Perfluoropolyether end group fluorination method

A technology of perfluoropolyether acyl fluoride and perfluoropolyether, applied in the field of perfluoropolyether end group fluorination, can solve the problems of product loss, molecular structure, average molecular weight viscosity change, perfluoropolyether self-polymerization, etc. Achieve the effect of less product loss and easy post-processing

Pending Publication Date: 2021-06-01
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are currently two main methods for fluorinating perfluoropolyether end groups, one is to use AlF 3 , SbF 5 Waiting for fluoride salt as a fluorinating agent, such as the method described in patent WO2009054569A1, the main disadvantage of this method is that fluoride salt is expensive, and the metal elements introduced into the product are difficult to separate, and will seriously affect product quality
Another method is the direct fluorination method using fluorine gas, such as the methods described in Chinese patents CN103111253A, CN106397761A, CN110092901A, etc., but the main disadvantage of this method is that the direct fluorination of fluorine gas generally requires high temperature and low molecular weight perfluorinated The boiling point of polyether is low, it is easy to cause los

Method used

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  • Perfluoropolyether end group fluorination method

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Effect test

Embodiment 1

[0038] Build the above-mentioned fluorination device, add 500g of perfluoropolyether acid fluoride to the reactor at 20°C, its average molecular weight is 1120g / mol, vacuumize the reactor to -0.1MPa, turn on the stirrer, and turn on the ultraviolet high pressure Mercury lamp (400W), open the valves of the nitrogen and fluorine cylinders, monitor and adjust the flow rate to 20mL / min for nitrogen and 80mL / min for fluorine with a gas flowmeter, and activate the mixture of nitrogen and fluorine in a photoactivated airtight container for 80s Finally, open the valve between the light-activated airtight container and the reactor, monitor it with a gas flowmeter and feed it into the reactor at a rate of 100mL / min for reaction. Monitor the progress of the reaction. After the reaction was finished (after 6.5 hours of continuous ventilating), nitrogen was passed into the reactor for purging, and after cooling, the discharge valve at the bottom of the reactor was opened, and the material ...

Embodiment 2

[0040] Build the above-mentioned fluorination device, add 500g of perfluoropolyether acid fluoride to the reactor at 20°C, its average molecular weight is 1480g / mol, vacuumize the reactor to -0.1MPa, turn on the agitator, turn on the ultraviolet high pressure Mercury lamp (400W), open the valves of the nitrogen and fluorine cylinders, monitor and adjust the flow rate to 20mL / min for nitrogen and 80mL / min for fluorine with a gas flowmeter, and activate the mixture of nitrogen and fluorine in a photoactivated airtight container for 80s Finally, open the valve between the light-activated airtight container and the reactor, monitor it with a gas flowmeter and feed it into the reactor at a rate of 100mL / min for reaction. Monitor the progress of the reaction. After the reaction finished (after 4.5 hours of continuous ventilating), feed nitrogen into the reactor for purging, open the discharge valve at the bottom of the reactor after cooling, and discharge to obtain 499g of product, ...

Embodiment 3

[0042] Build the above-mentioned fluorination device, add 500g of perfluoropolyether acid fluoride to the reactor at 25°C, with an average molecular weight of 550g / mol, vacuumize the reactor to -0.1MPa, turn on the agitator, and turn on the ultraviolet high pressure Mercury lamp (400W), open the valves of the nitrogen and fluorine cylinders, monitor and adjust the flow rate to 20mL / min for nitrogen and 80mL / min for fluorine with a gas flowmeter, and activate the mixture of nitrogen and fluorine in a photoactivated airtight container for 80s Finally, open the valve between the light-activated airtight container and the reactor, monitor it with a gas flowmeter and feed it into the reactor at a rate of 100mL / min for reaction. Monitor the progress of the reaction. After the reaction was finished (after 13 hours of continuous ventilation), nitrogen was passed into the reactor for purging, and after cooling, the discharge valve at the bottom of the reactor was opened, and the materi...

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Abstract

The invention provides a perfluoropolyether end group fluorination method which comprises the following steps: (1) irradiating mixed gas of fluorine gas and inert gas by using ultraviolet light, and activating; and (2) introducing the activated mixed gas into a reaction kettle filled with perfluoropolyether acyl fluoride, and reacting to obtain the end group fluorinated perfluoropolyether. According to the method disclosed by the invention, the fluorination reaction can be carried out at normal temperature, the obtained perfluoropolyether is easy to post-treat, the low-molecular-weight perfluoropolyether acyl fluoride product is less in loss, and the structure, the average molecular weight, the viscosity and the like of the fluorinated product are not changed.

Description

technical field [0001] The invention relates to the field of perfluoropolyether, in particular to a method for fluorinating the terminal group of perfluoropolyether. Background technique [0002] Perfluoropolyether is a fluoropolymer with high chemical inertness, oxidation resistance and corrosion resistance. Compared with perfluorocarbon chains, it has the advantages of flexibility, low glass transition temperature, and extremely wide co-liquid temperature range (freezing point to boiling point), and is widely used in the lubrication of aerospace, electronics, machinery and nuclear industries. agent. [0003] At present, there are two main methods for preparing perfluoropolyether, one is anionic ring-opening polymerization using hexafluoropropylene oxide as raw material, and the other is photooxidative polymerization using tetrafluoroethylene or hexafluoropropylene as raw material. The perfluoropolyether obtained by these two methods has a terminal acyl fluoride structure...

Claims

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Application Information

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IPC IPC(8): C08G65/323C08G65/00
CPCC08G65/3236C08G65/007
Inventor 李义涛阳峰侯琴卿贾渊唐尤健夏浪平彭军峰
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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