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Hexafluoroacetone hydrate dehydrolyzing method

A technology of hexafluoroacetone hydrate and hexafluoroacetone, which is applied in the preparation of organic compounds, carbon-based compounds, chemical instruments and methods, etc., can solve the problems of low yield and difficult precipitation

Active Publication Date: 2007-06-20
SHANGHAI 3F NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the melting point of hexafluoroacetone monohydrate (b.p.48°C) is relatively high, a small amount of hexafluoroacetone monohydrate carried in hexafluoroacetone is difficult to precipitate at room temperature
Therefore general laboratory method can only obtain the liquid phase hexafluoroacetone of a small amount of yield not high, containing part of hexafluoroacetone monohydrate

Method used

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  • Hexafluoroacetone hydrate dehydrolyzing method
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  • Hexafluoroacetone hydrate dehydrolyzing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0061] 1. Determination method of hexafluoroacetone monohydrate content in hexafluoroacetone gas

[0062] Use HP 6890 chromatograph, DB5 capillary column (specification: ￠0.25mm×30m); column temperature: 30°C; carrier gas: H2; pre-column pressure: 10psi; current: 200mA.

[0063] 2. Determination method of sulfur trioxide content in anhydrous hexafluoroacetone gas

[0064] Use HP 6890 chromatograph, DB1 capillary column (specification: ￠0.25mm×30m); column temperature: 30°C; carrier gas: H2; pre-column pressure: 10psi; current: 200mA.

Embodiment 1

[0074] Use 20% oleum as dehydrating agent and post-treatment with 98wt% sulfuric acid

[0075] Add 1,000 grams of 95% hexafluoroacetone trihydrate dropwise to 4,400 grams of 20% oleum, control the mixing temperature at 0-100°C, make it fully mixed, and use the above method to determine the concentration of hexafluoroacetone monohydrate. Content, the result is 4.1%; determination of sulfur trioxide content, the result is 2.0%.

[0076]When the generated gas is fully mixed with 5000 g of 98% sulfuric acid, the temperature is controlled at 0-50°C, and the content of sulfur trioxide and hexafluoroacetone monohydrate is determined to be 0.0% and 0.0% respectively. Then the gas was introduced into a cold trap cooled by dry ice-ethanol to obtain 713.6 g of hexafluoroacetone, and the yield of hexafluoroacetone was about 99.6%.

[0077] During the whole dropwise addition of hexafluoroacetone trihydrate, no increase in reaction pressure was observed, and no white obstruction was observ...

Embodiment 2

[0079] Use 50% oleum and 95% sulfuric acid sequentially as dehydrating agent (absorbent)

[0080] Add 1100 g of 90% hexafluoroacetone trihydrate dropwise to 2600 g of 50% oleum, control the temperature at 30-120° C., and make it fully mixed. The generated gas is fully mixed with 5000 grams of 95% sulfuric acid, and the mixing temperature is controlled at 20-60°C. Measure the content of hexafluoroacetone monohydrate and sulfur trioxide in the anhydrous hexafluoroacetone gas, wherein the content of sulfur trioxide is 0.0%; the content of hexafluoroacetone monohydrate is 0.0%. Then the gas was introduced into a cold trap cooled by dry ice-ethanol to obtain 740 g of hexafluoroacetone, and the yield of hexafluoroacetone was about 99.0%.

[0081] During the whole dropwise addition of hexafluoroacetone trihydrate, no increase in reaction pressure was observed, and no white obstruction was observed in the cold trap coil.

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Abstract

The hexafluoro acetone hydrate dewatering process includes the following steps: A. making hexafluoro acetone hydrate contact with SO3 or fuming sulfuric acid to form gas mixture of SO3 and hexafluoro acetone, or mixture of hexafluoro acetone-water compound and gaseous hexafluoro acetone, or mixture of hexafluoro acetone-water compound, SO3 and gaseous hexafluoro acetone and concentrated sulfuric acid; and B. making the gaseous mixture contact with concentrated sulfuric acid to eliminate its SO3 and hexafluoro acetone-water compound.

Description

technical field [0001] The invention relates to a method for dehydrating hexafluoroacetone hydrate to form anhydrous hexafluoroacetone. Background technique [0002] Hexafluoroacetone is the simplest and most important perfluoroketone compound, and also the most basic fine organic fluorine chemical. Using hexafluoroacetone as raw material can produce many valuable civilian or military chemical products, such as: [0003] (a) Preparation of excellent solvent-hexafluoroisopropanol as artificial fiber polyester, polyether spinning, comprehensive utilization of chitin, gel chromatography, etc.; [0004] (b) Monomer H used in the manufacture of high and low temperature resistant, radiation resistant and transparent materials (polyimide materials) used in the aerospace industry 2 NC 6 h 4 C(CF 3 ) 2 C 6 h 4 NH 2 , O 3 C 2 C 6 h 3 C(CF 3 ) 2 C 6 h 3 C 2 o 3 wait; [0005] (c) Manufacture of optical glass, surface protection layer of microelectronic circuit board...

Claims

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Application Information

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IPC IPC(8): C07C45/61C07C49/167
Inventor 应德雄粟小理江建安周荣明陆斌沈恩刘伯南
Owner SHANGHAI 3F NEW MATERIAL TECH CO LTD
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