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A kind of preparation method of perfluoroethyl isopropyl ketone

A technology of ethyl isopropyl ketone and methyl group, applied in the field of preparation of perfluoroethyl isopropyl ketone, can solve the problems of complicated post-processing, environmental pollution and the like, and achieve the effect of saving time and improving efficiency

Active Publication Date: 2020-09-08
JIANGSU UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation technology provided by the invention has the characteristics of easy-to-obtain raw materials, low cost, mild reaction conditions, safe and simple operation, high reaction selectivity and conversion rate, and small environmental impact, and is suitable for industrial applications; but the preparation method of the invention has certain limitations. Disadvantages: It uses perfluoro-4-methyl-2-pentene or perfluoro-2-methyl-2-pentene as raw material to prepare perfluoroethyl isopropyl through steps such as epoxidation and isomerization The ketone technology inevitably requires a large amount of toxic solvents such as acetonitrile and the highly corrosive and irritating oxidizing reagent sodium hypochlorite solution, resulting in a large amount of sewage and toxic solvents in post-processing, which has the disadvantages of complex post-processing and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 1g of potassium cyanide, 5g of N-picoline, 5g of dibenzo-18-crown-6 and 50g of acetonitrile into the flask, then add 300g of perfluoro-4-methyl-2-pentene into the reaction system, The reaction was stirred at 40 °C for 20 h. After separation and purification, it was found by analysis that perfluoro-4-methyl-2-pentene was converted into perfluoro-2-methyl-2-pentene, and the conversion rate of the reaction was 97.5%.

[0034] 0.3mol (CH 3 CH 2 CH 2 ) 2 NOH, 18.5mL N, N-dimethylacetamide and 0.05mol tetrabutylphosphine bromide were added to a three-necked flask, and then 0.1mol of the above-mentioned perfluoro-2-methyl-2-pentene was added, and heated at 40°C Continue to stir the reaction for 2h. After separation and purification, analysis revealed that perfluoro-2-methyl-2-pentene had been quantitatively converted into perfluoro-2-methyl-2,3-epoxypentane.

[0035] Add 30 mL of ethylene glycol dimethyl ether, 0.2 mol of N,N-dimethylbenzylamine, and 0.1 mol of methy...

Embodiment 2

[0037] Add 2g of potassium thiocyanate, 0.7g of N,N-dimethylbenzylamine, 2g of polyethylene glycol 4000 and 30g of diethylene glycol dimethyl ether into the flask, and then add 300g of perfluoro-4-methyl-2 -Pentene was added to the reaction system, and the reaction was stirred at 90°C and 0.3MPa for 6h. After separation and purification, it was found by analysis that perfluoro-4-methyl-2-pentene was converted into perfluoro-2-methyl-2-pentene, and the conversion rate of the reaction was 99.7%.

[0038] 0.1mol (CH 3 CH 2 ) 2 NOH and 15 mL of N,N-dimethylacetamide were added into a three-necked flask, and then 0.1 mol of the above-mentioned perfluoro-2-methyl-2-pentene was added, and the reaction was continuously stirred at 70° C. for 8 h. After separation and purification, it was found by analysis that perfluoro-2-methyl-2-pentene had been converted into perfluoro-2-methyl-2,3-epoxypentane, and the conversion rate of the reaction was 98.9%.

[0039] Add 40 mL of ethylene gl...

Embodiment 3

[0041] Add 1g of antimony pentafluoride, 3g of N-picoline and 1g of 18-crown-6 into the flask, then add 300g of perfluoro-4-methyl-2-pentene into the reaction system, and stir the reaction at 120°C 25h. After separation and purification, it was found by analysis that perfluoro-4-methyl-2-pentene was converted into perfluoro-2-methyl-2-pentene, and the conversion rate of the reaction was 98.1%.

[0042] 0.3mol (CH 3 ) 2 Add NOH, 40mL N,N-dimethylacetamide and 0.03mol tetrabutylphosphine bromide into the three-necked flask, then add the above-mentioned 0.1mol of the above-mentioned perfluoro-2-methyl-2-pentene, and continue at 20°C The reaction was stirred for 8h. After separation and purification, analysis revealed that perfluoro-2-methyl-2-pentene had been converted into perfluoro-2-methyl-2,3-epoxypentane.

[0043] Add 8 mL of tetraethylene glycol dimethyl ether, 0.1 mol of tributylamine and 0.08 mol of polyethylene glycol 4000 into the flask, then add 1 mol of perfluoro-...

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PUM

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Abstract

The present invention relates to a method for preparing perfluoroethyl isopropyl ketone, comprising: using perfluoro-4-methyl-2-amylene or a mixture of perfluoro-4-methyl-2-amylene and perfluoro-2-methyl-2-amylene as a raw material; firstly, converting perfluoro-4-methyl-2-amylene into perfluoro-2-methyl-2-amylene by means of an isomerization reaction; next, epoxidizing perfluoro-2-methyl-2-amylene as perfluoro-2-methyl-2,3-pentylene oxide; and then, enabling catalytic rearrangement of perfluoro-2-methyl-2,3-pentylene oxide to obtain perfluoroethyl isopropyl ketone. The present invention has the following advantages: the catalytic isomerization reaction in the present invention can be performed in a solvent-free condition so that the problems that a great number of toxic solvents are used in existing processes, recycling is difficult to be carried out and the like are avoided; tertiary amine nitrogen oxide or N,N-dialkyl hydroxylamine is used as an epoxidation reagent, such that perfluoro-2-methyl-2-amylene is quantitatively converted into perfluoro-2-methyl-2,3-pentylene oxide under a mild condition, and thus the problems that a great number of sodium hypochlorite solutions are used in existing processes so that devices are seriously corroded, a great number of salt solutions generated in post-treatment are difficult to be recycled, the use conditions are harsh and the like are avoided.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of perfluoroketone compounds in organic fluorine chemistry, [0002] Particularly relate to a kind of preparation method of perfluoroethyl isopropyl ketone. Background technique [0003] Perfluoroethyl isopropyl ketone is also known as dodecafluoro-2-methylpentan-3-one, abbreviated as fluorinated hexanone, and its molecular formula is CF 3 CF 2 C(O)CF(CF 3 ) 2 , CAS No. 756-13-8. When perfluoroethyl isopropyl ketone is used as a fire extinguishing agent, it has low fire extinguishing concentration, high fire extinguishing efficiency, good environmental performance, low toxicity, good safety, little impact on related equipment and materials, no residue, easy storage and transportation And a series of advantages such as wide application range. While ensuring high fire extinguishing efficiency, it solves the environmental protection problems of previous fluoroalkane halon substitute...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/167C07C45/58C07C17/358C07C21/18C07D303/08C07D301/03
CPCC07C17/358C07C45/58C07D301/03C07D303/08C07C21/18C07C49/167
Inventor 蔡星伟沙敏潘仁明姜标赵玉媛
Owner JIANGSU UNIV OF SCI & TECH
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