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Preparation method of 1,1,1,5,5,5-hexafluoro acetylacetone

A technology of hexafluoroacetylacetone and trifluoroacetoacetate, which is applied in the field of fluorine compound preparation, can solve the problems of environmental pollution, complicated process, and high production cost, and achieve the effects of less environmental pollution, simple process, and easy operation

Inactive Publication Date: 2011-11-30
XIAN CAIJING OPTO ELECTRICAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a preparation method of 1,1,1,5,5,5-hexafluoroacetylacetone to overcome the problems of high production cost, complex process and environmental pollution in the existing preparation process

Method used

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  • Preparation method of 1,1,1,5,5,5-hexafluoro acetylacetone

Examples

Experimental program
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Effect test

Embodiment 1

[0023] In a 1000mL three-neck flask, add 696 g (3 moles) of phenyl trifluoroacetoacetate, 210 g (1 mole) of trifluoroacetic anhydride and 1.2 g (0.03 moles) of magnesium oxide, start stirring, and heat the mixture in the bottle to 50 °C React for 8 hours; then increase the temperature and heat the mixture in the bottle to 140°C, and distill the generated 1,1,1,5,5,5-hexafluoroacetylacetone while reacting to obtain 1,1,1,5, 5,5-hexafluoroacetylacetone crude product; the resulting 1,1,1,5,5,5-hexafluoroacetylacetone crude product was rectified, and the fraction with a boiling range of 69-71°C was collected to obtain a colorless liquid 140 g, namely 1,1,1,5,5,5-hexafluoroacetylacetone, yield 67.3%.

Embodiment 2

[0025] In a 1000mL three-necked flask, add 552 g (3 moles) of ethyl trifluoroacetoacetate, 210 g (1 mole) of trifluoroacetic anhydride, and 1.2 g (0.03 moles) of magnesium oxide, start stirring, and heat the mixture in the bottle to 40 ℃ for 5 hours; then increase the temperature and heat the mixture in the bottle to 140 ℃, and distill the generated 1,1,1,5,5,5-hexafluoroacetylacetone while reacting to obtain 1,1,1,5 , 5,5-hexafluoroacetylacetone crude product; the obtained 1,1,1,5,5,5-hexafluoroacetylacetone crude product was rectified, and the fraction with a boiling range of 69-71°C was collected to obtain a colorless liquid 126 g, namely 1,1,1,5,5,5-hexafluoroacetylacetone, yield 60.5%.

Embodiment 3

[0027] In a 1000mL three-neck flask, add 738 g (3 moles) of benzyl trifluoroacetoacetate, 210 g (1 mole) of trifluoroacetic anhydride and 2 g (0.05 moles) of magnesium oxide, start stirring, and heat the mixture in the bottle to 60°C React for 10 hours; then increase the temperature to heat the mixture in the bottle to 140°C, and distill the generated 1,1,1,5,5,5-hexafluoroacetylacetone while reacting to obtain 1,1,1,5, 5,5-hexafluoroacetylacetone crude product; the obtained 1,1,1,5,5,5-hexafluoroacetylacetone crude product was rectified, and the fraction with a boiling range of 69-71°C was collected to obtain a colorless liquid 142 g, namely 1,1,1,5,5,5-hexafluoroacetylacetone, yield 68.2%.

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Abstract

The invention provides a preparation method of 1,1,1,5,5,5-hexafluoro acetylacetone. The preparation method comprises the following steps: carrying out first-stage reaction on trifluoroacetyl acetate and trifluoroacetic anhydride under the action of a catalyst at 40-60 DEG C for 5-10 hours; then raising the temperature to 120-150 DEG C for second-stage reaction, and distilling out the resulting 1,1,1,5,5,5-hexafluoro acetylacetone while reacting to obtain a crude 1,1,1,5,5,5-hexafluoro acetylacetone product; and finally purifying the crude product to obtain a refined 1,1,1,5,5,5-hexafluoro acetylacetone product. In the preparation method provided by the invention, as inexpensive trifluoroacetic anhydride and trifluoroacetyl acetate are used as raw materials for the reaction, the cost of the product is dramatically reduced; and as no acid is generated in the reaction process, the environmental pollution is low.

Description

technical field [0001] The invention belongs to the technical field of fluorine compound preparation, and in particular relates to a preparation method of 1,1,1,5,5,5-hexafluoroacetylacetone. Background technique [0002] 1,1,1,5,5,5-Hexafluoroacetylacetone is an important organic intermediate and has a wide range of applications in many fields. Hexafluoroacetylacetone combines with metals to form a metal-diketone compound. As a metal-organic precursor, it is widely used to deposit and grow various functional thin film materials, such as oxide superconducting thin films, electroluminescent thin films, ferroelectric oxide thin films, etc.; In addition, the complexes formed by hexafluoroacetylacetone and rare earth metals have good chemical stability and excellent luminescent performance, and have broad application prospects in the field of luminescence. The ternary complexes formed by hexafluoroacetylacetone and europium-terbium-gadolinium Its luminescent color changes with ...

Claims

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Application Information

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IPC IPC(8): C07C49/167C07C45/54
Inventor 高嫒嫒杜渭松胡明刚刘建韬李超群陈龙
Owner XIAN CAIJING OPTO ELECTRICAL SCI & TECH
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