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A Fluorination System of Unstable Terminal Groups of Perfluoropolyether

A perfluoropolyether, fluorinated technology, applied in chemical methods, chemical instruments and methods, chemical/physical processes, etc. to make liquids react with gaseous media, which can solve the problems of insufficient gas-liquid contact, high reaction cost, long time Reaction time and other issues to achieve the effect of improving utilization efficiency, improving mass transfer capacity, and increasing contact area

Active Publication Date: 2021-12-14
SHANGHAI OULEIFEN BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are two main methods for fluorinating the unstable terminal groups of perfluoropolyether, one is to use AlF 3 , SbF 5 High-temperature fluorination of solid fluorinating agents, but the price of fluorinating agents used in this method is relatively high, and the product separation is difficult, and the metal ions in it are difficult to remove completely, which will greatly affect product quality
The second method is to use fluorine gas to carry out end group fluorination of perfluoropolyether. The product obtained by this method is pure and the post-treatment is simple, but due to the low solubility of fluorine gas in the reactant, it is not easy to interact with the activity of perfluoropolyether. The terminal groups are fully reacted, and the existing fluorination reaction equipment such as reactors all have the disadvantages of insufficient gas-liquid contact and low utilization rate of fluorinating agent. The fluorine gas needs to be greatly excessive, and the general dosage needs to be ten times the theoretical value. several times, and requires a long reaction time, the overall reaction efficiency is low, the reaction cost is high, and the tail gas treatment capacity is increased, which is not conducive to environmental protection

Method used

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  • A Fluorination System of Unstable Terminal Groups of Perfluoropolyether
  • A Fluorination System of Unstable Terminal Groups of Perfluoropolyether
  • A Fluorination System of Unstable Terminal Groups of Perfluoropolyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1 provides a kind of perfluoropolyether unstable terminal fluorination system, including gas feed system, liquid feed system, reaction system, product acceptance system 7, tail gas treatment system 8; said gas feed system Including a gas injector 10 and a gas storage device; the liquid feed system includes a liquid storage device 1 and a material pump 5-1; the reaction system includes a bubble column fluorination reactor 4, the upper end of which is provided with a feed port and a back pressure valve 9; the gas injector 10 is arranged at the bottom of the bubble column fluorination reactor 4, and is connected with the gas storage device through a pipeline; the liquid storage device 1 is connected with the gas storage device through a pipeline The feeding port at the upper end of the bubble column fluorination reactor 4 is connected, and the material pump 5-1 is arranged on the connecting pipeline; the product receiving system 7 and the tail gas treatment syste...

Embodiment 2

[0061] Example 2 provides a fluorinated system for unstable terminal groups of perfluoropolyether. The fluorinated system in Implementation 1 is used. The specific steps in use include: pumping 50L of perfluoropolyether with a number average molecular weight of 3300Da after vacuuming acid raw material, and then the reactor was heated to 150°C, the circulation pump was turned on to circulate the material in the reactor, and the pressure of the back pressure valve was set to 0.5MPa. Open the fluorine gas valve, feed in a mixed gas of fluorine gas and nitrogen with a mass concentration of 20% fluorine gas, control the flow rate at 5.0g / min, and after ventilating for one hour, adjust the heating device of the bubble column fluorination reactor to raise the temperature to 250-255°C and keep After 30 hours, stop feeding the fluorine gas, turn off the heating, and feed nitrogen gas for purging. After the temperature dropped to 40°C, stop the nitrogen purge, open the discharge valve, ...

Embodiment 3

[0063]Example 3 provides a fluorinated system for unstable terminal groups of perfluoropolyether. The fluorinated system in Implementation 1 is used. The specific steps in use include: pumping 50L of perfluoropolyether with a number average molecular weight of 3300Da after vacuuming Acyl fluoride and perfluoropolyether acid are mixed raw materials with a mass ratio of 3:2, then the reactor is heated to 150°C, the circulation pump is turned on to circulate the material in the reactor, and the pressure of the back pressure valve is set to 0.5MPa. Open the fluorine gas valve, feed in a mixed gas of fluorine gas and nitrogen with a mass concentration of 50% of fluorine gas, control the flow rate to 3.0g / min, and after ventilating for one hour, adjust the heating device of the bubble tower fluorination reactor to raise the temperature to 255-260°C and keep After 20 hours, stop feeding the fluorine gas, turn off the heating, and feed nitrogen gas for purging. After the temperature d...

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Abstract

The invention relates to the technical field of fluorine chemical industry, in particular to a fluorination system for unstable terminal groups of perfluoropolyether. It includes a gas feed system, a liquid feed system, a reaction system, a product receiving system, and a tail gas treatment system; the gas feed system includes a gas injector and a gas storage device; the liquid feed system includes a liquid storage device and material pump; the reaction system includes a bubble tower fluorination reactor, the upper end of which is provided with a feeding port and a back pressure valve; the gas injector is arranged at the bottom of the bubble tower fluorination reactor, and is connected with the The gas storage device is connected; the liquid storage device is connected with the feeding port at the upper end of the bubble column fluorination reactor through a pipeline, and the material pump is arranged on the connecting pipeline; the product receiving system and tail gas treatment The system is respectively connected with the bubble column fluorination reactors.

Description

technical field [0001] The invention relates to the technical field of fluorine chemical industry, in particular to a fluorination system for unstable terminal groups of perfluoropolyether. Background technique [0002] Perfluoropolyether has excellent high and low temperature stability, low surface tension, chemical inertness, non-flammability, low volatility, good lubricity, water and solvent resistance, excellent radiation stability, compatibility with metal plastic elastomers, With high dielectric properties, non-toxicity and excellent viscosity-temperature characteristics, it is widely used as high-vacuum pump oil, lubricant, insulating fluid, heat transfer fluid and cooling fluid in the fields of electronics, military industry, nuclear energy, and high-end equipment. [0003] The currently marketed perfluoropolyethers mainly include K-type prepared by ring-opening polymerization of hexafluoropropylene oxide, Y-type prepared by oxygen oxidation of hexafluoropropylene, Z...

Claims

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Application Information

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IPC IPC(8): C08G65/323B01D53/18B01D53/02B01J10/00
CPCC08G65/323C08G65/3236B01D53/18B01D53/02B01J10/00B01D2252/10B01D2253/102
Inventor 栾英豪李福清杜文朝刘晨斌戴力
Owner SHANGHAI OULEIFEN BIOLOGICAL TECH