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Preparation method of hexafluoropropylene dimer

A technology of hexafluoropropylene dimer and hexafluoropropylene, which is applied in the field of preparation of hexafluoropropylene dimer, and can solve the problems of high price, insoluble, low catalytic efficiency and the like

Inactive Publication Date: 2012-06-20
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] The above-mentioned catalysts all have some disadvantages, such as metal fluoride and metal hydrofluoride catalysts are easy to absorb water and reduce the catalytic efficiency, and they are difficult to dissolve in organic solvents such as acetonitrile, so that the oligomerization reaction needs to be carried out at a higher temperature and a higher pressure. Only when expensive and highly toxic crown ether is added as a cocatalyst can the reaction be carried out at room temperature; although cyanide compounds can make hexafluoropropylene oligomerization at a lower temperature as a catalyst, the catalytic The by-products of the reaction are highly toxic substances, which pose a huge threat to environmental safety
Therefore, from the perspectives of energy saving, economy and environmental safety, the above catalytic systems are not suitable for the production of dimers of hexafluoropropylene

Method used

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  • Preparation method of hexafluoropropylene dimer
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  • Preparation method of hexafluoropropylene dimer

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[0026] The invention discloses a preparation method of hexafluoropropylene dimer, comprising the following steps:

[0027] The complex formed by cuprous halide and nitrogen-containing ligand is used as a catalyst, and an aprotic polar solvent is used as a medium to carry out oligomerization reaction of hexafluoropropylene to obtain hexafluoropropylene dimer.

[0028] According to the present invention, the above-mentioned step of oligomerizing hexafluoropropylene is as follows: step a) adding a catalyst and an aprotic polar solvent into the reaction kettle, freezing, and the catalyst is formed by cuprous halide and a nitrogen-containing ligand. Complex; step b) under the protection of nitrogen, feed hexafluoropropylene into the reaction kettle, and obtain a dimer of hexafluoropropylene after oligomerization. The oligomerization reaction of the above-mentioned hexafluoropropylene is shown in the following reaction formula:

[0029]

[0030] The catalyst is the key to the ol...

Embodiment 1

[0043] Fully grind 0.10 gram of cuprous bromide and 0.23 gram of 2,2'-bipyridine to obtain a complex formed by cuprous bromide and 2,2'-bipyridine;

[0044] Add the complex and 3 milliliters of acetonitrile into the autoclave, and freeze;

[0045] After the autoclave was evacuated / nitrogen circulated for 3 times, 17.8 grams of hexafluoropropylene gas was introduced, and the reaction was stopped after 1.5 hours at 20 ° C. The unreacted hexafluoropropylene was recovered, and the colorless product in the lower layer was separated to obtain 14.8 g of hexafluoropropylene dimer.

[0046] like figure 1 Shown, for the hexafluoropropylene dimer prepared in this example 19 F NMR spectrum, the yield based on hexafluoropropylene is 83.1%, and the hexafluoropropylene dimer with the structure of formula I(a) accounts for 95.7%.

Embodiment 2

[0048] Fully grinding 0.05 gram of cuprous bromide and 0.12 gram of 2,2'-bipyridine to obtain a complex formed by cuprous bromide and 2,2'-bipyridine;

[0049] Add the complex and 3 milliliters of acetonitrile into the autoclave, and freeze;

[0050] After the autoclave was evacuated / nitrogen circulated for 3 times, 16.7 grams of hexafluoropropylene gas was introduced, and the reaction was stopped after 1.5 hours at 20 ° C. The unreacted hexafluoropropylene was recovered, and the colorless product in the lower layer was separated to obtain 11.4 grams of hexafluoropropylene dimer, the yield based on hexafluoropropylene is 68.4%, and the hexafluoropropylene dimer with the structure of formula I(a) accounts for 95%.

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Abstract

The invention discloses a preparation method of hexafluoropropylene dimmer. The method comprises the following steps that: complexes formed by cuprous halide and nitrogen-containing ligands are used as catalysts, aprotic polar solvents are used as media, hexafluoropropylene is subjected to oligomerization, and the hexafluoropropylene dimmer is obtained. Because the hexafluoropropylene is an electron-lack monomer and can be activated by the cuprous halide complexed by the nitrogen-containing ligands, so the dimerization reaction is carried out, the complexes formed by cuprous halide and nitrogen-containing ligands are used as the catalysts, and the hexafluoropropylene dimmer is obtained through preparation. Compared with the prior art, the preparation method provided by the invention has the advantages that an environmental-friendly catalyst system is adopted for preparing the hexafluoropropylene dimmer, the adoption of a high-toxicity catalytic system is avoided, the catalyst consumption is low, and the reaction temperature is low.

Description

technical field [0001] The invention relates to the technical field of hexafluoropropylene dimer, and more specifically, relates to a preparation method of hexafluoropropylene dimer. Background technique [0002] Hexafluoropropylene dimer (HFPD) produced by oligomerization of hexafluoropropylene (HFP) usually contains three isomers, as shown in formula I(a), formula I(b) and formula II respectively. Wherein, formula I (a) and formula I (b) are cis-trans isomers, its double bond activity is lower, thermal stability and chemical stability are better, toxicity is lower, can directly be used as blowing agent, fire extinguishing agent and other end products, and can be converted into isomers shown in formula II under certain conditions. The isomer represented by formula II is generally not used directly, but its double bond is more active and can undergo nucleophilic addition reactions with many reagents, and is widely used in the preparation of fluorine-containing surfactants. ...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/26
Inventor 白如科鲁丹董其宝王浦澄刘磊
Owner UNIV OF SCI & TECH OF CHINA