Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing fluorine-containing vinyl ether

A vinyl ether and fluorine-containing carboxylate technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve environmental problems, waste of solvents and catalysts, and the inability to eliminate tetrafluoroethyl ether, etc. problems, to achieve the effect of high yield and easy recycling

Active Publication Date: 2010-03-03
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
View PDF3 Cites 20 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of this patented method is further improved, up to 96%, but there are also the following problems: 1) the method is suitable for preparing perfluorovinyl ethers with lower boiling points, but not suitable for preparing perfluorovinyl ethers with high boiling points ,E.g n≥1; 2) the generation of hydrogen-containing tetrafluoroethyl ether cannot be eliminated; 3) the method is to K 2 CO 3 or Na 2 CO 3 There are very strict requirements on the water content of solvents and catalysts. It is difficult to recycle the solvents and catalysts after the reaction, resulting in a large amount of waste of solvents and catalysts, causing environmental problems

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing fluorine-containing vinyl ether
  • Method for preparing fluorine-containing vinyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The experimental device is a 250ml stainless steel reaction kettle with a condensing reflux device and stirring. Place the reaction kettle in a cold trap, add 150ml of 20wt% KOH aqueous solution, and slowly drop in perfluoro-2-methoxypropionyl under vigorous stirring Fluorine 50g (chromatographic analysis purity 99%), the reaction temperature is -10 ° C, the reaction time is 30 minutes, the reaction product is dried in vacuum at 90 ° C to obtain 75 g of dry solids, and the water content is less than 20 ppm.

[0027] Put the dried solid into a 250ml stainless steel reaction kettle with a decompression condensation recovery device and a thermometer, and dry it for 12 hours at a temperature of 100°C and an absolute pressure of 50mmHg, and then raise the temperature to 220°C for cracking 1 After 1 hour, 31 g of the product was collected by the condenser under reduced pressure, and the content of perfluoromethyl vinyl ether was 70.6% according to chromatographic analysis.

Embodiment 2

[0029] The experimental device is a 250ml stainless steel reaction kettle with a condensing reflux device and a stirrer, the reaction kettle is placed in a cold trap, and 35g of K is added 2 CO 3 80 g of perfluoro-2-propoxypropionyl fluoride (chromatographic analysis purity 99%) was slowly added dropwise under vigorous stirring, the reaction temperature was -30°C, and the reaction time was 20 min. The reaction product was separated by centrifugation, and then the water and solvent were dried in vacuum at 90° C. to obtain 106 g of dry solid, and the measured water content was less than 10 ppm.

[0030] Put the dried solid into a 250ml stainless steel reaction kettle with a decompression condensation recovery device and a thermometer. Dry it for 12 hours at a temperature of 100°C and an absolute pressure of 50mmHg, then raise the temperature to 210°C and keep it warm for 1.5 hours. 53g of the product was collected by the condenser under high pressure, and the content of perfluo...

Embodiment 3

[0032] The experimental device is a 250ml stainless steel reactor with a condensing reflux device and stirring, the reactor is placed in a cold trap, and 20g of K is added 2 CO 3 And 150ml of F113, slowly drop into 80g of perfluoro-2-propoxypropionyl fluoride (chromatographic analysis purity 99%) under vigorous stirring, and react for 30 minutes at a reaction temperature of 40°C. After the reaction was completed, the solid was separated by centrifugation, and the water and solvent were dried at 90° C. under vacuum to obtain 107 g of dry solid.

[0033]Transfer the dry solid into a 250ml stainless steel reaction kettle with a decompression condensation recovery device and a thermometer. Dry it for 12 hours at a temperature of 100°C and an absolute pressure of 50mmHg, then raise the temperature to 190°C, keep it warm for 2 hours, and depressurize. 56g of the product was collected by the condenser under the conditions, and the content of perfluoro-n-propyl vinyl ether was 78.5% ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a method for preparing fluorine-containing vinyl ether, which comprises the following steps: 1) reacting a fluorine-containing acyl fluoride shown as formula (shown on the right) and an alkali metal salt / an alkali metal hydroxide in a solvent to prepare a corresponding fluorine-containing carboxylate, wherein Rfx is a fluorine-containing alkane radical which contains perfluorobenzene, O, Br, Cl or I; the weight ratio of the fluorine-containing acyl fluoride to the alkali metal salt / the alkali metal hydroxide is 1:2-3; 2) separating and drying the fluorine-containing carboxylate; and 3) thermally cracking the dried fluorine-containing carboxylate to prepare the fluorine-containing vinyl ether shown in a formula Rfx-O-CF=CF2. The method for preparing the fluorine-containing vinyl ether is suitable for preparing the fluorine-containing vinyl ether with either low boiling point or high boiling point; and the prepared fluorine-containing vinyl ether does not containharmful by-product, namely hydrogen-containing tetrafluoroethane ether, and the subsequent purification cost of a product is reduced greatly.

Description

technical field [0001] The invention belongs to the field of fluorine-containing fine chemistry. In particular, it relates to a preparation method of fluorine-containing vinyl ether. Background technique [0002] Fluorine-containing vinyl ether is an important fluorine-containing fine chemical. It can be copolymerized with other monomers for preparing fluoropolymers to prepare materials such as fluororesins and fluororubbers that have special properties and can be used under special conditions. [0003] Fluorinated vinyl ethers can be composed of Structured fluorine-containing fluoride preparations, such as etc., there are many patents and documents reporting this preparation method, and some documents believe that the basic principle of using fluorine-containing acyl fluoride to prepare the corresponding ether is: perfluoroacyl fluoride first reacts with a salt-forming agent to generate a perfluorocarboxylate, and then Sodium carbonate is an example, and its salt-formi...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/17C07C43/225C07C41/18
Inventor 张鸣孙凌云杨旭仓石彩霞彭孝凤柏荣屈均
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD