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Preparation method of perfluorethyl isopropyl ketone

A technology of ethyl isopropyl ketone and perfluoroalkene, which is applied in the field of preparation of perfluoroethyl isopropyl ketone, can solve problems such as complex process, achieve high reaction selectivity and conversion rate, enhance industrial application value, and react The effect of mild conditions

Inactive Publication Date: 2013-03-27
CHINESE PEOPLES ARMED POLICE FORCE ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The characteristic of this reaction is that starting from the readily available hexafluoropropylene dimer, the reaction yield is high, but due to the different reactivity of different epoxides in catalytic rearrangement, it needs to go through stages such as oxidation, separation, rearrangement, and purification. In order to obtain the target product, the process is too complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 0.005mol KF, 0.01mol benzyltriethylammonium bromide and 100mL acetonitrile into the flask, then add 0.01mol perfluoro-4-methyl-2-pentene into the reaction system and stir for 4h. After separation and purification, the analysis found that perfluoro-4-methyl-2-pentene had been converted into perfluoro-2-methyl-2-pentene, and the conversion rate of the reaction was 99.4%.

[0021] Add 70 mL of NaClO solution and 10 mL of diethylene glycol dimethyl ether into a three-necked flask, then add 15 g of the above-mentioned perfluoro-2-methyl-2-pentene and continue stirring for 4 h. After separation and purification, analysis found that 99.6% of perfluoro-2-methyl-2-pentene had been converted into perfluoro-2,3-epoxy-2-methylpentane.

[0022] In order to remove a small amount of perfluoro-2-methyl-2-pentene in perfluoro-2,3-epoxy-2-methylpentane, the fluorine phase can be washed with water and washed with anhydrous MgSO 4 After drying, perfluoro-2-methyl-2-pentene was removed...

Embodiment 2

[0025] Add 0.005mol KF, 0.005mol 18-crown-6-ether and 100mL acetonitrile into a three-necked flask, then add 30g hexafluoropropylene dimer mixture and keep stirring for 4h. Another 140 mL of NaClO solution was added into the reaction system, and the stirring was continued for 4 h. After separation and purification, the analysis found that the conversion rate of perfluoro-4-methyl-2-pentene was 95.4%, and the content of perfluoro-2,3-epoxy-2-methylpentane in the epoxidized product It is 96.3%, and the remaining components are mainly perfluoro-4-methyl-2-pentene, and the content of active component perfluoro-2-methyl-2-pentene is extremely low.

[0026] Add 0.005 mol of CsF, 0.01 mol of benzyltriethylammonium bromide and 50 mL of ethylene glycol dimethyl ether into the flask, then add the perfluoro-2,3-epoxy-2-methylpentane prepared above Stirring was continued for 10h. After separation and purification, analysis revealed that perfluoro-2,3-epoxy-2-methylpentane had been quant...

Embodiment 3

[0028] Add 70mL of NaClO solution, 10mL of acetonitrile and 2.75g of hydrotalcite into a three-necked flask, then add 15g of perfluoro-2-methyl-2-pentene and keep stirring for 4h. After separation and purification, analysis revealed that perfluoro-2-methyl-2-pentene had been quantitatively converted into perfluoro-2,3-epoxy-2-methylpentane.

[0029] Add 0.005 mol KF, 0.01 mol dodecyldimethylbenzyl ammonium chloride, and 50 mL acetonitrile into the flask, then add perfluoro-2,3-epoxy-2-methylpentane prepared above and continue Stir for 10h. After separation and purification, analysis revealed that perfluoro-2,3-epoxy-2-methylpentane had been quantitatively converted into perfluoroethyl isopropyl ketone.

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Abstract

The invention provides a preparation method of perfluorethyl isopropyl ketone. The preparation method specifically comprises the step of: with a hexafluoropropylene dipolymer mixture and perfluo-4-methyl-2-amylene or perfluo-2-methyl-2-amylene as raw materials, carrying out reaction processes such as olefin epoxidation, structural rearrangement of epoxide to prepare the perfluorethyl isopropyl ketone. An aprotic polar solvent, a catalyst and a phase transfer catalyst are used in a preparation process, high selectivity and high transformation rate of all steps of reactions are realized, and after a reaction mixture is simply separated so that an intermediate and a perfluorethyl isopropyl ketone product with high quality can be obtained. Meanwhile, a one-pot technology of double bond isomerization and epoxidation reaction is established. The preparation method provided by the invention has the characteristics that raw materials are easily available, the cost is low, reaction conditions are mild, operation is safe and simple, reaction selectivity and transformation rate are high, little environment influence is low; therefore, the preparation method is suitable for industrial application.

Description

technical field [0001] The invention relates to a preparation method of perfluoroethyl isopropyl ketone, especially a mixture of hexafluoropropylene dimers (mainly composed of perfluoro-4-methyl-2-pentene and perfluoro-2-methyl -2-pentene), perfluoro-4-methyl-2-pentene or perfluoro-2-methyl-2-pentene as raw materials for the preparation of perfluoroethyl isopropyl ketone. Background technique [0002] Perfluoroethyl isopropyl ketone is also known as dodecafluoro-2-methylpentan-3-one, referred to as fluorinated hexanone, and its molecular formula is CF 3 CF 2 C(O)CF(CF 3 ) 2 , CAS number 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, and is convenient for storage and transportation And a series of advantages such as wide application r...

Claims

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Application Information

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IPC IPC(8): C07C49/167C07C45/55
Inventor 杜建科王平乙华郝琪陈智伟
Owner CHINESE PEOPLES ARMED POLICE FORCE ACAD
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