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Refining method for hexafluoromethylene aromatic compound

An aromatic compound, hexafluoromethylene technology, applied in 2, can solve problems such as large amount of wastewater, complex process, and increased environmental pressure

Inactive Publication Date: 2007-02-28
SHANGHAI 3F NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Although the method of post-processing 2,2-bis(4-hydroxyphenyl)hexafluoropropane can obtain higher purity 2,2-bis(4-hydroxyphenyl)hexafluoropropane compound, but this method The process is complicated, involving secondary alkali and acid reactions; secondary evaporation, concentration, separation, washing, and drying chemical unit operations; and a large amount of waste water is generated, which not only increases the cost of the product, but also increases the pressure on the environment

Method used

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  • Refining method for hexafluoromethylene aromatic compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] In a 1-liter autoclave, add 270 grams of xylene and 330 grams of hydrofluoric anhydride, and introduce 210 grams of hexafluoroacetone under stirring. The reaction was continued for 5 hours under the reaction conditions of 95°C / 0.9Mpa. After the reaction, put the reaction product into 3 kg of water, then fully wash the precipitated solid with water, and then dry it to obtain light yellowish brown 2,2-bis(3,4-dimethylphenyl)hexafluoropropane Crude product with a purity of 97.5%.

[0075] Add 400 grams of 20.0 grams of tan-colored 2,2-bis(3,4-dimethylphenyl)hexafluoropropane at a temperature of 70° C. and 30 grams of acetone in water (the weight ratio of acetone to water is 1:11.7; the weight ratio of 2,2-bis(3,4-dimethylphenyl)hexafluoropropane to the mixed solvent is 1:19.5). Slowly and uniformly lower the temperature to 10°C under the action of stirring to obtain a mixture of crystallization and composite solvent, filter, wash the crystallization with 5 times of deion...

Embodiment 2

[0077] In the same manner as in Example 1, the aromatic compound 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane was obtained; 20 grams of 2,2-bis(3 -Nitro-4-hydroxyphenyl)hexafluoropropane crude product, 30 grams of acetonitrile, 250 grams of toluene to form a mixture of 85 ° C into the three-necked flask [wherein 2,2-bis (3-nitro-4-hydroxyphenyl ) the ratio of hexafluoropropane to the mixed solvent weight is 1: 14.4, acetonitrile: toluene (weight)=1: 8.3], under the effect of stirring, slowly and uniformly cool down to 10 ℃ for 10 hours to obtain the mixture of crystallization and composite solvent , filter, and wash the yellowish crystals with 5 times of deionized water, filter again, transfer the crystals to an oven, and keep the temperature at 135°C for 10 hours to obtain a yellowish coarse powder 2,2-bis(3-nitro-4 -Hydroxyphenyl) hexafluoropropane 18.0 g, purity 99.6%, yield 92.4%.

Embodiment 3

[0079] In the same way as in Example 1, the aromatic compound 2,2-bis(4-hydroxyphenyl)hexafluoropropane was obtained; 20 grams of 2,2-bis(4-hydroxyphenyl) with a purity of 97.0% A mixture of crude hexafluoropropane, 20 grams of ethanol, 5 grams of methylcyclohexane, and 550 grams of water at 90°C was added to a 1000-milliliter three-necked flask [wherein 2,2-bis(4-hydroxyphenyl)hexafluoropropane and The weight ratio of the mixed solvent is 1: 29.7, ethanol: methylcyclohexane: water (weight) = 4: 1: 110], under the action of stirring, slowly and uniformly cool down to 20°C for 18 hours to obtain crystallization and compound The mixture of solvents is filtered, and the crystals are washed with 5 times of deionized water, and then filtered, and the crystals are transferred to an oven at a constant temperature of 135°C for 10 hours to obtain milky white needle crystals 2,2-bis(4-hydroxyphenyl) 18.5 grams of hexafluoropropane, with a purity of 99.8%, and a yield of 95.2%.

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Abstract

The invention discloses a purifying method of aromatic methylene hexafluoride compound, which comprises the following steps: a) providing composite solvent with at least one soluble true solvent of aromatic methylene hexafluoride compound and at least one soluble non-solvent of aromatic methylene hexafluoride compound; b) dissolving aromatic methylene hexafluoride compound in the composite solvent to form solution; c) cooling; d) reducing solution temperature to obtain crystal-solution compound; filtering; washing; drying; crystallizing.

Description

technical field [0001] The present invention relates to a method for purifying hexafluoromethylene aromatic compounds, in particular to 2,2-bis(4-hydroxyphenyl)hexafluoropropane, 2,2-bis(3,4-dimethylphenyl) ) Purification method of hexafluoropropane. Background technique [0002] Hexafluoromethylene aromatic compounds are heat-resistant and radiation-resistant multi-active group compounds or their precursors in the chemical application field. Non-limiting examples of such hexafluoromethylene aromatic compounds include, for example, 2,2-bis(4-hydroxyphenyl)hexafluoropropane as a fluororubber crosslinking agent; 2,2-bis(3,4-dimethylphenyl)hexafluoropropane, and 2,2-bis(4-methylphenyl)hexafluoropropane, 2, 2-bis[4-(4-nitrophenoxy)phenyl]hexafluoropropane, 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane and other symmetrical bisaryl hexafluoropropanes , and 1,2-bis(2-hydroxyhexafluoroisopropyl)benzene, 1,4-bis(2-hydroxyhexafluoroisopropyl)benzene and other compounds contain...

Claims

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Application Information

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IPC IPC(8): C07C22/08C07C17/392
Inventor 应德雄粟小理江建安周荣明蒋振宁
Owner SHANGHAI 3F NEW MATERIAL
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