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Method for synthesis of 1,1,1,3,3,3-hexafluoroisopropanol

A technology of hexafluoroisopropanol and hexafluoroacetone is applied in the field of synthesis of 1,1,1,3,3,3-hexafluoroisopropanol, and can solve the problems of high cost, low efficiency of hexafluoroisopropanol, Problems such as unsatisfactory reaction efficiency

Active Publication Date: 2008-09-24
SHANGHAI 3F NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purification of hexafluoroacetone is relatively easy, but the efficiency of preparing hexafluoroisopropanol by liquid-phase catalytic hydrogenation reduction of hexafluoroacetone hydrate is low
[0010] Although the reaction time can be reduced by using a composite catalyst system, this catalyst system has the disadvantage of high cost, and the reaction efficiency is still not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 3

[0042] The palladium carbon catalyst was washed with hydrochloric acid / hexafluoroacetone mixed solvent for 5 minutes, and the volume mixing ratio of hydrochloric acid and hexafluoroacetone was 1:5. The palladium carbon catalyst after washing is soaked in a mixed solvent of hexafluoroisopropanol (HFIP) and hexafluoroacetone for 60 hours. Then the above catalyst was filtered out and added to 56Kg of hexafluoroacetone trihydrate solution with a catalyst concentration of 1%. Vacuum-nitrogen, vacuum-hydrogen are replaced repeatedly until the oxygen content in the autoclave is lower than 100ppm, the temperature is raised to 100°C, hydrogen is introduced, and the reaction is stirred. V 1 / V 0 When the temperature is 0.05, the hydrogenation is stopped, the reaction time is 4.5 hours, the temperature is cooled to room temperature, and the material is discharged. Sampling and filtration obtained hexafluoroisopropanol (HFIP) product clear liquid, and its GC test result was 97.5%.

Embodiment 4

[0044] The platinum carbon catalyst was soaked in hexafluoroacetone solvent for 2 minutes, and then filtered to remove hexafluoroacetone. The palladium carbon catalyst after washing is soaked in hexafluoroacetone hydrate for 50 hours. Then the above catalyst was filtered out and added to 52Kg of hexafluoroacetone trihydrate solution with a catalyst concentration of 0.8%. Vacuum-nitrogen, vacuum-hydrogen are replaced repeatedly until the oxygen content in the autoclave is lower than 100ppm, the temperature is raised to 100°C, hydrogen is introduced, and the reaction is stirred. V 1 / V 0 When the temperature is 0.05, the hydrogenation is stopped, the reaction time is 5 hours, the temperature is cooled to room temperature, and the material is discharged. Sampling and filtration obtained hexafluoroisopropanol (HFIP) product clear liquid, and its GC test result was 96.3%.

Embodiment 5

[0046] The palladium on carbon catalyst was washed with hexafluoroacetone solvent for 10 minutes. The washed palladium carbon catalyst is soaked in hexafluoroacetone hydrate for 40 hours. Then the above catalyst was filtered out and added to 56Kg of hexafluoroacetone trihydrate solution with a catalyst concentration of 0.9%. Vacuum-nitrogen, vacuum-hydrogen are replaced repeatedly until the oxygen content in the autoclave is lower than 100ppm, the temperature is raised to 100°C, hydrogen is introduced, and the reaction is stirred. V 1 / V 0 When the temperature is 0.05, the hydrogenation is stopped, the reaction time is 6 hours, the temperature is cooled to room temperature, and the material is discharged. Sampling and filtration obtained hexafluoroisopropanol (HFIP) product clear liquid, and its GC test result was 96.5%.

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Abstract

The invention discloses a preparing method of 1, 1, 1, 3, 3, 3-hexafluoroisopropanol, which comprises the following steps: a) adding catalyst in the reactor with hexafluoroacetone hydrate; b) aerating hydrogen in the reactor under inert gas to do reducing reaction; predisposing catalyst; i) proceeding acid-washing for catalyst; ii) immersing the catalyst through organic solvent for 10-100h.

Description

technical field [0001] The invention relates to a synthesis method for preparing 1,1,1,3,3,3-hexafluoroisopropanol by hydrogenation catalytic reduction of hexafluoroacetone. Background of the invention [0002] Hexafluoroisopropanol (HFIP for short) is an important fluorine-containing fine chemical. Hexafluoroisopropanol has a reactive group and is an important fluorine-containing intermediate that can be used to prepare high-end fluorine-containing fine chemicals such as anesthetics (for example, see US 3,689,571), surfactants, and the like. In addition, hexafluoroisopropanol has strong polarity, is easily miscible with water and many organic reagents, is heat-resistant and allows ultraviolet light to pass through, these characteristics make hexafluoroisopropanol an ideal solvent for many polymer systems, including polyamide, Universal solvent for polymer systems of polyesters, polyacrylonitriles, polyacetals and hydrolyzed polyvinyl esters. Hexafluoroisopropanol polymer ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/145C07C31/38
Inventor 冯东东粟小理张文渊
Owner SHANGHAI 3F NEW MATERIAL TECH CO LTD
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