium metasilicate pentahydrate, stir evenly, control the stirring speed to 100 r / min, then leave for 3 hours to obtain the precursor;

[0032] (2) Drying and calcination: move the precursor to an oven, dry it at 100°C for 24 hours, grind it, and finally bake it in an air atmosphere at 200°C for 6 hours to obtain a hydrolysis catalyst;

[0033] 2. Preparation of pentafluorophenol

[0034] In parts by weight, add 500 parts of water, 50 parts of sodium hydroxide, 3 parts of hydrolysis catalyst, 100 parts of hexafluorobenzene, 0.1 part of didodecyl secondary amine into the au...

Embodiment 3

[0038] 1. Preparation of hydrolysis catalyst:

[0039] (1) Preparation of the precursor: by weight, put 100 parts of sodium aluminate in an air atmosphere at 600 ° C for 2 hours; then add 10 parts of potassium fluoride, 0.1 part of 10-(2,5-dihydroxyphenyl )-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide, 1 part of 1,3,6,8-tetrakis(4-carboxyphenyl)pyrene, 10 parts of anhydrous trichloride Iron, 30 parts of sodium metasilicate pentahydrate, stir evenly, control the stirring speed to 120r / min, then leave for 10h to obtain the precursor;

[0040] (2) Drying and roasting: move the precursor to an oven, dry at 130°C for 12 hours, grind, and finally roast at 600°C in an air atmosphere for 2 hours to obtain a hydrolysis catalyst;

[0041] 2. Preparation of pentafluorophenol

[0042] In parts by weight, add 1000 parts of water, 100 parts of sodium hydroxide, 10 parts of hydrolysis catalyst, 100 parts of hexafluorobenzene, 1 part of didodecanyl secondary amine into the autoclave, h...

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Abstract

The invention provides a pentafluorophenol preparation method. The pentafluorophenol preparation method is characterized by comprising the following preparation steps: adding 500-1000 parts of water, 50-100 parts of sodium hydroxide, 3-10 parts of a hydrolysis catalyst, 100 parts of hexafluorobenzene and 0.1-1 part of dodecyl secondary amine into a high pressure kettle according to parts by weight, sealing the high pressure kettle, raising the temperature to 110-150 DEG C, reacting for 3-8 hours, cooling to the room temperature, filtering, acidizing, extracting with methyl tert-butyl ether, combining an organic phase, distilling to recycle a solvent, and obtaining a crude product of 2,3,4,5,6-pentafluorophenol, adsorbing the crude product of pentafluorophenol in a crude product tank through five rectifying columns, and obtaining a purified product of pentafluorophenol.

Description

technical field [0001] The invention relates to a method for preparing pentafluorophenol. Background technique [0002] Pentafluorophenol is used to prepare pentafluorophenyl active esters, which can promote the formation of peptide bonds and have almost no side effects. In addition, pentafluorophenol is also a liquid crystal material intermediate, which is especially suitable for the preparation of polyfluorinated monomer liquid crystal materials. This material is mixed with low viscosity and high dielectric anisotropy nematic liquid crystal materials to increase the molecular weight. The dipole moment, reducing the response time, improving the display performance of liquid crystal materials, and improving the clarity are of great significance to the production of high-performance liquid crystal materials. [0003] CN106588577A relates to a synthesis method of pentafluorophenol. Aiming at the problems of complicated process and high production cost in the current syntheti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/27C07C37/02C07C37/74C07C37/82
CPCC07C37/002C07C37/02C07C37/685C07C37/74C07C37/82C07C39/27
Inventor 冯晓亮吴晓秉曹鸣应亚斐章明华
Owner 衢州乾达科技有限公司
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