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Method for producing fluorine compound

A manufacturing method and technology of aluminum fluoride, applied in organic chemical methods, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as reactions that are not suitable for flow-through

Active Publication Date: 2013-02-13
NAT INST OF ADVANCED IND SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Here, aluminum chlorofluoride is obtained by reacting trichlorofluoromethane (CFC-11) with aluminum chloride, but it is in powder form and is not suitable for a flow-through reaction

Method used

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  • Method for producing fluorine compound
  • Method for producing fluorine compound
  • Method for producing fluorine compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] (Manufacture of Catalyst A)

[0063] 18 ml of alumina was added to a reaction tube with a diameter of 14 mm and a length of 300 mm. Under a nitrogen flow of 100 ml / min, the reaction tube was heated to 400°C. Next, dichlorodifluoromethane (CFC-12) was passed through at 400° C. and 100 ml / min for 3 hours to obtain catalyst A. Catalyst A has a surface area of ​​72.56m 2 / g.

[0064] (Manufacture of hexafluoro-2-butyne)

[0065] Catalyst A was added to the above reaction tube. Measure hexafluoro-1,3-butadiene with a mass flow meter and pass it into the reaction tube. The reaction is carried out at 20°C to 150°C, the product passes through a dryer and online GC, and the final product is collected in a trap at -100°C.

[0066] The experimental results are shown in Table 1 below.

[0067] [Table 1]

[0068]

Embodiment 2

[0070] (Manufacture of Catalyst B)

[0071] A sufficient amount of palladium chloride solution was impregnated into the porous aluminum fluoride (PAF) overnight. The amount of metal chloride in the solution was adjusted so that the final metal loading was about 3% by weight. After impregnation, the palladium-loaded carrier was heated at 200°C for 6 hours, further heated at 300°C for 6 hours, and then reduced at 200°C for 6 hours under a flow of hydrogen gas at a flow rate of 20ml / min, and then reduced at 300°C. After 6 hours, it was further reduced at 350°C for 5 hours to obtain catalyst B.

[0072] (Manufacture of cis-1,1,1,4,4,4-hexafluoro-2-butene)

[0073] Catalyst B was added to the above reaction tube. Measure hexafluoro-2-butyne with a mass flow meter and pass it into the reaction tube. The reaction is carried out at 20°C to 250°C, the product passes through a dryer and online GC, and the final product is collected in a trap at -100°C.

[0074] The experimental res...

Embodiment 3

[0083] (Manufacture of Catalyst C)

[0084] A sufficient solution of palladium chloride and bismuth chloride was impregnated into porous aluminum fluoride (PAF) overnight. The amount of the metal chloride in the solution was adjusted so that the supporting amount of palladium became about 2% by weight and the supporting amount of bismuth became about 0.1%. The palladium-loaded carrier was heated at 200°C for 6 hours, further heated at 300°C for 6 hours, and then reduced at 200°C for 6 hours and at 300°C for 6 hours under a flow of hydrogen gas at a flow rate of 20ml / min. It was further reduced at 350° C. for 5 hours to obtain catalyst C.

[0085] (Manufacture of cis-1,1,1,4,4,4-hexafluoro-2-butene)

[0086] Catalyst C was added to the above reaction tube. Measure hexafluoro-2-butyne with a mass flow meter and pass it into the reaction tube. The reaction is carried out at 20°C to 250°C, the product passes through a dryer and online GC, and the final product is collected in ...

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Abstract

Provided is a method for producing 1,1,1,4,4,4-hexafluoro-2-butene that is efficient and appropriate for a flow-through reaction. Cis-1,1,1,4,4,4-hexafluoro-2-butene is obtained by isomerization of hexafluoro-1,3-butadiene using a catalyst and then continuous catalytic hydrogen reduction, and in addition cis-1,1,1,4,4,4-hexafluoro-2-butene can be obtained efficiently by carrying out all steps by means of a flow-through catalytic reaction.

Description

technical field [0001] The present invention relates to the method for producing cis-1,1,1,4,4,4-hexafluoro-2-butene, in particular to hexafluoro-1,3-butadiene via hexafluoro-2-butyne A method for producing cis-1,1,1,4,4,4-hexafluoro-2-butene. Background technique [0002] Generally, fluorine compounds are widely used in industries such as polymer materials, refrigerants, detergents, medicines, and pesticides. In the present invention, unsaturated fluorine compounds, especially cis-1,1,1,4,4,4-hexafluoro-2-butene are targeted, and they are also expected to be used in the above-mentioned applications. [0003] Properties such as flammability, toxicity, and stability of unsaturated fluorine compounds vary greatly depending on their structures. Cis 1,1,1,4,4,4-hexafluoro-2-butene (boiling point about 32°C) and trans 1,1,1,4,4,4-hexafluoro as geometric isomers -2-Butene (boiling point about 9° C.) greatly differs in boiling point, and an efficient production method with high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/354B01J23/44B01J23/50B01J27/10B01J27/13B01J27/32B01J38/10C07C17/358C07C21/18C07B61/00
CPCB01J21/04B01J23/644B01J37/0205B01J37/0201C07C21/18B01J35/0006C07C17/358C07C17/354B01J27/13B01J35/1014B01J23/66B01J37/0207B01J27/12B01J37/16B01J23/44B01J37/18B01J21/18B01J35/19B01J35/613C07C21/22
Inventor 权恒道田村正则水门润治关屋章
Owner NAT INST OF ADVANCED IND SCI & TECH
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