CN104911732B - A kind of many defect carbon pipe hybridized fibers of PPS/ and preparation method thereof - Google Patents
A kind of many defect carbon pipe hybridized fibers of PPS/ and preparation method thereof Download PDFInfo
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- CN104911732B CN104911732B CN201510332160.0A CN201510332160A CN104911732B CN 104911732 B CN104911732 B CN 104911732B CN 201510332160 A CN201510332160 A CN 201510332160A CN 104911732 B CN104911732 B CN 104911732B
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Abstract
The present invention relates to many defect carbon pipe hybridized fibers of a kind of PPS/ and preparation method thereof, by mass percentage, hybridized fiber component is polyphenylene thioether PPS section 95 99.9%, many defect carbon pipes 0.1 5%.By dry many defect carbon pipes and PPS section extruding pelletizations, many defect carbon pipe hydridization sections of PPS/ are obtained, is dried, is then carried out spinning winding, obtain spun filament, drawing-off is produced.The many defect carbon pipe hybridized fibers of PPS/ of the present invention have stronger fracture strength；After xenon lamp aging processing 480h, higher mechanical property conservation rate is still kept, is 55.9 92.6%.
Description
Technical field
The invention belongs to hybridized fiber and its preparation field, more particularly to a kind of many defect carbon pipe hybridized fibers of PPS/ and its
Preparation method.
Background technology
PPS fibers are a kind of high-temperature fibres of exploitation at the beginning of the eighties, rotten with good heat resistance, excellent chemically-resistant
Corrosion and anti-flammability, have broad application prospects in necks such as military project, high temperature filtration, chemical protections.At present, the master of PPS fibers
It is used for the filtration fabrics of the coal-burning boiler bag house such as thermal power plant, steel plant.PPS fibers can be rotten in high temperature, high humidity and height
It is used for a long time under the conditions of the extremely rugged environment such as corrosion gas, as the filtrate of sack cleaner under the conditions of worst hot case,
Dedusting, thermal power plant and coal-burned industrial boiler dedusting, dedusting of waste incineration through being successfully applied to the ferroalloy industry etc., its sexual valence
Than high, dust removing effects are good.Nomex band, which is made, in this external application fiber is used in the drying belt of paper industry, is ideal
Heat-resisting and resistant material, simultaneously can be used for make electronics industry special type paper, the needle fabric of this fiber or
Woven fabric can be used for the filtering of the corrosive reagents of heat.
PPS has stronger UV-resistance.After ultraviolet irradiation, PPS macromolecular chains absorb photoelectron, and strand holds
Easily by dioxygen oxidation in air；Ar-S weak bonds are broken, and Photogenerated Radicals further crosslink reaction with macromolecular chain, no
It is disconnected to occur oxidation cross-linked degradation reaction；Macroscopically cause PPS product xanthochromias, under also resulting in the mechanical strengths of PPS products drastically
Drop, fragility is big.This causes current PPS fibers to be only capable of the field application in light protected environment.
At present, the research both at home and abroad on improving PPS fiber photostability is few, and improves the effect of its photostability and have
Limit.Patent CN102268751A, CN102839446A, CN102477594A use benzotriazole derivatives, triazines ultraviolet light
Stabilizer, hindered amine free raical quencher and its compound system are modified to PPS fibers, but in PPS fiber manufacturing process, drop
Solution generation sulfur-containing radicals, easily influence the light stablizing effect of its organic ultraviolet light stabilizer；And inhaled as organic ultraviolet
Agent is received, its heat endurance and solvent resistant extracting property are poor, it is difficult to reach efficiently permanent ultraviolet light stabilized effect.
CN101126182A, CN102677218A fill nano titanium oxide and benzotriazole derivatives, and PPS fibers are modified and ground
Study carefully.But, the nano-titanium dioxide modified effect of low content is limited, and the potential photocatalysis performance of nano titanium oxide, it is impossible to real
The long-term efficient photostability of existing PPS fibers.Sichuan University professor Ye Guangdou filling nano carbon black be modified, mechanical property and
Ultraviolet light stability still has much room for improvement.Therefore, new modified filler is developed, the higher fracture strength of PPS fibers is assigned and ultraviolet
Photostability, improves the service life of PPS fibres.
The content of the invention
The technical problems to be solved by the invention are to provide many defect carbon pipe hybridized fibers of a kind of PPS/ and preparation method thereof,
The many defect carbon pipe hybridized fibers of PPS/ of the present invention have stronger fracture strength；After xenon lamp aging processing 480h, still keep
Higher mechanical property conservation rate, is 55.9-92.6%.
A kind of many defect carbon pipe hybridized fibers of PPS/ of the present invention, it is characterised in that：By mass percentage, hybridized fiber group
It is divided into PPS sections 95-99.9%, many defect carbon pipe 0.1-5%.
The PPS sections are spinning-grade PPS sections (Ticona company of the U.S.), and relative molecular mass is 3-5 ten thousand.
A diameter of 5-10nm of many defect carbon pipes, length is 0.5-2 μm.
Many defect carbon pipes are：Nitric acid, Piranha solution, mixed acid etc. are heated to reflux after oxidation, and functionalization is gone by high temperature
Multi-walled carbon nanotube, D peaks and G peak intensities in its Raman spectrum compare ID：IG=0.8-1.1.
A kind of preparation method of many defect carbon pipe hybridized fibers of PPS/ of the present invention, including：
(1) multi-walled carbon nanotube is added in oxidizing acidic solution, the reflux condensation mode 2h under the conditions of 80 DEG C, filter, wash,
Dry, obtain oxidation multi-wall carbon nano-tube tube；Then the oxidation multi-wall carbon nano-tube tube of preparation is carried out going function dough to handle, ball
Mill, obtains many defect carbon pipes；
(2) by dry many defect carbon pipes and PPS section extruding pelletizations, many defect carbon pipe hydridization sections of PPS/ is obtained, are done
It is dry, spinning winding is then carried out, spun filament is obtained, drawing-off produces many defect carbon pipe hybridized fibers of PPS/.
Multi-walled carbon nanotube (product of Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences), diameter in the step (1)
For 5-10nm, length<2μm.
The length of the multi-walled carbon nanotube is 0.5-2 μm.
Oxidizing acidic solution is the one or more in concentrated nitric acid, concentrated nitric acid, Piranha solution in the step (1).
Gone in the step (1) function dough processing be specially：Oxidation multi-wall carbon nano-tube tube is added in alumina crucible, is put
In tube furnace, in N2Under atmosphere, 800-850 DEG C is warming up to 2-3 DEG C/min speed, goes function dough to handle 80-120min.
Extruding pelletization is to be granulated in double screw extruder in the step (2).
Spinning winding stretching is specially in the step (2)：In apparatus for melt spinning, extruder temperature is 315-325 DEG C,
Screw rod fusion pressure be 60-120bar under conditions of, using 600-1000m/min spinning speed carry out spinning winding stretching；Drawing-off
3.6-4.3 again.
Beneficial effect
The many defect carbon pipe composite fibres of PPS/ of the present invention, fracture strength is 3.0-3.56cN/dtex, and elongation at break is
15.3-29.2%.Kept after xenon lamp aging processing after the mechanical strength of PPS fibers, processing 192h, rupture strength retention is
After 85.53-100%, processing 480h, rupture strength retention is 60.56-91.24%.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
Length is added into salpeter solution for 0.5-2 μm of multi-walled carbon nanotube, 80 DEG C of reflux condensation mode 2h, filtering, water
Wash, dry after, obtain oxidation multi-wall carbon nano-tube tube；Then the oxidation multi-wall carbon nano-tube tube of preparation is added in alumina crucible,
It is placed in high temperature process furnances, in N2Under atmosphere, 850 DEG C are warming up to 2 DEG C/min speed, goes function dough to handle 120min,
It is levigate in ball mill, obtain many defect carbon pipes.
Then dried powder and section are put into double screw extruder and granulated, many defect carbon pipe hydridization of PPS/ are made
Section；The content of many defect carbon pipes is that the content of 0.1%, PPS sections is 99.9%.
The many defect carbon pipe hydridization sections of PPS/ after after drying are added in apparatus for melt spinning again, using 600m/min's
Spinning speed carries out spinning winding stretching and spun filament is made, and PPS UDY-DT fibers are prepared by first break draft.
The spinning technique of melt spinning is as follows：
Screw Extrusion temperature：315-325℃；
Spin manifold temperature：3315-325℃；
Screw pressure：<70kgf/cm2；
Component pressure：<60kgf/cm2；
Winding speed：600m/min；
Drafting multiple：4.3 again.
By characterizing, many defect carbon pipe composite fibres of PPS/ of the invention, fracture strength is 3.32cN/dtex, and fracture is stretched
Long rate is 29.2%, and after xenon lamp aging processing 196h, fibrous fracture strength retention is 87.80%, after processing 480h, is broken
Resistance to spalling conservation rate is 57.68%.
Embodiment 2
Length is added into Piranha solution for 0.5-2 μm of multi-walled carbon nanotube, 80 DEG C of reflux condensation mode 2h, filtering,
After washing, drying, oxidation multi-wall carbon nano-tube tube is obtained；Then the oxidation multi-wall carbon nano-tube tube of preparation is added into alumina crucible
In, it is placed in high temperature process furnances, in N2Under atmosphere, 850 DEG C are warming up to 2 DEG C/min speed, goes function dough to handle 120min,
It is levigate in ball mill, obtain many defect carbon pipes.
Then dried powder is put into double screw extruder and granulated, many defect carbon pipe hydridization sections of PPS/ are made；
The content of many defect carbon pipes is that the content of 0.1%, PPS sections is 99.90%.
Dried uvioresistant PPS sections are added in apparatus for melt spinning again, entered using 600m/min spinning speed
Spun filament is made in the stretching of row spinning winding, and PPS UDY-DT fibers are prepared by first break draft.
The spinning technique of melt spinning is as follows：
Screw Extrusion temperature：315-325℃；
Spin manifold temperature：315-325℃；
Screw pressure：<70kgf/cm2；
Component pressure：<60kgf/cm2；
Winding speed：600m/min；
Drafting multiple：4.3 again.
By characterizing, many defect carbon pipe composite fibres of PPS/ of the invention, fracture strength is 3.56cN/dtex, and fracture is stretched
Long rate is 29.2%, and after xenon lamp aging processing 196h, fibrous fracture strength retention is 85.53%, after processing 480h, is broken
Resistance to spalling conservation rate is 53.56%.
Embodiment 3
Length is added into salpeter solution for 0.5-2 μm of multi-walled carbon nanotube, 80 DEG C of reflux condensation mode 2h, filtering, water
Wash, dry after, obtain oxidation multi-wall carbon nano-tube tube；Then the carbonoxide pipe of preparation is added in alumina crucible, is placed in high temperature
In tube furnace, in N2Under atmosphere, 850 DEG C are warming up to 10 DEG C/min speed, thermal reduction 120min is levigate in ball mill, obtains
To many defect carbon pipes.
Then above-mentioned dried powder and section are put into double screw extruder and granulated, many defect carbon pipes of PPS/ are made
Compound slice；The compound content of many defect carbon pipes is that the content of 5.0%, PPS sections is 95.0%.
The many defect carbon pipe compound slices of dried PPS/ are added in apparatus for melt spinning again, using 1000m/min's
Spinning speed carries out spinning winding stretching and spun filament is made, and PPS UDY-DT fibers are prepared by first break draft.
The spinning technique of melt spinning is as follows：
Screw Extrusion temperature：315-325℃；
Spin manifold temperature：315-325℃；
Screw pressure：<70kgf/cm2；
Component pressure：<60kgf/cm2；
Winding speed：1000m/min；
Drafting multiple：3.8 again.
By characterizing, many defect carbon pipe composite fibres of PPS/ of the invention, fracture strength is 3.0cN/dtex, extension at break
Rate is 15.3%, and after xenon lamp aging processing 196h, fibrous fracture strength retention is 100%, and after processing 480h, fracture is strong
It is 91.24% to spend conservation rate.
Claims (10)
1. a kind of many defect carbon pipe hybridized fibers of PPS/, it is characterised in that：By mass percentage, hybridized fiber component is polyphenylene sulfide
Ether PPS sections 95-99.9%, many defect carbon pipe 0.1-5%.
2. many defect carbon pipe hybridized fibers of a kind of PPS/ according to claim 1, it is characterised in that：The PPS cuts into slices
Spinning-grade PPS cuts into slices, and relative molecular mass is 3-5 ten thousand.
3. many defect carbon pipe hybridized fibers of a kind of PPS/ according to claim 1, it is characterised in that：Many defect carbon pipes
A diameter of 5-10nm, length be 0.5-2 μm.
4. a kind of preparation method of many defect carbon pipe hybridized fibers of PPS/ as described in claim 1-3 is any, including：
(1) multi-walled carbon nanotube is added in oxidizing acidic solution, the reflux condensation mode 2h under the conditions of 80 DEG C, filters, washes, does
It is dry, obtain oxidation multi-wall carbon nano-tube tube；Then the oxidation multi-wall carbon nano-tube tube of preparation is carried out going function dough to handle, ball milling,
Obtain many defect carbon pipes；
(2) by dry many defect carbon pipes and PPS section extruding pelletizations, many defect carbon pipe hydridization sections of PPS/ is obtained, are dried, so
After carry out spinning winding, obtain spun filament, drawing-off produces many defect carbon pipe hybridized fibers of PPS/.
5. a kind of preparation method of many defect carbon pipe hybridized fibers of PPS/ according to claim 4, it is characterised in that：It is described
A diameter of 5-10nm of multi-walled carbon nanotube, length in step (1)<2μm.
6. a kind of preparation method of many defect carbon pipe hybridized fibers of PPS/ according to claim 5, it is characterised in that：It is described
The length of multi-walled carbon nanotube is 0.5-2 μm；Wherein the length of multi-walled carbon nanotube is not 2 μm.
7. a kind of preparation method of many defect carbon pipe hybridized fibers of PPS/ according to claim 4, it is characterised in that：It is described
Oxidizing acidic solution is the one or more in concentrated nitric acid, the concentrated sulfuric acid, Piranha solution in step (1).
8. a kind of preparation method of many defect carbon pipe hybridized fibers of PPS/ according to claim 4, it is characterised in that：It is described
Gone in step (1) function dough processing be specially：Oxidation multi-wall carbon nano-tube tube is added in alumina crucible, is placed in tube furnace,
In N2Under atmosphere, 800-850 DEG C is warming up to 2-3 DEG C/min speed, goes function dough to handle 80-120min.
9. a kind of preparation method of many defect carbon pipe hybridized fibers of PPS/ according to claim 4, it is characterised in that：It is described
Extruding pelletization is to be granulated in double screw extruder in step (2).
10. a kind of preparation method of many defect carbon pipe hybridized fibers of PPS/ according to claim 4, it is characterised in that：Institute
Stating spinning winding in step (2) is specially：In apparatus for melt spinning, extruder temperature is 315-325 DEG C, and screw rod fusion pressure is 60-
Under conditions of 120bar, spinning winding is carried out using 600-1000m/min spinning speed；Drafting multiple is 3.6-4.3 times.
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| CN107447288B (en) * | 2017-03-06 | 2020-04-07 | 东华大学 | Thermal-oxidative-aging-resistant PPS/large-lumen HNTs hybrid fiber and preparation method thereof |
| CN110409017B (en) * | 2019-08-12 | 2022-01-14 | 杭州高烯科技有限公司 | High-conductivity polyamide-polyester composite fiber and preparation method thereof |
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| CN101126182A (en) * | 2007-10-09 | 2008-02-20 | 东华大学 | Ultraviolet radiation resisting polyphenylene sulfide and preparation method thereof |
| CN102677218B (en) * | 2012-06-01 | 2014-05-28 | 东华大学 | Anti-ultraviolet polyphenyl thioether filament and preparation method thereof |
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