CN102277718B - Polyimide fiber with high acid resistance and preparation method thereof - Google Patents
Polyimide fiber with high acid resistance and preparation method thereof Download PDFInfo
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- CN102277718B CN102277718B CN2011101724721A CN201110172472A CN102277718B CN 102277718 B CN102277718 B CN 102277718B CN 2011101724721 A CN2011101724721 A CN 2011101724721A CN 201110172472 A CN201110172472 A CN 201110172472A CN 102277718 B CN102277718 B CN 102277718B
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- 239000000835 fiber Substances 0.000 title claims abstract description 81
- 239000004642 Polyimide Substances 0.000 title claims abstract description 47
- 229920001721 polyimide Polymers 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002253 acid Substances 0.000 title abstract description 12
- 239000011737 fluorine Substances 0.000 claims abstract description 32
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 13
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010521 absorption reaction Methods 0.000 claims abstract description 5
- 238000005102 attenuated total reflection Methods 0.000 claims abstract description 4
- 238000001228 spectrum Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 34
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000008246 gaseous mixture Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 11
- 238000001914 filtration Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000002791 soaking Methods 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 238000010792 warming Methods 0.000 description 10
- 230000032683 aging Effects 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004760 aramid Substances 0.000 description 3
- 229920003235 aromatic polyamide Polymers 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 125000001153 fluoro group Chemical group F* 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 description 2
- 229920006231 aramid fiber Polymers 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920002313 fluoropolymer Polymers 0.000 description 2
- 239000004811 fluoropolymer Substances 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 150000004984 aromatic diamines Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Images
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- Artificial Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a polyimide fiber with high acid resistance prepared by using the technology direct fluorination. The surface of the fiber contains a carbon-fluorine covalent bond structure; characteristic absorption peaks of polyimide appear near 1780 cm<-1>, 1720 cm<-1> and 1380 cm<-1> in the transmission infrared spectrogram of the fiber, while absorption peaks of the carbon-fluorine covalent bond appear in the range of 1100 to 1300 cm<-1> in attenuated total reflection infrared spectrogram; power spectrum peaks of the element fluorine appear near 688 eV binding energy in X-ray photoelectron spectrogram of the fiber; the retention rate of tensile strength of the fiber is 94 to 98% after the fiber has undergone soaking treatment for 240 hours in an aqueous solution of sulfuric acid with a concentration of 20 wt%. The invention also discloses a preparation method for the polyimide fiber with high acid resistance. The polyimide fiber disclosed in the invention has obviously enhanced acid resistance, maintains excellent high temperature resistance and mechanical properties, and can be used as a high-end filtering material. The preparation method disclosed in the invention has the advantages of a high fluorination rate, a short preparation time and capacity of realizing continuous and on-line surface treatment of the fiber.
Description
Technical field
The invention belongs to polyimide fiber and preparing technical field thereof, be specifically related to a kind of high acidproof polyimide fiber and preparation method thereof.
Background technology
Environmental problem has become one of several big problems of face of mankind at present, and wherein water pollution, air pollution, white garbage, noise pollution or the like are threatening our living environment just day by day.And one of several big important sources of air-polluting are the volumes of smoke that various occasions produce.
Since getting into 21 century, people pay attention to its research that produces the volume of smoke system of filtering that occasions such as factory and castoff burning field are used further.Though; Fiber is applied in the air cleaner with its special advantages more and more widely; But owing to need under conditions such as high temperature, deep-etching, work as the fiber of the tail gas filtering system of factory such as thermal power plant, smelting iron and steel factory, garbage burning factory etc., not only temperature is high such as the temperature of thermal power plant tail gas, and wherein also contains the gases such as sulfur trioxide that can generate sulfuric acid; Thereby the fiber that requires to be used for air cleaner is not only high temperature resistant, also wants resistance to acid attack.
The material that is used for the high-temperature flue gas filtration mainly contains high-performance fibers such as aramid fiber, glass fibre, polyphenylene sulfide, polyimide fiber and polytetrafluoroethylene (PTFE).But aramid fiber wherein is facile hydrolysis at high temperature; Glass fibre is more crisp, folding resistance difference and processing difficulties; Polyphenylene sulfide fibre is prone to oxidation; Polytetrafluoroethylene fibre not only price is higher, also wants dependence on import.Though and polyimide fiber can with its excellent heat resisting and favorable chemical resistance can and become one of most important fiber species in high temperature filtration field; But adopt the filter bag of polyimide fiber preparation to have only about 2 years general service life, and the service life of the filter bag of polytetrafluoroethylene fibre preparation is generally greater than 5 years.Therefore, the anti-sulfuric acid property of polyimide fiber is still waiting further raising.
At present, improve acidproof, the organic solvent resistance of material, normally in material, add age resister with the method that improves its ageing-resistant performance.Yet ageing-resistant adding can produce certain destruction to the mechanical property and the heat resistance of material body usually, thereby the combination property of material is reduced.Direct surface fluorination treatment technology is a kind of effective surface modifying method that fast development is in recent years got up, and it is to utilize the fluorine gas of high reaction activity to come high polymer is carried out surface modification as fluorination reagent.Because it forms nanometer layer at material surface, thereby neither influences the mechanical property of polymeric material body, and prepared surface fluorination polymeric material also has the low advantage of cost.Existing this method is mainly used in the surface treatment to polyolefin polymers, or improves the barrier property of TPO container, or material surfaces such as polyolefin are carried out activation processing, but to improve the adhesive property on its surface.Disclose the method that the oxygen fluorinated surface is handled like patent US7225561, US2006118988, CN1717438A, these methods mainly adopt the fluorine gas gaseous mixture that contains oxygen and water vapour that material surface is handled.CN101798748A discloses a kind of fluorine-contained surface aramid III fiber and preparation method thereof; The main gaseous mixture of fluorine gas and inert gas that adopts is handled the aramid III fiber surface; The purpose of its invention is to improve the surface-activity of this fiber, but with the shear bond strength that improves its surface cementability and composite thereof etc.Also can be used for improving the alignment film of polyimide orientation characteristic in addition.Disclose like patent CN101697049A and a kind ofly to have handled the method obtain polyimide liquid crystal direct action membrane with fluorine-contained surface through fluorinated surface, the purpose of its invention is to improve the tilt angle of alignment film of polyimide.In addition; US7267843B adopts the method for directly fluoridizing; Carry out graft reaction fluorochemical monomer or polymer at polyester, polyamide or aromatic polyamide fibre or its fabric face; Thereby make fiber or fabric face after the grafting have the fluorine structure of containing, improved the hydrophobic properties of the surface of fiber or fabric.This method comprises two steps: the first step adopts the F2/ inert gas that fiber or fabric are fluoridized; Second step was that fiber or the textile impregnation of fast first step being fluoridized carries out graft reaction in the aqueous suspension liquid of fluorochemical monomer (polymer).Its objective is the bonding way that the fluoropolymer that makes coating and fiber surface form chemical covalent bond, thereby overcome the caducous deficiency of fluoropolymer surface layer that traditional coating method causes.But also do not see to have and improve the acid proof bibliographical information of polyimide fiber through fluoridizing.
Summary of the invention
Primary and foremost purpose of the present invention is the high acidproof polyimide fiber that is directed against a kind of fluorine-contained surface that has the acid proof deficiency of polyimide fiber now and provide.
Another object of the present invention provides a kind of method for preparing the high acidproof polyimide fiber of above-mentioned fluorine-contained surface.
The acidproof polyimide fiber of height provided by the invention is characterized in that carbon-fluorine covalent bond structure is contained on the surface of this fiber; Its transmitted infrared light spectrogram is at 1780cm
-1, 1720cm
-1And 1380cm
-1Near the characteristic absorption peak of polyimides is arranged, the attenuated total reflectance infrared spectrogram is at 1100～1300cm
-1The absworption peak that carbon-fluorine covalent bond is arranged; Its x-ray photoelectron can have fluorine element power spectrum peak by spectrogram near the 688eV binding energy; It is that the stretching strength retentivity of immersion treatment after 240 hours is 94～98% in the 20wt% aqueous sulfuric acid in concentration.
The method of the high acidproof polyimide fiber that preparation provided by the invention is above-mentioned; It is characterized in that this method is earlier polyimide fiber to be placed reactor; Under atmosphere of inert gases, in reactor, charge into the fluorine gas gaseous mixture then, and under 5～100 ℃ of temperature, fluorination treatment was carried out 1～60 minute in its surface; Promptly obtain the polyimide fiber that carbon-fluorine covalent bond structure is contained on the surface, wherein the dividing potential drop of fluorine gas in reactor remains 5～100KPa.
The used fluorine gas gaseous mixture of said method is formed preferred fluorine gas and nitrogen composition by in fluorine gas and nitrogen, argon gas, helium or the carbon dioxide any.
The preferred 25-60 of the fluorination reaction temperature of said method ℃, preferred 5～20 minutes of fluorination reaction time.
Preferred 10～the 50KPa of fluorine gas dividing potential drop in reactor in the said method.
Be used to prepare high acidproof polyimide fiber in the said method and comprise business-like polyimide fiber, and polyimides long fiber that forms through prepared such as polymerization, spinning, imidizates by one or more aromatic series dianhydride monomers and one or more aromatic diamine monomer or staple fibre etc.
The present invention has following beneficial effect:
1, because the acidproof polyimide fiber of height provided by the invention has been introduced the fiber of carbon-fluorine polar covalence bond structure for the surface; Thereby not only further improved the polyimide fiber acid resistance; Obviously improved its service life under strong acid environment; Can satisfy more harsh environment for use and condition, also a kind of novel high-performance polyimide fiber kind that can match in excellence or beauty with polytetrafluoroethylene fibre is provided for the high temperature filtration field.
2, because the fluorine gas gaseous mixture that uses in the method for the fluorine-contained surface polyimide fiber of preparation acid resistance provided by the invention excellence does not contain air (oxygen and moisture content); Thereby can improve the fluorination rates of fluoridizing the stage effectively; Shorten the processing cycle; Reduce production costs, can be implemented in wire gauge modelling continuous surface and handle, can reduce its corrosion simultaneously fluorizating apparatus.
3, the method technology of the high acidproof polyimide fiber of preparation provided by the invention is simple, cost is low, have stronger application prospect.
Description of drawings
Fig. 1 is the transmitted infrared light spectrogram of the high acidproof polyimide fiber of the embodiment of the invention 1 prepared fluorine-contained surface, from figure, can see at 1780cm
-1, 1720cm
-1And 1380cm
-1Near the characteristic absorption peak of polyimides is arranged;
Fig. 2 is the attenuated total reflectance infrared spectrogram of the high acidproof polyimide fiber of the embodiment of the invention 1 prepared fluorine-contained surface, and wave number is 1100～1300cm among the figure
-1It is the absworption peak of carbon-fluorine covalent bond;
Fig. 3 is the embodiment of the invention 1 a prepared fluorine-contained surface polyimide fiber x-ray photoelectron ability spectrogram, and the peak at 688eV binding energy place is fluorine element power spectrum peak among the figure.
The specific embodiment
Through embodiment the present invention is carried out concrete description below; Be necessary to be pointed out that at this following examples only are used for the present invention is further specified; Can not be interpreted as restriction to protection domain of the present invention; Some nonessential improvement and adjustment that the person skilled in the art in this field makes according to the content of the invention described above still belong to protection scope of the present invention.
What be worth explanation in addition is; In following examples and the Comparative Examples; The acid resistance of polyimide fiber is that to adopt it be to handle 240 hours through soaking accelerated ageing in the 20wt% aqueous sulfuric acid in concentration; Carry out TENSILE STRENGTH test after cleaning repeatedly, dry with distilled water then, and the conservation rate of the TENSILE STRENGTH of the aging front and back through test is estimated.Stretching strength retentivity is the TENSILE STRENGTH of fiber after the persulfuric acid immersion treatment and soaks the ratio of the TENSILE STRENGTH of this fiber before.The stretching strength retentivity that soaks the back fiber is high more, shows that its acid resistance is good more.
Embodiment 1
Earlier polyimide fiber is placed the enclosed vacuum reactor; Vacuumize then; And with behind the air in the nitrogen replacement reactor three times; In vacuum reactor, charge into the gaseous mixture of delivery of fluorine/nitrogen, wherein fluorine gas dividing potential drop in reactor is 10KPa, and is warming up under 25 ℃ and it to be carried out surface fluorination handled 20 minutes.Promptly get the high acidproof polyimide fiber of fluoridizing after adopting nitrogen repeatedly to replace the still reaction gases then.
This stretching strength retentivity of fluoridizing fiber is 95%.
Embodiment 2
It is 50KPa that present embodiment removes fluorine gas dividing potential drop in vacuum reactor, and is warming up under 50 ℃ the condition and fluoridizes outside 1 minute, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 95%.
Embodiment 3
It is 100KPa that present embodiment removes fluorine gas dividing potential drop in vacuum reactor, and is warming up under 5 ℃ the condition and fluoridizes outside 5 minutes, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 97%.
Embodiment 4
It is 5KPa that present embodiment removes fluorine gas dividing potential drop in vacuum reactor, and is warming up under 100 ℃ the condition and fluoridizes outside 10 minutes, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 96%.
Embodiment 5
It is 30KPa that present embodiment removes fluorine gas dividing potential drop in vacuum reactor, and is warming up under 50 ℃ the condition and fluoridizes outside 10 minutes, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 96%.
Embodiment 6
It is fluorine gas/argon gas that present embodiment removes the fluorine gas gaseous mixture, and fluorine gas dividing potential drop in vacuum reactor is 40KPa, and is warming up under 60 ℃ the condition and fluoridizes outside 30 minutes, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 98%.
Embodiment 7
It is 25KPa that present embodiment removes fluorine gas dividing potential drop in vacuum reactor, and is warming up under 25 ℃ the condition and fluoridizes outside 10 minutes, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 95%.
Embodiment 8
It is 30KPa that present embodiment removes fluorine gas dividing potential drop in vacuum reactor, and is warming up under 60 ℃ the condition and fluoridizes outside 10 minutes, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 98%.
Embodiment 9
It is 40KPa that present embodiment removes fluorine gas dividing potential drop in vacuum reactor, and is warming up under 60 ℃ the condition and fluoridizes outside 30 minutes, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 96%.
It is 30KPa that present embodiment removes fluorine gas dividing potential drop in tubular reactor, and is warming up under 100 ℃ the condition and fluoridizes outside 1 minute, and all the other technologies are not stated so omit because of identical with embodiment 1.
This stretching strength retentivity of fluoridizing fiber is 94%.
Comparative Examples
Directly polyimide fiber being immersed in concentration is after accelerated ageing is handled 240 hours in the 20wt% aqueous sulfuric acid, carries out the TENSILE STRENGTH test after cleaning repeatedly, dry with distilled water.
The stretching strength retentivity of this fiber is 76%.
Claims (4)
1. one kind high acidproof polyimide fiber is characterized in that carbon-fluorine covalent bond structure is contained on the surface of this fiber; Its transmitted infrared light spectrogram is at 1780cm
-1, 1720cm
-1And 1380cm
-1Near the characteristic absorption peak of polyimides is arranged, the attenuated total reflectance infrared spectrogram is at 1100～1300cm
-1The absworption peak that carbon-fluorine covalent bond is arranged; Its x-ray photoelectron can have fluorine element power spectrum peak by spectrogram near the 688eV binding energy; It is that the stretching strength retentivity of immersion treatment after 240 hours is 94～98% in the 20wt% aqueous sulfuric acid in concentration.
2. method for preparing the acidproof polyimide fiber of the described height of claim 1; It is characterized in that this method is earlier polyimide fiber to be placed reactor; Then under the atmosphere of inert gases; In reactor, charge into the fluorine gas gaseous mixture, and under 5～100 ℃ of temperature, fluorination treatment was carried out 1～60 minute in its surface, promptly obtain the polyimide fiber that carbon-fluorine covalent bond structure is contained on the surface; Wherein the fluorine gas gaseous mixture is made up of in fluorine gas and nitrogen, argon gas, helium or the carbon dioxide any, and the dividing potential drop of fluorine gas in reactor remains 5～100Kpa.
3. the preparation method of the acidproof polyimide fiber of height according to claim 2, the fluorination reaction temperature that it is characterized in that this method is 25-60 ℃, the fluorination reaction time is 5～20 minutes.
4. according to the preparation method of claim 2 or the acidproof polyimide fiber of 3 described height, it is characterized in that fluorine gas dividing potential drop in reactor is 10～50KPa in this method.
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| CN102587058B (en) * | 2012-02-28 | 2013-07-10 | 四川大学 | Direct fluorination method for producing surface fluorine-containing fiber |
| CN105821655B (en) * | 2016-05-16 | 2017-11-07 | 四川大学 | A kind of aromatic polymer fiber of high composite performance and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101697049A (en) * | 2009-10-23 | 2010-04-21 | 四川大学 | Polyimide liquid crystal direct action membrane with fluorine-contained surface and preparation method thereof |
| CN101798748A (en) * | 2010-02-10 | 2010-08-11 | 成都百塑高分子科技有限公司 | Aramid III fiber with fluorine-containing surface and preparation method thereof |
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| DE10239004B4 (en) * | 2002-08-26 | 2007-11-15 | Performance Fibers Gmbh | Textile fabrics made of synthetic fibers, process for its production and its use |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101697049A (en) * | 2009-10-23 | 2010-04-21 | 四川大学 | Polyimide liquid crystal direct action membrane with fluorine-contained surface and preparation method thereof |
| CN101798748A (en) * | 2010-02-10 | 2010-08-11 | 成都百塑高分子科技有限公司 | Aramid III fiber with fluorine-containing surface and preparation method thereof |
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