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Method of batch fractionating and purifying 1,1,1,3,3,3-hexafluoroisopropanol

A technology of hexafluoroisopropanol and rectification, applied in 1 field, can solve the problems such as difficult to purify and obtain, low water content and the like

Active Publication Date: 2007-08-15
SHANGHAI 3F NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the primary product of hexafluoroisopropanol produced by liquid-phase catalytic hydrogenation reduction of hexafluoroacetone hydrate contains a large amount of water and impurities, and it is difficult to purify and obtain low-water High purity hexafluoroisopropanol with low content and low impurity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0032] Preparation of crude hexafluoroisopropanol

[0033] The palladium-carbon catalyst was rinsed with hexafluoroacetone solvent for 10 minutes. The washed palladium-carbon catalyst was soaked with hexafluoroacetone hydrate for 40 hours. Then the above catalyst was filtered out and added to 56Kg of hexafluoroacetone trihydrate solution, and the catalyst concentration was 0.9%. Repeat vacuum-nitrogen and vacuum-hydrogen replacement until the oxygen content in the autoclave is lower than 100 ppm, heat up to 100 degrees, introduce hydrogen, and stir to react. The reaction time was 6 hours, the temperature was lowered to room temperature, and the material was discharged. The HFIP product clear liquid was obtained by sampling and filtering, and the GC test result was 70%.

Embodiment 1

[0038] Add 100 grams of anhydrous copper sulfate to the hexafluoroisopropanol crude product obtained in 400ml of Preparation Example 1, and use the same rectifying column as in Comparative Example 1 to carry out the obtained hexafluoroisopropanol crude product / copper sulfate mixed solution. Atmospheric rectification, with a reflux ratio of 1:15, obtains hexafluoroisopropanol with a purity of 98.8% by distillation, its water content is 0.85% by distillation, and the distillation yield of primary rectified hexafluoroisopropanol is 95% by weight.

Embodiment 2

[0040] In 400ml hexafluoroisopropanol crude product, add 100 grams of anhydrous magnesium sulfate, adopt the same rectifying tower as Comparative Example 1 to carry out atmospheric rectification to the obtained hexafluoroisopropanol crude product / magnesium sulfate mixed solution, reflux. The ratio is 1:15 to obtain hexafluoroisopropanol with a purity of 98.9 wt %, a water content of 0.7 wt %, and a distillation yield of 96 wt % of primary rectified hexafluoroisopropanol.

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PUM

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Abstract

The invention discloses a purifying method of 1, 1, 1, 3, 3, 3-hexafluoride isopropanol (HFIP) catalyzed and hydrogenated by hexafluoroacetone (HFA), which is characterized by the following: removing partial water and impurity from rough product of HFIP; adding non-volatile soluble inorganics to rectify; improving impurity to 99.9%.

Description

technical field [0001] The invention relates to a purification method of 1,1,1,3,3,3-hexafluoroisopropanol prepared by hydrogenation catalytic reduction of hexafluoroacetone. Background technique [0002] Hexafluoroisopropanol (HFIP for short) is an important fluorine-containing fine chemical. With reactive groups, hexafluoroisopropanol is an important fluorine-containing intermediate, which can be used to prepare high-end fluorine-containing fine chemicals such as anesthetics (eg, see US 3689571) and surfactants. In addition, hexafluoroisopropanol has a strong polarity, is easily miscible with water and many organic reagents, is heat-resistant and allows ultraviolet rays to pass through. These properties make hexafluoroisopropanol an ideal solvent for many polymer systems, including polyamide, Universal solvent for polymer systems of polyester, polyacrylonitrile, polyacetal and hydrolyzed polyvinyl esters. Hexafluoroisopropanol polymer solutions are particularly important...

Claims

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Application Information

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IPC IPC(8): C07C29/76C07C31/38
Inventor 冯东东粟小理
Owner SHANGHAI 3F NEW MATERIAL TECH CO LTD
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