Synthesis method and application of perfluoro(2-methyl-3-pentanone)

A technology of perfluorohexanone and a synthesis method is applied in the field of synthesis of perfluorohexanone, and can solve the problems of complex production process of perfluorohexanone, influence on the purity of perfluorohexanone finished product, low relative volatility of perfluorohexanone, etc. , to achieve the fire-extinguishing effect of green environmental protection, good fire-extinguishing effect, and the effect of improving yield and purity

Inactive Publication Date: 2017-11-24
航天康达(北京)科技发展有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

At the same time, the relative volatility of the organic solvent used in the production process and perfluorohexanone is relatively small, and it is not easy to separate, which seriously affects the purity of the finished product of perfluorohexanone
[0004] Since perfluorohexanone is a new generation of halon substitute, the research significance of its production process and product separation and purification is relatively high, but in the prior art, the production process of perfluorohexanone is relatively complicated, the loss rate is high, and the yield and low purity

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  • Synthesis method and application of perfluoro(2-methyl-3-pentanone)
  • Synthesis method and application of perfluoro(2-methyl-3-pentanone)

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[0018] The synthesis method of perfluorohexanone in this embodiment may include the following steps: mixing hexafluoropropylene dimer with a solvent, cooling to 13-17° C., adding an oxidizing agent, performing an oxidation reaction, and collecting the reaction product with the largest specific gravity. Preferably, the substances in the oxidation reaction can be statically separated and separated, and the lower layers are collected to obtain perfluoroepoxides.

[0019] As an option, the above-mentioned solvent may be selected from at least one of aprotic polar solvents, such as acetonitrile and dimethylformamide. The oxidizing agent includes hypochlorite solution, preferably, the hypochlorite solution may include sodium hypochlorite solution and calcium hypochlorite solution. The mass concentration of active chlorine in the hypochlorite solution is 8-12%, so that the hexafluoropropylene dimer can be fully oxidized.

[0020] Preferably, sodium hypochlorite solution is used as t...

Embodiment 1

[0039] Mix 90 kg of acetonitrile, 3 kg of tetramethylethylenediamine, and 1 kg of a mixture of sodium fluoride and cesium fluoride, blow in nitrogen gas, and react with stirring at 35° C. for 1.2 h to obtain a yellow catalyst solution. Then add 18 kilograms of hexachloropropene per hour in the catalyst solution, adding 90 kilograms of hexachloropropene in total. React under the conditions of 30°C and 0.1MPa, stand still for 6min every 0.8h, collect the lower layer, and obtain a hexafluoropropylene dimer containing perfluoro-2-methyl-2-pentene with a purity of 88%.

[0040] Add 250 kg of the above-mentioned hexafluoropropylene dimer and 40 kg of dimethylformamide into the reaction kettle, stir and cool to 13°C, then add 500 kg of calcium hypochlorite solution dropwise for 7.5 hours . Wherein, the mass concentration of active chlorine contained in the calcium hypochlorite solution is 8%. Adjust the temperature of the reaction system after adding the calcium hypochlorite soluti...

Embodiment 2

[0043] Mix 100 kilograms of acetonitrile, 5 kilograms of tetramethylethylenediamine and 3 kilograms of potassium hydrofluoride, phosphorus pentafluoride and sulfur tetrafluoride mixture, feed nitrogen, and stir the reaction at 45 ° C for 0.8 h, to obtain a yellow catalyst solution. Then add 22 kilograms of hexachloropropene per hour in the catalyst solution, adding 110 kilograms of hexachloropropene in total. React under the conditions of 40°C and 0.15MPa, stand still for 4min every 1.2h, collect the lower layer, and obtain a hexafluoropropylene dimer containing perfluoro-2-methyl-2-pentene with a purity of 90%.

[0044] Add 130 kg of the above-mentioned hexafluoropropylene dimer to the reactor, then add 90 kg of acetonitrile and dimethylformamide mixture, 3 kg of 15-crown-5 amine and 0.8 kg of powdered potassium fluoride , The reaction was stirred at 40° C. for 15 h. After standing still for 15 min, the lower layer was collected to obtain perfluoro-2-methyl-2-pentene with a...

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Abstract

The invention relates to a synthesis method and application of perfluoro(2-methyl-3-pentanone), and belongs to the technical field of organic synthesis. The synthesis method comprises the following steps: mixing perfluoro(4-methylpent-2-ene) with a solvent; cooling to 13-17 DEG C; adding an oxidant; collecting a reaction product with the largest specific gravity to obtain a perfluoroepoxide; isomerizing the perfluoroepoxide in the presence of the solvent and an amine catalyst; collecting a reaction product with the largest specific gravity; and rectifying and collecting rectification products having a boiling point of 48 to 50 DEG C to obtain the perfluoro(2-methyl-3-pentanone), wherein the solvent comprises acetonitrile and / or dimethylformamide. The synthesis method has the advantages of simple process and relatively high product purity and synthesis yield; the synthesized perfluoro(2-methyl-3-pentanone) can be used as a fire extinguishing agent for fire extinguishing, and is good in fire extinguishing effect, green and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, and in particular to a synthesis method and application of perfluorohexanone. Background technique [0002] Perfluorohexanone is a new type of halon substitute. Its ODP value is 0 and GWP value is 1. It is a green environmental protection compound and has almost zero harm to the environment and human body. It is a colorless liquid at room temperature and is easy to vaporize. , normal temperature and pressure, easy to store, the heat of evaporation is only 1 / 25 of that of water, and has a strong heat absorption capacity. It can be used for physical fire extinguishing, with excellent fire extinguishing performance, suitable for protecting compact and valuable equipment. When used as a clean fire extinguishing agent, it does not belong to dangerous goods, does not leave residue after release, and is convenient for transportation. [0003] In the production process of perfluorohexanone, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/167C07C45/58C07D303/48C07D301/03A62D1/08
CPCC07C45/58A62D1/0028C07D301/03C07D303/48C07C49/167
Inventor 苗广州
Owner 航天康达(北京)科技发展有限公司
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