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A kind of fluorination process containing 1,3-dioxolane ester or 1,3-dioxane ester perfluorinated compound

A technology for dioxane and dioxolane, which is applied in the field of perfluorinated compound synthesis, can solve the problems of low purity and yield, difficult process control and the like, and achieves simple method, low cost and high yield Effect

Active Publication Date: 2020-01-03
BARUCH MATERIALS (SHENZHEN) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The fluorination process using mercury and silver fluoride as a catalyst requires a large amount of highly toxic chemicals, the process is difficult to control, and the purity and yield are low

Method used

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  • A kind of fluorination process containing 1,3-dioxolane ester or 1,3-dioxane ester perfluorinated compound
  • A kind of fluorination process containing 1,3-dioxolane ester or 1,3-dioxane ester perfluorinated compound
  • A kind of fluorination process containing 1,3-dioxolane ester or 1,3-dioxane ester perfluorinated compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Dissolve 150 grams of 2,4,5-trimethyl-1,3-dioxolane-2-acid methyl ester and 6 grams of perfluorooctanesulfonic acid in 300 milliliters of FC-75, and fully stir to form a raw material solution. Add 2.5 liters of FC-75 and 15 grams of cobalt trifluoride into a 5-liter nickel reactor, stir well and keep it at minus 10 degrees, and the temperature of the condenser is minus 20 degrees. Pass nitrogen gas for one hour to drive away the air in the reaction system, then pass 20% fluorine gas (diluted with nitrogen) at a rate of 0.5L / min for half an hour, then slowly increase the flow rate of fluorine gas to 0.8L / min, and within 30 hours Inject the raw material solution. The temperature of the reaction system was maintained at minus 10 degrees. After the injection of the raw material solution, keep the flow rate of the fluorine gas constant, and continue to pass the fluorine gas for half an hour. After the reaction was finished, the product was discharged from the discharge val...

Embodiment 2

[0069] Dissolve 200 grams of 2-methyl-1,3-dioxolane-2-acid methyl ester and 8 grams of perfluorononanoic acid in 300 milliliters of FC-75, and fully stir to form a raw material solution. Add 2.5 liters of FC-75 and 20 grams of cobalt trifluoride into a 5-liter nickel reactor, stir well and keep it at minus 15 degrees, and the temperature of the condenser is minus 30 degrees. Pass nitrogen for one hour to drive away the air in the reaction system, then pass in 20% fluorine gas (diluted with nitrogen) for half an hour at a rate of 0.5L / min, then slowly increase the flow rate of fluorine gas to 1L / min, and inject it within 30 hours raw material liquid. The temperature of the reaction system was maintained at minus 15 degrees. After the injection of the raw material solution, keep the flow rate of the fluorine gas constant, and continue to pass the fluorine gas for half an hour. After the reaction, the product was discharged from the discharge valve, and after the crude product ...

Embodiment 3

[0071] Dissolve 120 grams of 2,4,6-trimethyl-1,3-dioxane-2-oic acid methyl ester and 15 grams of perfluorooctane sulfonic acid in 300 ml of FC-75, stir well to form raw materials liquid. Add 2.5 liters of FC-75 and 15 grams of cobalt trifluoride into a 5-liter nickel reactor, stir well and keep it at zero degrees, and the temperature of the condenser is minus 20 degrees. Pass nitrogen for one hour to drive away the air in the reaction system, then pass in 20% fluorine gas (diluted with nitrogen) for half an hour at a rate of 0.5L / min, then slowly increase the flow rate of fluorine gas to 1L / min, and inject it within 30 hours raw material liquid. The temperature of the reaction system was maintained at zero degrees. After the injection of the raw material solution, keep the flow rate of the fluorine gas constant, and continue to pass the fluorine gas for half an hour. After the reaction, the product is discharged from the discharge valve, and the crude product is obtained by...

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Abstract

The invention provides a fluorination process of 1,3-dioxolame ester or 1,3-dioxane ester containing perfluorinated compounds. The process comprises the following steps of putting a first fluorinationsolvent and a catalyst into a reaction kettle, wherein the catalyst is selected from one or several of boron trifluoride, cobalt trifluoride, bismuth trifluoride and arsenic trifluoride; dissolving ahydrocarbon substrate and a surfactant in a second fluorination solvent to obtain a raw material solution, wherein the surfactant is selected from one or several of perfluorononanoic acid, perfluorooctane sulfonate and tetrabutylammonium fluoride, and the hydrocarbon substrate is of a structure of a formula (I) or a formula (II); performing fluorination reaction on the raw material liquid and fluorine gas in the reaction kettle to obtain the perfluorinated compounds. In the specific fluorine-containing solvent, the low-cost hydrocarbon compounds are used as starting raw materials; the specialfluorine-containing surfactants and catalysts are used as the assistance so that the fluorine gas and the raw materials are in direct contact to be converted into the perfluorinated compounds. The method is simple; the cost is low; meanwhile, the yield is high.

Description

technical field [0001] The invention relates to the technical field of synthesis of perfluorinated compounds, in particular to a fluorination process for perfluorinated compounds containing 1,3-dioxolane esters or 1,3-dioxane esters. Background technique [0002] Perfluorinated compounds, because of their unique chemical properties, biological activity and biological adaptability, are widely used in medicine, pesticides, special dyes, coatings, special surfactants, lubricants and other industries, and are highly irreplaceable. The industrial-grade synthesis of perfluorinated compounds has always been an important indicator of a country's high-end chemical technology. At present, there are four kinds of relatively mature technological routes, one is to use tetrafluoroethylene as the basic raw material, and use various fluorocarbon alcohols as intermediates to synthesize perfluorinated compounds with different carbon chain lengths through the method of thermal telomerization; ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/32C07D319/06
CPCC07D317/32C07D319/06
Inventor 张浩温乐乐李丹
Owner BARUCH MATERIALS (SHENZHEN) CO LTD
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