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Catalyst for industrial production of fluorophosphazene and its derivatives

A technology for fluorophosphazene and derivatives, which is applied in the field of catalysts for industrial production of fluorophosphazenes and derivatives thereof, can solve the problems of difficulty in separation, increase separation and purification processes, reduce product purity, etc., and achieve mild reaction conditions and high reliability. Good operability and simple separation effect

Active Publication Date: 2019-08-02
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Since fluorophosphazene and its derivatives have good electrochemical compatibility, the inventors of the present application optimize the existing industrial production process of fluorophosphazene and its derivatives by using polyethylene glycol catalysts However, the problem of using polyethylene glycol catalysts in industrial production is: polyethylene glycol catalysts are a kind of phase transfer catalysts, which have good solubility in organic solvents and water, so that there are a large amount of polyethylene glycol in the product. Glycol catalysts, it is difficult to separate the polyethylene glycol catalysts from the product, resulting in a decrease in product purity, which not only affects the application of the polyethylene glycol catalysts in industrialization, but also cannot recover the polyethylene glycol catalysts. Utilization, if the product in the product is purified, and the polyethylene glycol catalyst is recycled, it not only needs to increase the research and development cost, but also needs to increase the separation and purification process, increasing the process cost
Although the use of polyethylene glycol catalysts can increase the yield of fluorophosphazene and its derivatives, the cost increase due to the above problems is far higher than the benefits brought by the increase in yield
As a result, the use of catalysts in the industrial production of fluorophosphazene and its derivatives has resulted in a bottleneck in the process research and development of improving the economic benefits of enterprises

Method used

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  • Catalyst for industrial production of fluorophosphazene and its derivatives

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Dissolve 34.7g of hexachlorocyclotriphosphazene crystals in 200mL of tetrahydrofuran to form a hexachlorocyclotriphosphazene solution, add 27g of sodium fluoride to the solution as a fluorinating agent, add 2g of industrial grade graphene as a catalyst, and After reacting for 10 h under temperature conditions, the phosphazene derivative hexafluorocyclotriphosphazene was obtained after filtration and vacuum distillation with a yield of 99% and a purity of 98%.

Embodiment 2

[0040] 27.5g ethoxy pentachlorocyclotriphosphazene crystals are dissolved in 200mL tetrahydrofuran to form ethoxy pentachlorocyclotriphosphazene solution, add 27g sodium fluoride as fluorinating agent in the solution, add 2g industrial grade graphene as Catalyst, reacted at 30°C for 15 hours, filtered and distilled under reduced pressure to obtain phosphazene derivative ethoxypentafluorocyclotriphosphazene with a yield of 99% and a purity of 97%.

Embodiment 3

[0042] 34.7g of hexachlorocyclotriphosphazene crystals were dissolved in 200mL of DMF to form a hexachlorocyclotriphosphazene solution, 27g of sodium fluoride was added to the solution as a fluorinating agent, 2g of graphene oxide was added as a catalyst, and at a temperature of 60°C After reacting for 5 hours under the conditions, the phosphazene derivative hexafluorocyclotriphosphazene was obtained after filtration and vacuum distillation with a yield of 99% and a purity of 98%.

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Abstract

The invention discloses a catalyst for the industrial production of fluorophosphazene and its derivatives. The catalyst is applied to a fluorination reaction of chlorophosphazene and its derivatives to prepare fluorophosphazene and its derivatives, ad the catalyst is one or a mixture of two or more of industrial grade graphene, graphene oxide, fullerene, Mxene, hydroxylated carbon nanotubes and expanded graphite. The catalyst has the advantages of simplicity in separation, increase of the purity of the products, repeated use, and reduction of the use cost.

Description

technical field [0001] The invention relates to the industrialized production of fluorophosphazene and its derivatives, in particular to a catalyst for the industrialized production of fluorophosphazene and its derivatives. Background technique [0002] Phosphazene compounds are a kind of inorganic-organic hybrid compounds whose skeletons are alternately arranged by phosphorus and nitrogen, and can be divided into cyclic phosphazenes and polyphosphazenes. Among them, chlorophosphazene is the most representative compound among cyclic phosphazene compounds, because the chlorine atom has a strong activity and is easily replaced by various nucleophiles. Therefore, using chlorophosphazene as an intermediate, fluorophosphazene and its phosphazene derivatives with various organic functional groups can be synthesized. Chlorine atoms have poor compatibility in lithium battery electrolytes, while fluorophosphazenes and their derivatives have good electrochemical compatibility. [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/18C07F9/6593H01M10/0566
CPCB01J21/18B01J21/185C07F9/65815H01M10/0566Y02E60/10
Inventor 冯金奎安永灵
Owner SHANDONG UNIV