559-40-0Relevant academic research and scientific papers
Preparation method of octafluorocyclopentene
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Paragraph 0029; 0031-0032; 0034-0035; 0037, (2021/04/14)
The invention relates to a preparation method of octafluorocyclopentene, and belongs to the technical field of chemical engineering. The method comprises the following steps: (1) dissolving 1, 2-dichlorocyclopentane in carbon tetrachloride, cooling to 0-20 DEG C, introducing diluted fluorine gas, stirring, heating to 30-50 DEG C, carrying out fluorination and fluorination reaction for 1-2 hours to obtain a product, and separating and purifying to obtain 1, 2-dichlorooctafluorocyclopentane; and (2) dissolving a reductive dechlorination reagent in a dry polar solvent, stirring, protecting by protective gas, heating to 50-80 DEG C, dropwise adding the 1, 2dichlorooctafluorocyclopentane by adopting a constant-pressure dropping funnel, continuously reacting for 0.5-1.5 hours when no foam is generated, and collecting the generated gas by using a cold trap. The method is simple to operate; high-temperature and high-pressure conditions are not set, and reaction conditions are mild; and less three wastes are generated, the environmental pressure is low, and the method belongs to a green synthesis process.
Synthetic method of octafluorocyclopentene
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, (2021/01/24)
The invention relates to a synthetic method of octafluorocyclopentene, and belongs to the technical field of chemical engineering. The method comprises the following steps: dissolving perfluorocyclopentane, FeCp*2 and trifluoromethanesulfonate of alkali metal in a dry aprotic solvent, conducting stirring, conducting irradiating with a mercury lamp for 1-2 hours under the protection of protective gas to obtain a reaction product, and conducting separating and purifying to obtain octafluorocyclopentene. In the method, reactants react fully, operation is simple, reaction conditions are mild, hightemperature and high pressure are avoided, pollution discharge is easy after the reaction is finished, three wastes are few, aftertreatment is simple, the problem that many impurities are caused dueto the fact that fluorine-chlorine exchange cannot react fully is solved, the solvent can be recycled, pollution in the synthesis process is reduced, and the method is environmentally friendly and belongs to a green synthesis method.
Preparation method of halogenation cycloolefin
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Paragraph 0064; 0065, (2019/08/20)
The invention relates to a preparation method of halogenation cycloolefin and belongs to the field of chemical synthesis. According to the preparation method, in an amide or alkylamine solvent, with halogenation cycloparaffin as a raw material, a dehalogenation reaction is conducted, and the target product halogenation cycloolefin is obtained. According to the method, the reaction conditions are mild, the yield of the halogenation cycloolefin is high, dangerous reduction agents such as metal or hydrogen do not need to be used, the technology is safe and reliable, solid waste such as metal halide is not generated, and a common distillation means can be used for effective industrial separation.
Continuous chemical industry preparation method of octafluorocyclopentene
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Paragraph 0020-0054, (2019/12/25)
The invention relates to the field of fine chemical industry, in particular to a continuous chemical industry preparation method of octafluorocyclopentene. The continuous chemical industry preparationmethod comprises the steps of gas phase chlorination reaction, intermediate product purification, gas phase fluorination reaction and the like. The final product octafluorocyclopentene is obtained from easily obtained raw material cyclopentene by using a gas phase method, compared with an existing liquid phase fluorination-method technology for preparing octafluorocyclopentene, the preparation method of the octafluorocyclopentene has the advantages of cheap reaction raw materials, simplicity in reaction, no applicability to solvent, no organic waste liquid generation, short reaction time, high product yield, capability of continuous production and great prospect of industrial production.
Industrial production method for perfluorocyclopentene
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Paragraph 0042; 0049; 0053; 0054; 0056; 0057, (2018/07/07)
The invention discloses an industrial production method for perfluorocyclopentene, and belongs to the field of fine chemical intermediate synthesis. Cyclopentene, chlorine and pyridine hydrofluoride which are used as raw materials undergo high-temperature chlorination in a solvent sulfolane to obtain octachlorocyclopentene, and the octachlorocyclopentene and pyridine hydrofluoride undergo high-temperature fluorination substitution to obtain the perfluorocyclopentene. Residues obtained after the separation of the product undergo reduced pressure distillation to obtain the solvent sulfolane which can be reused. The method allows the product yield to reach 45-55%, the product content to be more than 99%, the water content to be less than 0.1% and the chloride ion content to be less than 0.1%. The method has the advantages of no pollution in the production process, green production process, high yield, simple steps, facilitation of the reduction of the production cost, high product purity, and facilitation of later application.
Industrialized production method for 1,2,3,3,4,4,5,5-octafluorocyclopentene
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Paragraph 0046-0080, (2018/07/30)
The invention discloses an industrialized production method for 1,2,3,3,4,4,5,5-octafluorocyclopentene, and belongs to the field of synthesis of fine chemical intermediates. Cyclopentene, a chlorine gas and anhydrous potassium fluoride are used as raw materials, sulfolane is used as a solvent, chlorination is performed step by step through programmed heating, and the chlorinated product and the potassium fluoride are subjected to a high-temperature substitution reaction to form the 1,2,3,3,4,4,5,5-octafluorocyclopentene. According to the method provided by the invention, kettle residues afterseparation of the product can be reused after the solvent sulfolane is distilled out under reduced pressure; and the method provided by the invention has the advantages of simple production process steps, greenness, environmental protection, a high yield and low production cost, and the obtained product has high purity and is beneficial to a later application.
Study on the Preparation of Cr-based Catalysts Doped by Zn using Sol–Gel Auto-Combustion Method and Its Application for Synthesis of 1-Chloro-2,3,3,4,4,5,5-heptafluorocyclopentene
Han, Yajun,He, Jinwei,Wu, Zhenhai,Zhou, Xiaomeng
, p. 1128 - 1138 (2017/10/31)
High-surface-area chromium-based catalysts in the presence of a small amount of zinc were prepared via a sol–gel auto-combustion method using chromic nitrate, zinc nitrate, and citric acid. First, the auto-combustion behavior of the dried gel was investigated by derivative thermogravimetry and (DTG)-TG and infrared (IR) techniques. The results revealed that the dried gel exhibited self-propagating combustion properties. Second, the as-burnt powders were characterized by IR, X-ray diffraction (XRD), Brunauer–Emmett–Teller analysis (BET), and scanning electron microscopy (SEM). The findings showed that the gels were directly converted into CrZn-O nanoparticles with high surface area during the auto-combustion process. Third, the pre-fluorination Cr-Zn catalysts were characterized by XRD, BET, SEM, X-ray photoelectron spectroscopy (XPS), and Fourier transform (FT)-IR spectroscopy of pyridine adsorption techniques. It was found that the presence of zinc led to significant structural changes in the catalyst, the particle size was smaller, the surface area became larger, and more active sites appeared. Finally, the catalytic activities of the samples were tested for the fluorination of 1,2-dichlorohexafluorocyclopentene (1,2-F6) with anhydrous hydrogen fluoride. The obtained results indicated that the pre-fluorination activated Cr-Zn catalysts prepared by this sol–gel auto-combustion method exhibited high efficiency in the synthesis of cyclic hydrofluorocarbons.
A novel strategy for synthesis of dichlorooctafluorocyclopentane and reaction mechanism investigation
Zhang, Pingli,Lu, Dayong,Zhou, Biao,Zhou, Xiaomeng
, p. 33 - 39 (2016/05/09)
A novel method was used for preparing 1,1-dichlorooctafluorocyclopentane and 1,2-dichlorooctafluorocyclopentane through the reaction of 1,2-dichlorohexafluorocyclopentene, anhydrous hydrogen fluoride, and chlorine. A series of single- and multi-component catalysts were prepared by means of impregnation and coprecipitation, respectively. The catalyst containing Fe(III), Zr(IV), Co(II), Zn(II) and Cu(II) showed the highest catalytic activity among these catalysts. Moreover, the main reaction routes and catalytic mechanism were investigated through experiments and theoretical analysis. Given the environmental and economic benefits, this method has a great application potential in industrial production.
Synthesis of 1,1,2,2,3,3,4-heptafluorocyclopentane as a new generation of green solvent
Zhang, Chengping,Qing, Feiyao,Quan, Hengdao,Sekiya, Akira
, p. 11 - 16 (2015/11/24)
1,1,2,2,3,3,4-Heptafluorocyclopentane is a new generation of green solvent. It was synthesized by the liquid-phase fluorination reactions from hexachlorocyclopentadiene to 1-chloroheptafluoro-cyclopentene in the presence of KF in DMF and by the vapor-phase hydrogenation reaction from 1-chloroheptafluorocyclopentene to 1,1,2,2,3,3,4-heptafluorocyclopentane in the presence of Pd-based hydrogenation catalyst. Quantum chemical calculations for the isomers energies using Gaussian09 were conducted to verify the chemical equilibriums between isomers of trichloropentafluorocyclopentene or dichlorohexafluorocyclopentene in the fluorination reactions. Possible mechanisms for 1,1,2,2,3,3,4-heptafluorocyclopentane synthesis were proposed.
PROCESSES FOR THE SYNTHESIS OF 3-CHLOROPERFLUORO-2-PENTENE, OCTAFLUORO-2-PENTYNE, AND 1,1,1,4,4,5,5,5-OCTAFLUORO-2-PENTENE
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Page/Page column 14-15, (2009/07/18)
Disclosed is a process comprising reacting CF3CF2CCI2CF2CF3 (CFC-41 -10mca) with hydrogen in the presence of a dehalogenation catalyst to produce CF3CF2CCI=CFCF3 (CFC-1419myx). Also disclosed herein is a process comprising reacting CF3CF2CCI=CFCF3 (CFC- 1419myx) with hydrogen in the presence of a dehalogenation catalyst to produce CF3CF2C≡CCF3 (octafluoro-2-pentyne). Also disclosed herein is a process comprising reacting CF3CF2CCI2CF2CF3 (CFC-41 -10mca) with hydrogen in the presence of a dehalogenation catalyst to produce CF3CF2C≡CCF3 (octafluoro-2-pentyne). In addition, a process for reacting CF3CF2C≡CCF3, in a pressure vessel, with a Lindlar catalyst and hydrogen to produce CF3CF2CH=CHCF3 (1,1,1,4,4,5,5,5-octafluoro-2- pentene) is disclosed.
