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

Synthesis method of medium-chain-length perfluoroalkyl iodide telomer

A technology of perfluoroalkyl iodide and synthesis method, which is applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., and can solve problems such as small production capacity, low pressure reaction rate, and easy coverage of light sources by polymers. Achieve the effect of improving conversion rate and controlling chain length distribution

Inactive Publication Date: 2018-03-06
SHANDONG DONGYUE POLYMER MATERIAL
View PDF12 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] CN1379008A has introduced the method that a kind of light-induced telomerization prepares alkyl iodide, and this method is to C 2 f 5 The mixture of I and tetrafluoroethylene is added to a reactor with a low-pressure light source as the source of initiation for telomerization. Although this method has lower pressure and higher reaction rate, the light source is easily covered by the polymer and cannot continue. The production capacity is small due to the reaction caused, and it is impossible to realize large-scale industrial production

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 600mL stainless steel vertical reaction kettle, after drying and removing water, add 8g electrolytic copper powder and 2g triphenylphosphine. After the kettle is evacuated, it is replaced with dry nitrogen to remove oxygen, and the oxygen content reaches below 10ppm. Add C to the kettle with an auxiliary pump at room temperature 2 f 51 780g, open stirring, feed tetrafluoroethylene, be warming up to start reaction, when rising to 110 ℃, pressure is about 2MPa, when the pressure in the kettle drops to 1.8MPa, feed tetrafluoroethylene again to pressure be 2MPa, Repeat several times, react until the pressure no longer changes, lower the temperature, and recover unreacted C 2 f 5 I, to obtain the product C 2 f 5 (CF 2 CF 2 ) n I have a total of 190g. After the product was washed with alkali and dehydrated, the components and their proportions in the product were analyzed by gas chromatography-mass spectrometry, as shown in Table 1.

[0030] Table 1 analysis results...

Embodiment 2

[0040] 600mL stainless steel vertical reaction kettle, after drying and removing water, add 8g of tin powder and 2g of tributylphosphine. After the kettle is evacuated, it is replaced with dry nitrogen to remove oxygen, and the oxygen content reaches below 10ppm. Add C to the kettle with an auxiliary pump at room temperature 2 f 5 I 800g, turn on the stirring, feed tetrafluoroethylene, heat up to start the reaction, when the pressure rises to 95°C, the pressure is about 2MPa, when the pressure in the kettle drops to 1.7MPa, feed tetrafluoroethylene again until the pressure is 1.9MPa , repeated several times, react until the pressure no longer changes, lower the temperature, and recover unreacted C 2 f 5 I, to obtain the product C 2 f 5 (CF 2 CF 2 ) n I have a total of 186g. After the product was washed with alkali and dehydrated, the components and their proportions in the product were analyzed by GC-MS, as shown in Table 3.

[0041] Table 3 analysis results

[0042...

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 belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of a medium-chain-length perfluoroalkyl iodide telomer. The synthesis method comprisesthe following step: adding a polymerized monomer CF2=CR1R2, a telogen RfI, a metal catalyst and a promoter into a reaction container for polymerization reaction to obtain a perfluoroalkyl iodide telomer with a carbon number of 3 to 14, wherein the perfluoroalkyl iodide telomer has the following general formula: Rf(CF2CR1R2)nI, where Rf is a perfluoroalkyl group with a carbon number of 1 to 8, R1and R2 can be the same or different, and are respectively selected from a fluorine atom and a saturated perfluoroalkyl group with a carbon number of 1 to 4, and n is an integer from 1 to 6; the promoter is PR1R2R3, and R1, R2 and R3 can be the same or different, and are selected from an alkyl group and an aryl group. The method is suitable for industrial large-scale production, and can effectivelyproduce the medium-chain-length perfluoroalkyl iodide telomer at low temperature, with very few impurities produced; furthermore, a target compound is narrow in molecular weight distribution and highin yield.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for synthesizing a medium-chain-length perfluoroalkyl iodide telomer. Background technique [0002] As we all know, perfluoroalkyl iodides are monoiodoperfluoroalkane compounds in which hydrogen atoms are completely replaced by fluorine atoms. They are generally composed of a series of perfluoroalkyl groups with different chain lengths. The most valuable ones are those with 6 carbon atoms. -12 perfluoroalkyl iodides, among which perfluorooctane with 8 carbon atoms has the best performance. Perfluoroalkyl iodide is a key intermediate in the production of fluorine finishing agents, fluorine-containing surfactants and other fluorine-containing fine chemicals. Its downstream products are used in light water fire extinguishing agents, magnetic recording materials, water and oil repellent fabric finishing agents, paper Finishing agent, oil field chemistr...

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
IPC IPC(8): C07C17/278C07C19/16
CPCC07C17/278C07C19/16
Inventor 陈越孟章富王金枝罗永振
Owner SHANDONG DONGYUE POLYMER MATERIAL