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Environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane

A technology of hydroxyphenyl and hexafluoropropane, which is applied in the field of 2,2-dihexafluoropropane preparation process, can solve problems affecting the quality of reaction products, corrosion, damage to equipment, etc., and reduce the generation of toxic, harmful and high-risk by-products , the effect of eliminating pollution

Active Publication Date: 2016-07-13
LIANYUNGANG TETRAFLUOR NEW MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The green environmental protection preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl) hexafluoropropane of the present invention discloses a new scheme, adopts dinitrogen pentoxide (N 2 o 5 ) as a nitrating agent provides a new option for the nitration reaction process, eliminates the use of strong acid nitrating agents from the source, and solves the problem that the existing strong acid nitrating agent solution is prone to serious environmental pollution, corrosion and damage to equipment, and large hidden dangers in reaction safety. And problems that affect the quality of subsequent reaction products

Method used

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  • Environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane
  • Environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane
  • Environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane

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Effect test

Embodiment 1

[0024] In a 500 ml three-necked flask equipped with an electric stirrer, add 67 grams of bisphenol AF and 335 grams of 1,2-dichloroethane, dissolve under stirring, add 1.5 grams of catalyst A, cool in an ice bath, and at 20 ° C Add 100ml of 12mol / L N dropwise 2 o 5 / 1,2-dichloroethane solution, after the dropwise addition is completed, the temperature is raised to 30-45°C, and the reaction is continued for 4 hours. After the reaction, filter, pour the filtrate into a separatory funnel, add about 60 ml of 5% sodium carbonate solution and deionized water to wash to neutrality, separate the organic layer, and continue to use about 50 grams of 1,2 -Dichloroethane was extracted and separated, the organic phases were combined, dried by adding 30 grams of anhydrous sodium sulfate, filtered, and the filtrate was distilled under negative pressure (about 400-500kPa vacuum) to recover 1,2-dichloroethane, and the residual solid Add 300 milliliters of absolute ethanol and 1 gram of activa...

Embodiment 2

[0027] In a 500 ml three-neck flask equipped with an electric stirrer, add 67 grams of bisphenol AF and 268 grams of 1,2-dichloroethane, dissolve under stirring, add 1.5 grams of catalyst A, cool in an ice bath, and at 0 ° C Add 120ml of 12mol / L N dropwise 2 o 5 / 1,2-dichloroethane solution, after the dropwise addition is completed, the temperature is raised to 20-30°C, and the reaction is continued for 5 hours. After the reaction, filter, pour the filtrate into a separatory funnel, add about 60 ml of 5% sodium carbonate solution and deionized water to wash to neutrality, separate the organic layer, and continue to use about 50 grams of 1,2 -Dichloroethane was extracted and separated, the organic phases were combined, dried by adding 30 grams of anhydrous sodium sulfate, filtered, and the filtrate was distilled under negative pressure (about 400-500kPa vacuum) to recover 1,2-dichloroethane, and the residual solid Add 300 milliliters of absolute ethanol and 1 gram of activate...

Embodiment 3

[0030] In a 500 ml three-necked flask equipped with an electric stirrer, add 67 grams of bisphenol AF and 268 grams of 1,2-dichloroethane, dissolve under stirring, add 1.5 grams of catalyst A, cool in an ice bath, and at 10 ° C Add 120ml of 12mol / L N dropwise 2 o 5 / 1,2-dichloroethane solution, after the dropwise addition is completed, the temperature is raised to 15-20°C, and the reaction is continued for 6 hours. After the reaction, filter, pour the filtrate into a separatory funnel, add about 60 ml of 5% sodium carbonate solution and deionized water to wash to neutrality, separate the organic layer, and continue to use about 50 grams of 1,2 -Dichloroethane was extracted and separated, the organic phases were combined, dried by adding 30 grams of anhydrous sodium sulfate, filtered, and the filtrate was distilled under negative pressure (about 400-500kPa vacuum) to recover 1,2-dichloroethane, and the residual solid Add 300 milliliters of absolute ethanol and 1 gram of activ...

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Abstract

The invention relates to an environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane. The technology comprises the following steps: preparing a 1,2-dichloroethane solution of bisphenol AF; preparing a 1,2-dichloroethane solution of N2O5; carrying out a nitration reaction to generate 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane; filtering the 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, washing the 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, and layering the 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane to obtain a lower layer organic phase; carrying out dehydration drying, filtering the obtained material, and carrying out vacuum distillation to obtain crude 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane; and re-crystallizing the crude 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, cooling the re-crystallized 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, filtering the cooled 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, and carrying out vacuum drying to obtain purified 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane. The preparation technology adopts dinitrogen pentoxide (N2O5) as a nitration agent and allows the reaction to be carried out a low temperature, so pollution of waste acids is thoroughly eliminated, and toxic, harmful and highly risky byproducts are reduced, and the nitration reaction is clean and environmentally friendly.

Description

technical field [0001] The invention relates to a preparation process of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, in particular to a process using dinitrogen pentoxide (N 2 o 5 ) nitrating agent 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane green preparation process, which belongs to 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane field of preparation. Background technique [0002] 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane is an important chemical raw material, especially for the synthesis of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane It is widely used in aviation, aerospace, electronics industry, light wave communication, gas separation and precision machinery and other fields. At present, nitrating agents such as nitric acid mixed acid, nitrates, and metal nitrates are widely used in industry to prepare 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane. During the production process, a large amount of waste acid and organic acid waste wat...

Claims

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Application Information

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IPC IPC(8): C07C205/26C07C201/08
Inventor 吕志强姚洪星
Owner LIANYUNGANG TETRAFLUOR NEW MATERIALS
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