CN103145971A - Synthetic method of perfluoropolyether - Google Patents
Synthetic method of perfluoropolyether Download PDFInfo
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- CN103145971A CN103145971A CN2013100731712A CN201310073171A CN103145971A CN 103145971 A CN103145971 A CN 103145971A CN 2013100731712 A CN2013100731712 A CN 2013100731712A CN 201310073171 A CN201310073171 A CN 201310073171A CN 103145971 A CN103145971 A CN 103145971A
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Abstract
The invneiton discloses a synthetic method of perfluoropolyether. The synthetic method comprises the following steps of: reacting a first volume part of purified hexafluoropropylene gas and alkali metal fluoride in an aprotic solvent at 0 DEG C to 50 DEG C to obtain low polymer; cooling the temperature of the obtained low polymer to the range of -40 DEG C to -20 DEG C, and adding a second volume part of purified hexafluoropropylene gas for reaction with the low polymer to obtain perfluoropolyether. According to the synthetic method of perfluoropolyether disclosed by the invention, the synthetic process for feeding materials and controlling temperature in stages is adopted to prepare perfluoropolyether, so that the conversion rate of hexafluoropropylene reaches 99% and above; moreover, the prepared perfluoropolyether has high average molecular weight. Besides, the material hexafluoropropylene gas is purified by using alkali substances and silica gel, so that the used alkali substance and silica gel are low in cost and can be repeatedly used while the material gas reaches the using requirements. Meanwhile, in the process of synthesizing perfluoropolyether, the use of diluents is avoided, so that the process is simple and the cost is lower, therefore, the synthetic method is suitable for industrial application.
Description
Technical field
The present invention relates to technical field of polymer materials, relate in particular to a kind of synthetic method of PFPE.
Background technology
PFPE is a kind of water white perfluoro-polymer material.Compare with common pfpe molecule structure, PFPE has replaced c h bond with the C-F key, and the fluorine atom with strong electronegativity makes the magnetism between molecule little, has less surface tension; Simultaneously the C-F key makes it have heat-resisting, resistance to oxidation, corrosion-resistant, anti-irradiation to the shielding effect of main chain and the characteristic such as does not fire.The high molecular PFPE is through having low volatility, wider fluid temperature scope and excellent viscosity-temperature profile after stabilization treatment, as the lubricant applications of excellence in fields such as aerospace industry, electronic industry, electrical industry and nuclear industry.
At present, the production technology of PFPE mainly contains two kinds, and a kind of is the photoxidation polymerization technique of tetrafluoroethylene or R 1216, although this production technology production cost is lower, hazard level is high simultaneously for complex process; Another is perfluoroepoxide, anionic polymerization as Propylene oxide hexafluoride or tetrafluoro trimethylene oxide, simple and the safety of this method Production Flow Chart, it is present widely used production method, but its reaction conditions, as all influential to the molecular-weight average of feed stock conversion, polymer product in material purity, temperature of reaction and material viscosity, this just makes the PFPE product molecular-weight average of preparation lower, and the Propylene oxide hexafluoride transformation efficiency is lower, can not satisfy practical application request.
Prior art discloses the employing metal hydride raw material Propylene oxide hexafluoride gas has been purified, and add R 1216 as thinner, reduce material viscosity, the technique of preparation PFPE, but it is higher to there is the metal hydride cost, and the thinner R 1216 is difficult to reclaim, the shortcoming that the Propylene oxide hexafluoride transformation efficiency is lower, and the PFPE molecular-weight average of preparation is lower, does not reach industrial requirements.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of synthetic method of PFPE, makes Propylene oxide hexafluoride have higher transformation efficiency, and synthetic PFPE molecular-weight average is higher.
The invention provides a kind of synthetic method of PFPE, comprising:
A) with the Propylene oxide hexafluoride gas after the first parts by volume purifying and alkaline metal fluoride cpd in aprotic solvent, 0 ℃～50 ℃ are reacted and obtain oligopolymer;
B) with steps A) the oligopolymer temperature that obtains is down to-40 ℃～-20 ℃, adds wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, and reaction obtains PFPE.
Preferably, the Propylene oxide hexafluoride gas after described purifying obtains in accordance with the following methods:
Adopt successively alkaline matter and silica gel to carry out purifying to Propylene oxide hexafluoride gas, obtain the Propylene oxide hexafluoride gas after purifying; Described alkaline matter is selected from any one or a few in alkali metal hydroxide, alkaline earth metal hydroxides, alkaline earth metal oxide and aluminium hydroxide.
Preferably, the summation of the Propylene oxide hexafluoride gas after described the first parts by volume purifying and the Propylene oxide hexafluoride gas after the second parts by volume purifying and the mass ratio of described aprotic solvent are 1:0.1～0.3.
Preferably, the volume ratio of the Propylene oxide hexafluoride gas after described the first parts by volume purifying and the Propylene oxide hexafluoride gas after the second parts by volume purifying is 1:3～5.
Preferably, described step B) being specially: with steps A) the oligopolymer temperature that obtains is down to-30 ℃～-25 ℃, adds wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, and reaction obtains PFPE.
Preferably, the summation of the Propylene oxide hexafluoride gas after described the first parts by volume purifying and the Propylene oxide hexafluoride gas after the second parts by volume purifying and the mol ratio of described alkaline metal fluoride cpd are 50～100:1.
Preferably, described aprotic solvent is multiethylene-glycol dme compounds.
Preferably, the pressure that reacts in aprotic solvent of the Propylene oxide hexafluoride gas after described purifying and alkaline metal fluoride cpd is negative pressure.
Compared with prior art, the present invention after with the first parts by volume purifying Propylene oxide hexafluoride gas and alkaline metal fluoride cpd in aprotic solvent, 0 ℃～50 ℃ are reacted and obtain oligopolymer; Then the oligopolymer temperature that obtains is down to-40 ℃～-20 ℃, adds wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, reaction obtains PFPE.The present invention adopts the synthesis technique of reinforced temperature control stage by stage, and the preparation PFPE makes the transformation efficiency of Propylene oxide hexafluoride gas reach more than 99%, and the PFPE of preparation has higher molecular-weight average; In addition, the present invention carries out purifying with alkaline matter and silica gel to raw material Propylene oxide hexafluoride gas, and when making unstripped gas reach service requirements, the alkaline matter of use and silica gel have advantage with low cost, reusable; In the process of synthetic PFPE, avoided the use of thinner simultaneously, made technique simple, cost is lower, is fit to industrial applications.
Embodiment
The invention provides a kind of synthetic method of PFPE, comprising:
A) with the Propylene oxide hexafluoride gas after the first parts by volume purifying and alkaline metal fluoride cpd in aprotic solvent, 0 ℃～50 ℃ are reacted and obtain oligopolymer;
B) with steps A) the oligopolymer temperature that obtains is down to-40 ℃～-20 ℃, adds wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, and reaction obtains PFPE.
The present invention adopts the synthesis technique of reinforced temperature control stage by stage, the preparation PFPE, at first with the Propylene oxide hexafluoride gas after the first parts by volume purifying and alkaline metal fluoride cpd in aprotic solvent, 0 ℃～50 ℃ are reacted and obtain oligopolymer; Then the oligopolymer temperature that obtains is down to-40 ℃～-20 ℃, add wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, reaction obtains PFPE, make the transformation efficiency of Propylene oxide hexafluoride gas reach more than 99%, and the PFPE of preparation have higher molecular-weight average; In addition, the present invention carries out purifying with alkaline matter and silica gel to raw material Propylene oxide hexafluoride gas, and when making unstripped gas reach service requirements, the alkaline matter of use and silica gel have advantage with low cost, reusable; In the process of synthetic PFPE, avoided the use of thinner simultaneously, made technique simple, cost is lower, is fit to industrial applications.
At first the present invention carries out purifying to raw material Propylene oxide hexafluoride gas, preferred, adopts successively alkaline matter and silica gel to carry out purifying to Propylene oxide hexafluoride gas, obtains the Propylene oxide hexafluoride gas after purifying; Described alkaline matter is preferably any one or a few in alkali metal hydroxide, alkaline earth metal hydroxides, alkaline earth metal oxide and aluminium hydroxide, more preferably any one or a few in aluminium hydroxide, sodium hydroxide and calcium oxide; The present invention there is no particular requirement to the source of described alkaline matter, can be for generally commercially available; The present invention there is no particular restriction to described silica gel, can be general commercially available discolour silica gel; Described silica gel can reclaim use, and preferred, it is carried out high temperature dehydration is recyclable use, and described bake out temperature is preferably 150 ℃～200 ℃.The present invention there is no particular requirement to the mode that described alkaline matter and silica gel carry out purifying to unstripped gas, can be purification for gas mode well known to those skilled in the art, the preferred absorption method that adopts is carried out purification for gas, such as alkaline matter and silica gel are placed in respectively the gas adsorption tower, make Propylene oxide hexafluoride gas successively by the adsorption tower of alkaline matter and silica gel is housed, obtain the Propylene oxide hexafluoride gas after purifying; Described alkaline matter and silica gel are solid, and the present invention there is no particular requirement to its shape, and sheet, particulate state, bulk all can.After testing, the content of acid gas of the Propylene oxide hexafluoride gas after purifying is lower than 0.1wt%, and water-content is less than 5ppm, and Perfluoroacetone content meets the industrial application requirement lower than 0.01wt%.The present invention uses alkaline matter and silica gel to carry out purifying to unstripped gas, and it is lower that the alkaline matter that uses and silica gel are cost, and the material of recoverable, has therefore reduced process costs, is conducive to suitability for industrialized production.
After unstripped gas is carried out purifying, first with the Propylene oxide hexafluoride gas after the first parts by volume purifying and alkaline metal fluoride cpd in aprotic solvent, 0 ℃～50 ℃ are reacted and obtain oligopolymer; Described alkaline metal fluoride cpd is catalyzer, is preferably cesium fluoride, and is preferred in the present invention, before use described alkaline metal fluoride cpd is dewatered, and grind into powder, make catalyzer easily disperse in reaction system, improve its reactive behavior; Described aprotic solvent is preferably multiethylene-glycol dme compounds, tetraethyleneglycol dimethyl ether more preferably, in the present invention, preferably, adopt before use sodium Metal 99.5 or its hydride that described aprotic solvent is dewatered, make its water content lower than 1ppm, make and react carry out more abundant, improve the transformation efficiency of raw material.Preferably, the pressure that reacts in aprotic solvent of the Propylene oxide hexafluoride gas after described purifying and alkaline metal fluoride cpd is negative pressure.
After obtaining oligopolymer, its temperature is down to-40 ℃～-20 ℃, adds wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, reaction obtains PFPE.Propylene oxide hexafluoride gas after described the first parts by volume purifying and the volume ratio of the Propylene oxide hexafluoride gas after the second parts by volume purifying are preferably 1:3～5, more preferably 1:3.5～4.5; Propylene oxide hexafluoride gas after described the first parts by volume purifying and the summation of the Propylene oxide hexafluoride gas after the second parts by volume purifying and the mass ratio of described aprotic solvent are preferably 1:0.1～0.3, more preferably 1:0.15～0.25; Propylene oxide hexafluoride gas after described the first parts by volume purifying and the summation of the Propylene oxide hexafluoride gas after the second parts by volume purifying and the mol ratio of described alkaline metal fluoride cpd are preferably 50～100:1, more preferably 65～85:1.The present invention preferably reacts under the protection of rare gas element, and described rare gas element is preferably nitrogen.
In the present invention, adopt the synthesis technique of reinforced temperature control stage by stage, add Propylene oxide hexafluoride gas in batches, and adopt temperature stage by stage to react, preferred, the temperature of fs is 0 ℃～50 ℃, more preferably 10 ℃～30 ℃, most preferably be 15 ℃～25 ℃, in this stage, Propylene oxide hexafluoride gas rapid polymerization in the aprotic solvent that contains the alkaline metal fluoride cpd catalyzer becomes oligopolymer; The temperature of subordinate phase is preferably-40 ℃～-20 ℃, more preferably-25 ℃～-30 ℃, most preferably be-26 ℃～-28 ℃, in this stage, constantly polymerization in the oligopolymer that a large amount of Propylene oxide hexafluoride gases that add obtained in the fs, thereby prepare the higher PFPE product of molecular-weight average, and Propylene oxide hexafluoride gas has higher transformation efficiency.Simultaneously, the present invention need not to add thinner, reaction raw materials can carry out polyreaction in aprotic solvent, avoided thinner is carried out the operation of purifying and recovery, after reaction finishes, PFPE product and aprotic solvent natural layering, need not complex separations technique, make technique simple, cost is lower, is fit to industrial applications.
The PFPE product for preparing has the structure shown in formula I:
Wherein, 60≤n≤70;
Use F19-NMR to carry out analyzing and testing to the PFPE of preparation, result shows, the PFPE product molecular-weight average that obtains reaches 10000 left and right; The transformation efficiency of Propylene oxide hexafluoride is 99% left and right.
The present invention after with the first parts by volume purifying Propylene oxide hexafluoride gas and alkaline metal fluoride cpd in aprotic solvent, 0 ℃～50 ℃ are reacted and obtain oligopolymer; Then the oligopolymer temperature that obtains is down to-40 ℃～-20 ℃, adds wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, reaction obtains PFPE.The present invention adopts the synthesis technique of reinforced temperature control stage by stage, and the preparation PFPE makes the transformation efficiency of Propylene oxide hexafluoride gas reach more than 99%, and the PFPE of preparation has higher molecular-weight average; In addition, the present invention carries out purifying with alkaline matter and silica gel to raw material Propylene oxide hexafluoride gas, and when making unstripped gas reach service requirements, the alkaline matter of use and silica gel have advantage with low cost, reusable; In the process of synthetic PFPE, avoided the use of thinner simultaneously, made technique simple, cost is lower, is fit to industrial applications.
In order to further illustrate the present invention, below in conjunction with embodiment, the synthetic method of PFPE provided by the invention is described in detail.
Embodiment 1
Raw material Propylene oxide hexafluoride gas is passed in 2 groups of adsorption towers that are filled with scavenging agent, wherein fill aluminium hydroxide in first group of adsorption tower, filling gel in second group of adsorption tower; When the adsorption tower internal pressure rises to 0.2MPa, discharge Propylene oxide hexafluoride gas after purifying with the gas speed of 4L/h from the adsorption tower end, after stablizing 2h, in tower, purification for gas reaches equilibrium state, after testing, in the Propylene oxide hexafluoride gas after purifying, content of acid gas is 0.01wt%, water-content is 5ppm, and Perfluoroacetone content is 0.006wt%.
Under the protection of high pure nitrogen, will add rapidly in the stainless steel cauldron of 2L through 10g cesium fluoride powder and the 200g tetraethyleneglycol dimethyl ether that strictly dewaters, then reactor is sealed and system in still is pumped into negative pressure; Controlling the interior system temperature of reactor is 20 ℃, the Propylene oxide hexafluoride gas after the 30L purifying is passed in reactor insulated and stirred reaction 2h; Then temperature in the kettle is down to-25 ℃, then passes into the Propylene oxide hexafluoride gas after the 118L purifying, and insulated and stirred reaction 4h; After reaction finishes, temperature in the kettle is slowly risen to room temperature (25 ℃), blowing obtains the PFPE product at the bottom of the still, is thick liquid.By F19-NMR, product is analyzed, result shows, the PFPE molecular-weight average for preparing is 9900, and transformation efficiency is 99%.
Embodiment 2
Raw material Propylene oxide hexafluoride gas is passed in 2 groups of adsorption towers that are filled with scavenging agent, wherein fill sodica calx in first group of adsorption tower, filling gel in second group of adsorption tower; When the adsorption tower internal pressure rises to 0.1MPa, discharge Propylene oxide hexafluoride gas after purifying with the gas speed of 4L/h from the adsorption tower end, after stablizing 2h, in tower, purification for gas reaches equilibrium state, after testing, in the Propylene oxide hexafluoride gas after purifying, content of acid gas is 0.06wt%, water-content is 0.5ppm, and Perfluoroacetone content is 0.004wt%.
Under the protection of high pure nitrogen, will add rapidly in the stainless steel cauldron of 2L through 12g cesium fluoride powder and the 160g tetraethyleneglycol dimethyl ether that strictly dewaters, then reactor is sealed and system in still is pumped into negative pressure; Controlling the interior system temperature of reactor is 20 ℃, the Propylene oxide hexafluoride gas after the 35L purifying is passed in reactor insulated and stirred reaction 2h; Then temperature in the kettle is down to-30 ℃, then passes into the Propylene oxide hexafluoride gas after the 155L purifying, and insulated and stirred reaction 4h; After reaction finishes, temperature in the kettle is slowly risen to room temperature (25 ℃), blowing obtains the PFPE product at the bottom of the still, is thick liquid.By F19-NMR, product is analyzed, result shows, the PFPE molecular-weight average for preparing is 11000, and transformation efficiency is 100%.
Embodiment 3
Raw material Propylene oxide hexafluoride gas is passed in 2 groups of adsorption towers that are filled with scavenging agent, wherein fill sodica calx in first group of adsorption tower, filling gel in second group of adsorption tower; When the adsorption tower internal pressure rises to 0.2MPa, discharge Propylene oxide hexafluoride gas after purifying with the gas speed of 4L/h from the adsorption tower end, after stablizing 2h, in tower, purification for gas reaches equilibrium state, after testing, in the Propylene oxide hexafluoride gas after purifying, content of acid gas is 0.05wt%, water-content is 1ppm, and Perfluoroacetone content is 0.008wt%.
Under the protection of high pure nitrogen, will add rapidly in the stainless steel cauldron of 2L through 15g cesium fluoride powder and the 200g tetraethyleneglycol dimethyl ether that strictly dewaters, then reactor is sealed and system in still is pumped into negative pressure; Controlling the interior system temperature of reactor is 20 ℃, the Propylene oxide hexafluoride gas after the 45L purifying is passed in reactor insulated and stirred reaction 2h; Then temperature in the kettle is down to-30 ℃, then passes into the Propylene oxide hexafluoride gas after the 180L purifying, and insulated and stirred reaction 4h; Reaction slowly rises to room temperature (25 ℃) with temperature in the kettle after finishing, and blowing obtains the PFPE product, is thick liquid.By F19-NMR, product is analyzed, result shows, the PFPE molecular-weight average for preparing is 10500, and transformation efficiency is 99%.
Embodiment 4
Raw material Propylene oxide hexafluoride gas is passed in 2 groups of adsorption towers that are filled with scavenging agent, wherein fill sodica calx in first group of adsorption tower, filling gel in second group of adsorption tower; When the adsorption tower internal pressure rises to 0.2MPa, discharge Propylene oxide hexafluoride gas after purifying with the gas speed of 4L/h from the adsorption tower end, after stablizing 2h, in tower, purification for gas reaches equilibrium state, after testing, in the Propylene oxide hexafluoride gas after purifying, content of acid gas is 0.04wt%, water-content is 2ppm, and Perfluoroacetone content is 0.007wt%.
Under the protection of high pure nitrogen, will add rapidly in the stainless steel cauldron of 2L through 9g cesium fluoride powder and the 200g tetraethyleneglycol dimethyl ether that strictly dewaters, then reactor is sealed and system in still is pumped into negative pressure; Controlling the interior system temperature of reactor is 30 ℃, the Propylene oxide hexafluoride gas after the 30L purifying is passed in reactor insulated and stirred reaction 2h; Then temperature in the kettle is down to-35 ℃, then passes into the Propylene oxide hexafluoride gas after the 105L purifying, and insulated and stirred reaction 4h; Reaction slowly rises to room temperature (25 ℃) with temperature in the kettle after finishing, and blowing obtains the PFPE product, is thick liquid.By F19-NMR, product is analyzed, result shows, the PFPE molecular-weight average for preparing is 10500, and transformation efficiency is 99%.
Embodiment 5
Raw material Propylene oxide hexafluoride gas is passed in 2 groups of adsorption towers that are filled with scavenging agent, wherein fill sodica calx in first group of adsorption tower, filling gel in second group of adsorption tower; When the adsorption tower internal pressure rises to 0.2MPa, discharge Propylene oxide hexafluoride gas after purifying with the gas speed of 4L/h from the adsorption tower end, after stablizing 2h, in tower, purification for gas reaches equilibrium state, after testing, in the Propylene oxide hexafluoride gas after purifying, content of acid gas is 0.04wt%, water-content is 2ppm, and Perfluoroacetone content is 0.009wt%.
Under the protection of high pure nitrogen, will add rapidly in the stainless steel cauldron of 2L through 12g cesium fluoride powder and the 200g tetraethyleneglycol dimethyl ether that strictly dewaters, then reactor is sealed and system in still is pumped into negative pressure; Controlling the interior system temperature of reactor is 25 ℃, the Propylene oxide hexafluoride gas after the 30L purifying is passed in reactor insulated and stirred reaction 2h; Then temperature in the kettle is down to-20 ℃, then passes into the Propylene oxide hexafluoride gas after the 150L purifying, and insulated and stirred reaction 4h; Reaction slowly rises to room temperature (25 ℃) with temperature in the kettle after finishing, and blowing obtains the PFPE product, is thick liquid.By F19-NMR, product is analyzed, result shows, the PFPE molecular-weight average for preparing is 11000, and transformation efficiency is 99%.
By above-described embodiment and comparative example as can be known, the present invention adopts the synthesis technique of reinforced temperature control stage by stage, and the preparation PFPE makes the transformation efficiency of Propylene oxide hexafluoride gas reach more than 99%, and the PFPE of preparation has higher molecular-weight average.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (8)
1. the synthetic method of a PFPE comprises:
A) with the Propylene oxide hexafluoride gas after the first parts by volume purifying and alkaline metal fluoride cpd in aprotic solvent, 0 ℃～50 ℃ are reacted and obtain oligopolymer;
B) with steps A) the oligopolymer temperature that obtains is down to-40 ℃～-20 ℃, adds wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, and reaction obtains PFPE.
2. method according to claim 1, is characterized in that, the Propylene oxide hexafluoride gas after described purifying obtains in accordance with the following methods:
Adopt successively alkaline matter and silica gel to carry out purifying to Propylene oxide hexafluoride gas, obtain the Propylene oxide hexafluoride gas after purifying; Described alkaline matter is selected from any one or a few in alkali metal hydroxide, alkaline earth metal hydroxides, alkaline earth metal oxide and aluminium hydroxide.
3. method according to claim 1, is characterized in that, the Propylene oxide hexafluoride gas after described the first parts by volume purifying and the summation of the Propylene oxide hexafluoride gas after the second parts by volume purifying and the mass ratio of described aprotic solvent are 1:0.1～0.3.
4. method according to claim 1, is characterized in that, the Propylene oxide hexafluoride gas after described the first parts by volume purifying and the volume ratio of the Propylene oxide hexafluoride gas after the second parts by volume purifying are 1:3～5.
5. method according to claim 1, it is characterized in that, described step B) being specially: with steps A) the oligopolymer temperature that obtains is down to-30 ℃～-25 ℃, adds wherein the Propylene oxide hexafluoride gas after the second parts by volume purifying, and reaction obtains PFPE.
6. method according to claim 1, is characterized in that, the Propylene oxide hexafluoride gas after described the first parts by volume purifying and the summation of the Propylene oxide hexafluoride gas after the second parts by volume purifying and the mol ratio of described alkaline metal fluoride cpd are 50～100:1.
7. method according to claim 1, is characterized in that, described aprotic solvent is multiethylene-glycol dme compounds.
8. method according to claim 1, is characterized in that, the pressure that the Propylene oxide hexafluoride gas after described purifying and alkaline metal fluoride cpd react in aprotic solvent is negative pressure.
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| CN104513390A (en) * | 2013-12-24 | 2015-04-15 | 东莞市长安东阳光铝业研发有限公司 | Method for preparing hexafluoropropylene oxide oligomer |
| CN105273178A (en) * | 2014-05-30 | 2016-01-27 | 东莞市长安东阳光铝业研发有限公司 | Preparation method for hexafluoropropylene oxide homopolymers |
| CN106397761A (en) * | 2016-09-06 | 2017-02-15 | 天津长芦新材料研究院有限公司 | Fluorination method for end groups of perfluoropolyether acid |
| CN111495108A (en) * | 2020-04-22 | 2020-08-07 | 浙江利化新材料科技有限公司 | Method for separating and purifying hexafluoropropylene oxide and adsorbent used by same |
| CN113321798A (en) * | 2021-06-24 | 2021-08-31 | 南开大学 | Preparation method of high-stability low-molecular-weight saturated perfluoropolyether |
| CN114395122A (en) * | 2021-12-31 | 2022-04-26 | 西安近代化学研究所 | Terpolymer perfluoropolyether and preparation method thereof |
| CN114456369A (en) * | 2021-12-31 | 2022-05-10 | 西安近代化学研究所 | Binary copolymerization perfluoropolyether and preparation method thereof |
| CN115785433A (en) * | 2022-12-21 | 2023-03-14 | 浙江诺亚氟化工有限公司 | Preparation method of perfluoropolyether acyl fluoride |
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| CN104513390A (en) * | 2013-12-24 | 2015-04-15 | 东莞市长安东阳光铝业研发有限公司 | Method for preparing hexafluoropropylene oxide oligomer |
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| CN106397761A (en) * | 2016-09-06 | 2017-02-15 | 天津长芦新材料研究院有限公司 | Fluorination method for end groups of perfluoropolyether acid |
| CN106397761B (en) * | 2016-09-06 | 2021-06-18 | 天津长芦新材料研究院有限公司 | Process for fluorinating acid end groups of perfluoropolyethers |
| CN111495108A (en) * | 2020-04-22 | 2020-08-07 | 浙江利化新材料科技有限公司 | Method for separating and purifying hexafluoropropylene oxide and adsorbent used by same |
| CN111495108B (en) * | 2020-04-22 | 2022-03-15 | 浙江利化新材料科技有限公司 | Method for separating and purifying hexafluoropropylene oxide and adsorbent used by same |
| CN113321798A (en) * | 2021-06-24 | 2021-08-31 | 南开大学 | Preparation method of high-stability low-molecular-weight saturated perfluoropolyether |
| CN114395122A (en) * | 2021-12-31 | 2022-04-26 | 西安近代化学研究所 | Terpolymer perfluoropolyether and preparation method thereof |
| CN114456369A (en) * | 2021-12-31 | 2022-05-10 | 西安近代化学研究所 | Binary copolymerization perfluoropolyether and preparation method thereof |
| CN114395122B (en) * | 2021-12-31 | 2023-06-09 | 西安近代化学研究所 | Ternary copolymer perfluoropolyether and preparation method thereof |
| CN114456369B (en) * | 2021-12-31 | 2023-06-09 | 西安近代化学研究所 | Binary copolymerization perfluoropolyether and preparation method thereof |
| CN115785433A (en) * | 2022-12-21 | 2023-03-14 | 浙江诺亚氟化工有限公司 | Preparation method of perfluoropolyether acyl fluoride |
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