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Method for preparing halogenated pentacyclic olefin by gas-phase isomerization reaction

A technology of isomerization and five-membered rings, which is applied in the field of gas-phase isomerization to prepare halogenated five-membered ring olefins, can solve the problem of harsh technology, environmental pollution and difficult control of trichloropentafluorocyclopentene isomers and other problems, to achieve the effect of cheap isomerization catalyst and easy-to-obtain raw materials

Active Publication Date: 2017-12-08
BEIJING YUJI SCI & TECH
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  • Abstract
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  • Claims
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Problems solved by technology

[0008] The above-mentioned method has the following defects: (1) The technology for preparing trichloropentafluorocyclopentene isomers is too harsh, and Na-Ag-Hg alloys that are difficult to control and highly toxic, or high-temperature (600° C.) Pyrolysis, or the price of fluorinating reagent xenon difluoride is too expensive; (2) the yield of preparing chlorofluorocyclopentene isomers is low, mostly around 10%; (3) most reaction routes adopt liquid phase reaction, using a large amount of organic solvents and metal fluorides, it is difficult to recycle, and it is easy to cause serious environmental pollution; in addition, the method for preparing halogenated halogenated five-membered cycloalkenes by gas phase isomerization has not been reported in the literature

Method used

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  • Method for preparing halogenated pentacyclic olefin by gas-phase isomerization reaction
  • Method for preparing halogenated pentacyclic olefin by gas-phase isomerization reaction
  • Method for preparing halogenated pentacyclic olefin by gas-phase isomerization reaction

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preparation example Construction

[0046] Preparation of isomerization catalyst: Dissolve metal soluble salt in water, drop concentrated ammonia water for precipitation, adjust pH value to 7.5, then age for 12 hours, wash with water, filter, dry in an oven at 80°C for 36 hours, and then Under the protection of nitrogen, calcined at 450° C. for 8 hours to obtain metal oxide, which is the precursor of metal fluoride carrier. According to the percentage composition of the alkali metal fluoride and the metal fluoride carrier, the composition is 0-10% and 10%-90%, and at a temperature of 50 ° C, the alkali metal fluoride is impregnated and supported on the metal oxide by impregnation, filtered, and heated at 80 ℃ and dried for 12 hours, the resulting solid was pulverized, tableted and formed to obtain a catalyst precursor, and 10 mL of the catalyst precursor was packed into a tube reactor made of Monel material with an inner diameter of 1 / 2 inch and a length of 30 cm, and nitrogen gas was passed into the reactor. Ro...

Embodiment 1

[0049] 10 milliliters of isomerization catalyst 100% CrF prepared by the above-mentioned method is filled in the tubular reactor made of Incon alloy with inner diameter 1 / 2 inch and long 30cm 3 . The reaction conditions are as follows: the reaction temperature is raised to 120° C., the contact time of 1,4-dichlorohexafluorocyclopentene is 5 s, and the reaction pressure is 0.1 MPa. After reacting for 100 hours, the reaction product was washed with water to separate the organic matter, and after drying to remove water, the composition of the organic matter was analyzed by gas chromatography. The reaction result was: the conversion rate of 1,4-dichlorohexafluorocyclopentene was 75.0%, 1, The selectivity of 3-dichlorohexafluorocyclopentene was 63.4%, and the selectivity of 1,2-dichlorohexafluorocyclopentene was 36.6%.

[0050] The above organic phase is rectified to obtain dichlorohexafluorocyclopentene isomer 1,4-dichlorohexafluorocyclopentene with a boiling point of 80-84°C (76...

Embodiment 2

[0052] 10 milliliters of isomerization catalysts 5% CsF / CrF prepared by the above method are filled in a tubular reactor made of Incon alloy with an inner diameter of 1 / 2 inch and a length of 30 cm 3 . The reaction conditions are as follows: the reaction temperature is raised to 400° C., the contact time of 1,4-dichlorohexafluorocyclopentene is 5 s, and the reaction pressure is 0.1 MPa. After reacting for 100 hours, the reaction product was washed with water to separate the organic matter, and after drying to remove water, the composition of the organic matter was analyzed by gas chromatography. The reaction result was: the conversion rate of 1,4-dichlorohexafluorocyclopentene was 100%, 1, The selectivity of 3-dichlorohexafluorocyclopentene was 0.7%, and the selectivity of 1,2-dichlorohexafluorocyclopentene was 99.3%.

[0053] The above organic phase was rectified to obtain 1,2-dichlorohexafluorocyclopentene, an isomer of dichlorohexafluorocyclopentene, with a boiling point o...

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Abstract

The invention relates to a method for preparing halogenated pentacyclic olefin by gas-phase isomerization reaction. The method comprises the following steps of: by adopting the halogenated pentacyclic olefin C5HxFyClz as a material, under the existence of an isomerization catalyst, generating the gas-phase isomerization reaction to obtain isomers of the halogenated pentacyclic olefin, wherein X is an integer from 0 to 2, Y is an integer from 4 to 7, Z is an integer from 0 to 4, the sum of X and Y and Z is 8, and the isomerization catalyst is prepared by adopting at least one of lithium fluoride, potassium fluoride, sodium fluoride, rubidium fluoride or cesium fluoride as an active component and loading the active component on at least one of carriers such as aluminium fluoride, magnesium fluoride, iron fluoride, chromium fluoride and zinc fluoride. The method has the advantages that the material is easy to obtain, the isomerization catalyst is low in price, the yield of the isomer is higher, and the method is applicable to large-scale preparation of the isomers of the halogenated pentacyclic olefin by gas-phase reaction.

Description

technical field [0001] The present invention relates to a method for preparing halogenated five-membered ring olefins by gas-phase isomerization, in particular to a method for obtaining halogenated five-membered rings through isomerization reaction of halogenated five-membered rings under the catalysis of an isomerization catalyst Process for the preparation of isomers of olefins. Background technique [0002] Halogenated five-membered cyclic olefins are extremely important chemical raw materials or intermediates. For example, 1,2-dichlorohexafluorocyclopentene, hexachlorocyclopentadiene, etc. are important fluorine-containing building blocks. Therefore, the synthesis of halogenated five-membered cycloalkenes has become one of the research focuses in the field of fluorine chemistry. [0003] The literature [Chemische Berichte; vol.117; nb.3; (1984); p.1153-1160] reported that 1,2,3,4,5-pentachloropentafluorocyclopentane was used as raw material, and Na-Ag- Hg alloy reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/358C07C23/08B01J27/128B01J27/125B01J27/138
CPCB01J27/125B01J27/128B01J27/132B01J27/138C07C17/358C07C23/08
Inventor 张呈平贾晓卿权恒道
Owner BEIJING YUJI SCI & TECH
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