CN101525785B - Fibre and method for forming same - Google Patents
Fibre and method for forming same Download PDFInfo
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- CN101525785B CN101525785B CN2008100816851A CN200810081685A CN101525785B CN 101525785 B CN101525785 B CN 101525785B CN 2008100816851 A CN2008100816851 A CN 2008100816851A CN 200810081685 A CN200810081685 A CN 200810081685A CN 101525785 B CN101525785 B CN 101525785B
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Abstract
The invention discloses a fibre and a method for forming the same. The fibre comprises a polyester fibre and a plurality of nanometer carbon tubes dispersed in the polyester fibre, wherein the nanometer carbon tubes are mainly cis-arranged in the extending direction of the polyester fibre in sequence. The method guides the nanometer carbon tubes with flexural structures to the polyester fibre and can remarkably increase the thermal resistance of the polyester fibre. The addition of the nanometer carbon tubes can also control the strength, the wearing resistance and the elongation so as to meet the requirement on various applications.
Description
Technical field
The present invention relates to a kind of fiber, and relate in particular to the polyester fiber that contains CNT.
Background technology
In the application of industrial fiber, polyester fiber is the important materials of using always.The application surface of polyester fiber is very wide, for example tire cord, transport tape, tarpaulin, sail cloth, camp or the like.These use used fiber need have high strength, flatness degree, and character such as abrasion performance.
In order further to promote the quality and the application surface of polyester fiber, need manage to increase the intensity and the abrasion performance characteristic of polyester fiber, and lower its degree of stretching.In addition, also need manage to promote the glass transition temperature and the crystallisation by cooling temperature of polyester fiber.The lifting of glass transition temperature helps to improve the heat endurance of polyester fiber, makes environment that its application product can be applicable to that temperature is higher and softening, increases range of application.The lifting of crystallisation by cooling temperature can impel polyester fiber in technology, just to begin crystallization in higher temperature, can make crystallization rate accelerate also can obtain the more polyester fiber of crystalline phase, helps the intensity of fortifying fibre.
Except the application of above-mentioned flatness degree fiber, industry also has the demand than the heat resistance fiber of high ductility.
Therefore, industry is needed the polyester fiber and the method for making thereof of high thermal stability badly, and the intensity of polyester fiber, degree of stretching, and abrasion resistance also want can change easily to meet the demand of various different application.
Summary of the invention
Technical problem to be solved by this invention is fiber that provides a kind of high thermal stability and forming method thereof, and the intensity of fiber, degree of stretching, and abrasion resistance also want can change easily to meet the demand of various different application.
For realizing above-mentioned purpose, the present invention provides a kind of fiber, comprises polyester fiber, and is scattered in a plurality of CNTs in the polyester fiber, and wherein on the whole CNT forward is arranged in the bearing of trend of polyester fiber.
And; For realizing above-mentioned purpose, the present invention provides a kind of method that forms fiber in addition, and comprising provides the polyester grain; A plurality of CNTs are provided; CNT and polyester grain are carried out mixing, and carry out fusion for the CNT after mixing and polyester grain and reel off raw silk from cocoons and obtain polyester fiber, wherein on the whole CNT forward is arranged in the polyester fiber.
In sum, the present invention has CNT around bent structure in polyester fiber through importing, can increase the heat-resisting character of polyester fiber significantly.Intensity, abrasion performance degree and the degree of stretching that also can control polyester/nano carbon pipe fiber through the interpolation of CNT are to meet various demands of applications.
Describe the present invention below in conjunction with accompanying drawing and specific embodiment, but not as to qualification of the present invention.
Description of drawings
Fig. 1 is a kind of SEM photo of winding carved CNT;
Fig. 2 a～Fig. 2 b is the SEM photo of PET/CNT fiber among the embodiment;
Fig. 3 is a kind of low around the SEM of bent CNT photo.
The specific embodiment
The present invention provides a kind of polyester fiber and method for making thereof at this.Mainly be that (carbonnanotube CNT) imports in the polyester fiber and increases the heat endurance of polyester fiber with CNT.And intensity, ABRASION RESISTANCE and the degree of stretching that can regulate fiber through different CNT additions increase its range of application to meet various demands of applications.
Polyester fiber provided by the present invention is of wide application, and for example can be used for tire cord, transport tape, tarpaulin, sail cloth, camp or various textile fibers etc.Particularly high strength, high abrasion, flatness degree, and the application of high heat stability degree are arranged about need.In addition, part embodiment of the present invention also can obtain to have the fiber of high heat stability degree and high ductility.Can be for example as the elastomer under the higher temperature environment.
In order to improve each item character of polyester fiber, the present invention imports CNT in the polyester fiber, utilizes mixing mode, and CNT is fully mixed with the polyester grain.Then gained polyester grain/CNT mixed ester grain is carried out fusion and disperse to reel off raw silk from cocoons, and obtain polyester/nano carbon pipe fiber.Through kind and the addition of suitably selecting CNT for use, and cooperate proper technical conditions, on the whole CNT is forward arranged along the bearing of trend of polyester fiber, can overcome CNT when reeling off raw silk from cocoons and assemble and produce the problem that fracture of wire can't moulding.Utilize the characteristic such as small size, high strength, high tenacity, high conductivity, high fineness ratio of CNT, can increase the intensity of polyester fiber effectively, and its ABRASION RESISTANCE and heat endurance are significantly promoted.
Below, the formation method of the fiber of the embodiment of the invention is provided.At first provide in order to form the polyester grain of polyester fiber; The material of polyester grain can comprise PETG (polyethyleneterephthalate; PET), polybutylene terephthalate (PBT) (polybutylene terephthalate; PBT), polytrimethylene terephthalate (polypropylene terephthalate; PPT), Aromatic polyester (Polyarylate, PAR), PETG (Glycol modifiedpolyethylene terephthalate PETG) etc. or aforesaid combination.Then, can the CNT of polyester grain with trace evenly be mixed through the various suitable method of prior art.For example can adopt twin-screw mixer machine, single screw mixing machine, single screw rod extruder, twin-screw extruder, ten thousand horsepowers of machines, continuous mixer or aforesaid combinations the polyester grain fully to be mixed and forms the mixed polyester grain of polyester/nano carbon pipe with CNT.The addition of CNT can be about 0.05phr to about 1phr with respect to the polyester grain.The diameter of the CNT that is fit to can be about 10 nanometers to about 40 nanometers, and the length that is fit to can be about 1 micron to about 25 microns.The CNT that is fit to also can have various degree different around bent structure.
Then, the ester grain after mixing being carried out fusion reels off raw silk from cocoons and can obtain polyester/nano carbon pipe fiber.For example; Can the ester grain after mixing be put into the spinning reative cell (spinning chamber) of heating and through spinning head ejection or flow out, the hole that can for example have about 0.005 inch of several diameters to about 0.030 inch in the spinning head is for fiber moulding by hole ejection or outflow.Can use forced air air-flow for example that the polyester/nano carbon pipe fiber of ejection melting attitude is quickly cooled to its glass from hardening into silk below the conversion temperature in the process of fiberizing.A formed polyester/nano carbon pipe fiber winding drum capable of using is collected.The winding speed of winding drum can be for example about 1000 meters/minute to about 6000 meters/minute.Fusion reel off raw silk from cocoons the temperature that adopted can be for example between about 200 ℃ to about 300 ℃.The ester grain extracts in the process of silk through melting; May form along fiber along the tensile stress (for example the pulling force of air draught and friction are at the stress that process caused of fiber hardening by cooling) that stretch direction polyester fiber and inner CNT thereof, this tensile stress may be impelled CNT on the whole to stretch direction along the edge of fiber forward to arrange.
The heat resisting temperature (being glass transition temperature) of the polyester/nano carbon pipe fiber of the embodiment of the invention can be greater than about 86 ℃, and it is about 12% that intensity can promote, and degree of stretching is less than about 27.9%, and abrasion performance intensity can promote about 41%.In addition, the polyester/nano carbon pipe fiber of the embodiment of the invention can reel off raw silk from cocoons continuously and make its length can be greater than about more than 100 meters.For example, can per minute 800 meters speed reeled off raw silk from cocoons continuously 5 minutes and obtain the about 4000 meters polyester/nano carbon pipe fiber of length.Can optionally obtain the polyester/nano carbon pipe fiber of Len req with the different speed of reeling off raw silk from cocoons.
The size of the CNT that imports, kenel, and addition very big to the property effect of polyester/nano carbon pipe fiber.The present invention has CNT around bent structure in polyester fiber through importing, can increase the heat-resisting character of polyester fiber significantly.The less CNT of caliber can use the fiber of the CNT that caliber is bigger around Qu Chengdu is lower that higher heat stability arranged around Qu Chengdu is big in the polyester/nano carbon pipe fiber employing of one embodiment of the invention.Addition through the control CNT can make CNT on the whole forward be arranged in the bearing of trend of polyester fiber, and the moulding of can reeling off raw silk from cocoons smoothly.Suitable CNT addition can make the polyester fiber strength enhancing and degree of stretching decline.The less polyester fiber of addition can have higher degree of stretching and good heat resistance.In addition, CNT also can optionally adjust around degree or its size (comprising caliber and length) of song.The CNT that is imported also not necessarily only limits to a kind of structure or form, for example can import two or morely to have different-diameter, different length, different CNT around curvature or different additions in fiber.Below, will enumerate embodiments of the invention explanation.
Embodiment 1
Get about 100 grams of PET ester grain and mix with the CNT of 0.15g, 0.3g, 0.5g, 1g, through twin-screw mixer with the full and uniform mixed polyester grain that mixes and form PET/CNT of CNT (CNT) and PET ester grain.Among this embodiment, the screw diameter of used twin-screw mixer machine is about 45 millimeters (mm), and its draw ratio (L/D) is about 30, and screw speed is about 200rpm.Adopt ten sections temperature to carry out twin-screw mixer altogether, be respectively 180 ℃, 210 ℃, 230 ℃, 240 ℃, 250 ℃, 250 ℃, 260 ℃, 260 ℃, 260 ℃, reach 250 ℃.In this embodiment, the CNT that is adopted belongs to winding carved, and its SEM photo is shown among Fig. 1, and its diameter is about 20nm, and its length is about 1 micron to about 25 microns, and its structure is that essence is around song.The addition of CNT is respectively about 0phr to about 1phr with respect to PET ester grain.Then, to the PET/CNT ester grain after the twin-screw mixer carry out fusion reel off raw silk from cocoons (fusion reel off raw silk from cocoons temperature be about 270 ℃ to about 280 ℃) obtain the PET/CNT fiber.
Fig. 2 a shows the SEM photo of PET/CNT fiber, and Fig. 2 b shows the SEM photo of the PET/CNT fiber that enlargement ratio is higher.Shown in Fig. 2 a and Fig. 2 b, on the whole CNT forward is arranged in the bearing of trend of PET fiber, and still part is possessed it around bent structure.Via the addition and the control of process parameters of the size of suitably selecting CNT for use, control CNT, on the whole gained PET/CNT fiber forward is arranged in the bearing of trend of fiber and is not easy fracture of wire, and the shaping of can reeling off raw silk from cocoons smoothly.For example reeled off raw silk from cocoons 5 minutes, and obtain length greater than about 4000 meters fiber with 800 meters/minute speed.Table one is listed each item material character of the PET/CNT fiber that has different winding carved CNT additions among this embodiment, and each item character that lists file names with the PET fiber that does not contain CNT is for relatively.
Table one
| Winding carved CNT content | Tm (℃) | Tg (℃) | Tcc (℃) | Fineness (den) | Abrasion (%) | Intensity (g/d) | Degree of stretching (%) |
| PET(blank) | 250 | 70 | 186 | 612 | 0.161 | 1.74±0.4 | 67.2±31.9 |
| 0.15phr | 259 | 86 | 209 | 577 | - | 1.32±0.3 | 102.8±46.1 |
| 0.3phr | 258 | 85 | 207 | 583 | - | 1.53±0.08 | 100.2±3.6 |
| 0.5phr | 260 | 84 | 206 | 560 | 0.103 | 1.95±0.12 | 33.8±4.9 |
| 1phr | 258 | 83 | 211 | - | 0.096 | - | - |
Wherein, phr (part per hundred resin): the gram number that adds other additives in per 100 gram polyester; Den (red Buddhist nun's number): the weight kilogram number of per 9000 meters fibers.
Shown in table one, can find out that the importing of winding carved CNT can promote the heat endurance of PET fiber significantly.The glass transition temperature of PET/CNT fiber (Tg) can promote at least about more than 10 ℃ compared to PET (blank) fiber, can improve the heat resisting temperature (greater than about 70 ℃) of fiber, and enable application is in the environment of higher temperatures.Except glass transition temperature, the crystallisation by cooling temperature (Tcc) of PET/CNT fiber has also promoted about more than 20 ℃ compared to PET (blank) fiber.The lifting of crystallisation by cooling temperature can impel the fusion fiber that reels off raw silk from cocoons just to begin crystallization in higher chilling temperature, crystallization rate is accelerated and is obtained the more fiber of crystalline phase, helps to promote the intensity of fiber.The reason of PET/CNT fiber crystallisation by cooling temperature increase it be not immediately clear; Do not get rid of is because the interpolation of winding carved CNT has formed many CNT/PET interfaces; PET is easy near interface and produces heterogeneous nucleation, crystallization is early taken place, thereby improved the crystallisation by cooling temperature.When the addition of winding carved CNT increases to 0.5phr; The intensity of PET/CNT fiber begins to reach about 1.95 ± 0.12g/d greater than 1.74 ± 0.4g/d of PET (blank) fiber, and its degree of stretching significantly is reduced to 33.8 ± 4.9% compared to 67.2 ± 31.9% of PET (blank) fiber.Wherein, the about 0.15phr of CNT content has preferable heat endurance to the fiber of about 0.3phr, but its intensity is lower and degree of stretching is higher, and its reason it be not immediately clear.The fiber that these are more heat-resisting and degree of stretching is higher still can have many other to use, and for example can be used as the elastomer under the higher temperature environment.Table one is also listed the abrasion performance assay of part PET/CNT fiber; It shows that each fiber is under identical abrasion condition; The percentage by weight (before the abrasion of ratio) that is worn and torn can be found from table one, along with the lifting of CNT addition; Can effectively reduce the abrasion loss (reducing about more than 35%) of PET/CNT fiber, promote its abrasion performance degree.Wherein, CNT content be 0.5phr with the PET/CNT fiber of 0.1phr under identical abrasion condition, the PET (blank) of its abrasion loss ratio has reduced 35.627% and 40.277% respectively, more helps the application of PET/CNT fiber under higher abrasion environment.
Embodiment 2
Prepare the PET/CNT fiber among the embodiment 2 with the mode that is same as embodiment 1, only the winding carved CNT among the embodiment is replaced with lower and that diameter is bigger is low around bent CNT around Qu Chengdu.Used hanging down is shown among Fig. 3 around the SEM of bent CNT photo among this embodiment, and its diameter is extremely about 90nm of about 30nm, and its length is about 1 micron to about 2 microns.Each item character of the PET/CNT fiber of gained is listed in the table two.
Table two
| Low around bent CNT content | Tm(℃) | Tg(℃) | Tcc(℃) |
| PET(blank) | 250 | 70 | 186 |
| 0.3phr | 222 | 72 | 175 |
| 1phr | 246 | 78 | 195 |
Wherein, Den (red Buddhist nun's number): the weight kilogram number of per 9000 meters fibers.
Shown in table two, import low heat endurance and also can obtain to promote around the PET/CNT of bent CNT fiber.Along with hanging down when the addition of bent CNT increases to 1phr, its glass transition temperature (Tg) can increase to about 78 ℃, and its crystallisation by cooling temperature (Tcc) can increase to about 195 ℃.Comparison sheet one can find out that with table two adding the low amplitude that is promoted around the glass transition temperature or the crystallisation by cooling temperature of the PET/CNT of bent CNT fiber is significantly less than the PET/CNT fiber that adds winding carved CNT.Its reason it be not immediately clear; Do not get rid of be because among the embodiment 2 among the embodiment 1 of used CNT ratio used CNT have bigger diameter with more not around the structure of song; Less around the CNT of song than major diameter with the area of the contact interface of PET fiber on every side with more not; Therefore the nucleating point of heterogeneous nucleation is less between PET and CNT, causes amplitude that the crystallisation by cooling temperature increases less and around the PET/CNT of song fiber less than the diameter that adopts CNT.
By embodiment 1 and embodiment 2 can know CNT pattern (as around Qu Chengdu), size, and addition influence the character of polyester fiber very huge, can selecting for use and add each item character of adjusting polyester fiber through CNT.
In sum, the present invention has CNT around bent structure in polyester fiber through importing, can increase the heat-resisting character of polyester fiber significantly.Intensity, abrasion performance degree and the degree of stretching that also can control polyester/nano carbon pipe fiber through the interpolation of CNT are to meet various demands of applications.Wherein, add 0.5phr has 84 ℃ glass transition temperature (exceeding 14 ℃ than PET blank), 1.95 ± 0.12g/d around the PET/CNT of bent CNT fiber intensity (exceeding about 12%), and about degree of stretching of 33% (being about the half the of PET blank degree of stretching) than PET blank.In addition, the abrasion performance degree of PET/CNT fiber also can improve along with the increase of CNT addition, helps the application of PET/CNT fiber under higher abrasion environment.
Certainly; The present invention also can have other various embodiments; Under the situation that does not deviate from spirit of the present invention and essence thereof; Those of ordinary skill in the art work as can make various corresponding changes and distortion according to the present invention, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (11)
1. a fiber is characterized in that, comprising:
One polyester fiber; And
A plurality of CNTs; Be scattered in this polyester fiber; And on the whole those CNTs forward are arranged in the bearing of trend of this polyester fiber, and wherein the diameter of those CNTs is 10 nanometer to 40 nanometers, and the length of those CNTs is 1 micron to 25 microns; Those CNTs have one around bent structure, and the content that per 100 grams of this polyester fiber have those CNTs is that 0.05 gram is to 1 gram;
The said polyester fiber that is dispersed with CNT reels off raw silk from cocoons through fusion and utilizes a winding drum to collect and obtains, and the winding speed of said winding drum is 1000 meters/minute to 6000 meters/minute.
2. fiber according to claim 1 is characterized in that, the material of this polyester fiber comprises PETG, polybutylene terephthalate (PBT), polytrimethylene terephthalate, Aromatic polyester or aforesaid combination.
3. a method that forms the described fiber of claim 1 is characterized in that, comprising:
One polyester grain is provided;
A plurality of CNTs are provided;
This CNT and this polyester grain are carried out one mixing; And
This CNT for this after mixing and this polyester grain carry out a fusion and reel off raw silk from cocoons and utilize a winding drum to collect and obtain a polyester/nano carbon pipe fiber, and wherein, the winding speed of said winding drum is 1000 meters/minute to 6000 meters/minute;
On the whole those CNTs forward are arranged in this polyester/nano carbon pipe fiber.
4. the method for the described fiber of formation claim 1 according to claim 3; It is characterized in that the material of this polyester grain comprises PETG, polybutylene terephthalate (PBT), polytrimethylene terephthalate, Aromatic polyester or aforesaid combination.
5. the method for the described fiber of formation claim 1 according to claim 3 is characterized in that, the diameter of those CNTs is 10 nanometer to 40 nanometers.
6. the method for the described fiber of formation claim 1 according to claim 3 is characterized in that, the length of those CNTs is 1 micron to 25 microns.
7. the method for the described fiber of formation claim 1 according to claim 3 is characterized in that, those CNTs that forward are arranged in this polyester/nano carbon pipe fiber have one around bent structure.
8. the method for the described fiber of formation claim 1 according to claim 3 is characterized in that, being provided as of this polyester grain and those CNTs whenever provides this polyester grain of 100 grams, and those CNTs of 0.05 gram to 1 gram just are provided.
9. the method for the described fiber of formation claim 1 according to claim 3 is characterized in that, the heat resisting temperature of this polyester/nano carbon pipe fiber is greater than 70 ℃.
10. the method for the described fiber of formation claim 1 according to claim 3 is characterized in that, this polyester/nano carbon pipe fiber reduces more than 35% than the polyester fiber abrasion loss that does not comprise CNT under identical abrasion condition.
11. the method for the described fiber of formation claim 1 according to claim 3 is characterized in that, the length of this polyester/nano carbon pipe fiber is greater than 100 meters.
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| CN2008100816851A CN101525785B (en) | 2008-03-05 | 2008-03-05 | Fibre and method for forming same |
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| CN2008100816851A CN101525785B (en) | 2008-03-05 | 2008-03-05 | Fibre and method for forming same |
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| CN101525785B true CN101525785B (en) | 2012-05-23 |
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| CN104264270A (en) * | 2014-10-13 | 2015-01-07 | 张家港市安顺科技发展有限公司 | Carbon nano tube regenerated polyester staple fiber production method |
| CN108950864A (en) * | 2018-07-27 | 2018-12-07 | 望江汇通纺织有限公司 | A kind of medical sheath core fiber non-woven fabrics of hydrophilic and oleophilic |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1869291A (en) * | 2005-05-23 | 2006-11-29 | 中国科学院化学研究所 | Fibre structure of polyester/carbone nanotube nano composite and its preparation method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1869291A (en) * | 2005-05-23 | 2006-11-29 | 中国科学院化学研究所 | Fibre structure of polyester/carbone nanotube nano composite and its preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 沈锂鸣等.多壁碳纳米管增强PET纤维的初步研究.《合成纤维》.2007,(第10期),23－26. * |
| 钱建华等.添加碳纳米管聚酯母粒的制备及性能.《纺织学报》.2005,第26卷(第3期),21-23. * |
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