Synthetic method of perfluoropolyether

A technology of perfluoropolyether and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of high cost, high degree of danger, complex process of metal hydride, etc., and achieve the effects of avoiding the use of diluent, low cost and simple process

Active Publication Date: 2013-06-12
湖南有色郴州氟化学有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are two main production technologies of perfluoropolyether. One is the photo-oxidative polymerization technology of tetrafluoroethylene or hexafluoropropylene. Although the production cost of this production technology is low, the process is complicated and the risk is high; the other is The first is perfluoroepoxide, such as the anionic polymerization method of hexafluoropropylene oxide or tetrafluorooxetane. This method has a simple and safe production process and is currently a widely used production method. However, its reaction conditions are Such as raw material purity, reaction temperature and material viscosity all have influence on raw material conversion rate, the average molecular weight of polymer

Method used

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preparation example Construction

[0018] The invention provides a kind of synthetic method of perfluoropolyether, comprising:

[0019] A) react the first volume part of purified hexafluoropropylene oxide gas with alkali metal fluoride in an aprotic solvent at 0°C to 50°C to obtain an oligomer;

[0020] B) Lower the temperature of the oligomer obtained in step A) to -40°C to -20°C, add the second volume part of purified hexafluoropropylene oxide gas to it, and react to obtain perfluoropolyether.

[0021] The present invention adopts a synthesis process of feeding materials and temperature control in stages to prepare perfluoropolyether. Firstly, the first volume part of purified hexafluoropropylene oxide gas and alkali metal fluoride are carried out in an aprotic solvent at 0°C to 50°C. Reaction to obtain oligomers; then lower the temperature of the obtained oligomers to -40°C to -20°C, add the second volume of purified hexafluoropropylene oxide gas to it, and react to obtain perfluoropolyether, so that six Th...

Embodiment 1

[0033] The raw material hexafluoropropylene oxide gas is passed into two groups of adsorption towers filled with purifying agents, wherein the first group of adsorption towers is filled with aluminum hydroxide, and the second group of adsorption towers is filled with silica gel; when the pressure in the adsorption tower rises to 0.2 At MPa, discharge the purified hexafluoropropylene oxide gas from the end of the adsorption tower at a gas velocity of 4L / h. After stabilizing for 2 hours, the gas purification in the tower reaches an equilibrium state. After testing, the purified hexafluoropropylene oxide gas is , the acid gas content is 0.01wt%, the water content is 5ppm, and the hexafluoroacetone content is 0.006wt%.

[0034] Under the protection of high-purity nitrogen, 10g of cesium fluoride powder and 200g of tetraethylene glycol dimethyl ether, which have been strictly dewatered, were quickly added to a 2L stainless steel reaction kettle, and then the reaction kettle was seal...

Embodiment 2

[0036] The raw material hexafluoropropylene oxide gas is passed into two groups of adsorption towers filled with purifiers, wherein the first group of adsorption towers is filled with soda lime, and the second group of adsorption towers is filled with silica gel; when the pressure in the adsorption tower rises to 0.1MPa , discharge the purified hexafluoropropylene oxide gas from the end of the adsorption tower at a gas velocity of 4L / h. After stabilizing for 2 hours, the gas purification in the tower reaches an equilibrium state. After testing, in the purified hexafluoropropylene oxide gas, The acid gas content is 0.06wt%, the water content is 0.5ppm, and the hexafluoroacetone content is 0.004wt%.

[0037] Under the protection of high-purity nitrogen, 12g of cesium fluoride powder and 160g of tetraethylene glycol dimethyl ether, which have been strictly dewatered, were quickly added to a 2L stainless steel reaction kettle, and then the reaction kettle was sealed and the system ...

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Abstract

The invneiton discloses a synthetic method of perfluoropolyether. The synthetic method comprises the following steps of: reacting a first volume part of purified hexafluoropropylene gas and alkali metal fluoride in an aprotic solvent at 0 DEG C to 50 DEG C to obtain low polymer; cooling the temperature of the obtained low polymer to the range of -40 DEG C to -20 DEG C, and adding a second volume part of purified hexafluoropropylene gas for reaction with the low polymer to obtain perfluoropolyether. According to the synthetic method of perfluoropolyether disclosed by the invention, the synthetic process for feeding materials and controlling temperature in stages is adopted to prepare perfluoropolyether, so that the conversion rate of hexafluoropropylene reaches 99% and above; moreover, the prepared perfluoropolyether has high average molecular weight. Besides, the material hexafluoropropylene gas is purified by using alkali substances and silica gel, so that the used alkali substance and silica gel are low in cost and can be repeatedly used while the material gas reaches the using requirements. Meanwhile, in the process of synthesizing perfluoropolyether, the use of diluents is avoided, so that the process is simple and the cost is lower, therefore, the synthetic method is suitable for industrial application.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a method for synthesizing perfluoropolyether. Background technique [0002] Perfluoropolyether is a colorless and transparent perfluoropolymer material. Compared with the molecular structure of ordinary polyether, perfluoropolyether replaces the C-H bond with the C-F bond, and the strong electronegative fluorine atom makes the attraction between the molecules smaller and has a smaller surface tension; The shielding effect of the chain makes it heat-resistant, oxidation-resistant, corrosion-resistant, radiation-resistant and non-combustible. High molecular weight perfluoropolyether has low volatility, wide liquid temperature range and excellent viscosity-temperature characteristics after stabilization treatment. It is used as an excellent lubricant in aerospace industry, electronics industry, electrical industry and nuclear industry, etc. field. [0003] At present, t...

Claims

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Application Information

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IPC IPC(8): C08G65/24C07D303/48C07D301/32
Inventor 周济苍洪满贵敖明喻京鼎
Owner 湖南有色郴州氟化学有限公司
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