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

A synthetic method, methyl technology, applied in the preparation of heterocyclic compounds, fire prevention equipment, organic chemistry, etc., can solve the problems of complex perfluorinated production process, low yield and purity, and affect the purity of perfluorinated, and achieve a green fire extinguishing effect Environmental protection, high product purity, good fire extinguishing effect

Inactive Publication Date: 2017-12-08
航天康达(北京)科技发展有限公司
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  • 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 perfluoro(2-methyl-3-pentanone) is small, and it is not easy to separate, which seriously affects the finished product of perfluoro(2-methyl-3-pentanone). the purity of
[0004] Since perfluoro(2-methyl-3-pentanone) is a new generation of halon substitutes, the research significance of its production process and product separation and purification is relatively high, but in the prior art, perfluoro(2-methyl-3-pentanone) 3-pentanone) production process is comparatively complicated, and loss rate is higher, and yield and purity are all lower

Method used

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

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preparation example Construction

[0018] The synthesis method of perfluoro(2-methyl-3-pentanone) of the present embodiment may comprise the following steps: under the condition that solvent and amine catalyst exist, perfluoroepoxide isomerized, and the collection specific gravity is the largest reaction product. Preferably, after the isomerization reaction, it is cooled to 0-5° C., left to stand for stratification, and then the reactant (lower layer) with the largest specific gravity is collected for rectification, and the rectification product with a boiling point of 48-50° C. is collected to obtain perfluoro( 2-methyl-3-pentanone).

[0019] As an option, the solvent mentioned above may be at least one selected from aprotic polar solvents, such as acetonitrile and 1,1,2-trichlorotrifluoroethane. Because the anion donor is usually composed of a positively charged part and a negatively charged part, in order to weaken the electric attraction force between the positively charged part and the negatively charged ...

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 acetonitrile 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 solution to -...

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] Put 130 kg of the above-mentioned hexafluoropropylene dimer into the reaction kettle, then add 90 kg of acetonitrile, 3 kg of 15-crown-5 amine and 0.8 kg of powdered potassium fluoride, and stir at 40°C Reaction 15h. After standing still for 15 min, the lower layer was collected to obtain perfluoro-2-methyl-2-pentene with a purity of 92%. Next, the perfluor...

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Abstract

The invention relates to a synthesizing method of perfluoro(2-methyl-3-pentanone) and application, and belongs to the field of organic synthesizing. The synthesizing method comprises the following steps of isomerizing perfluoro cyclic oxide under the condition of existence of solvent and amine catalyst, collecting a reaction product with maximum proportion, and rectifying, so as to obtain the perfluoro(2-methyl-3-pentanone), wherein the solvent comprises acetonitrile and/or 1,1,2-trichlorotrifluoroethane; the amine catalyst comprises at least one of N,N-dimethylcyclohexylamine, bis(2-dimethylamino ethyl)ester, N,N,N',N'-tetramethyl alkylidene diamine, triethylamine, N,N-dimethylbenzylamine, triethanolamine, and N,N'-dimethyl pyridine; the isomerizing reaction is refluxing reaction for 10 to 14h at the temperature of 48 to 52 DEG C. The synthesizing method has the advantages that the technology is simple, and the purity and synthesizing yield of the product are higher; the synthesized perfluoro(2-methyl-3-pentanone) can be used as fire extinguishing agents for fire protection and fire extinguishing, the fire extinguishing effect is good, and the green and environment-friendly effects are realized.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, and in particular to a synthesis method and application of perfluoro(2-methyl-3-pentanone). Background technique [0002] Perfluoro(2-methyl-3-pentanone) is a new type of halon substitute, its ODP value is 0, GWP value is 1, it is a green environmental protection compound, and its harm to the environment and human body is almost zero; It is a colorless liquid at normal temperature, 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/58C07C49/167C07D301/03C07D303/48A62D1/00
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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