CN101864609A - Thermoplastic polymer micro-nanometer fiber and preparation method thereof - Google Patents
Thermoplastic polymer micro-nanometer fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to thermoplastic polymer micro-nanometer fiber and a preparation method thereof. The thermoplastic polymer micro-nanometer fiber comprises the ingredients of 100 percent thermoplastic polymers. The preparation comprises the following steps: (1) blending the thermoplastic polymers and polylactic acid or polyhydroxy alk acid ester, carrying out fused extrusion coiling by a double-screw spinning machine, and forming thermoplastic polymer/polylactic acid or thermoplastic polymer/polyhydroxy alk acid ester multi-ingredient blending fiber; and (2) dissolving the blending fiber into solvents, removing matrix phase polylactic acid or polyhydroxy alk acid ester, and obtaining the thermoplastic polymer micro-nanometer fiber. The fiber of the invention has the diameter ranged from 50 to 1000 nm. The preparation method is simple and efficient, and the mass production can be easily realized.
Description
Technical field
The invention belongs to polymer micro-nanometer fiber and preparation field thereof, particularly relate to a kind of thermoplastic polymer micro-nanometer fiber and preparation method thereof.
Background technology
Nanofiber is meant the fiber of diameter less than 100nm, and in fact people are referred to as nanofiber with electrostatic spinning or diameter that other preparation methods obtain less than the fiber of 1000nm.Because the special micro-nano-scale effect of nanofiber has extensive use field and huge commercial value.
The method for preparing nanofiber has: compound vapor deposition, masterplate polymerization and MOLECULE DESIGN method, spinning process method etc.The compound vapor deposition is mainly used in the inorganic and metal nano fiber of preparation; Masterplate polymerization and MOLECULE DESIGN method are the novel methods of preparation nanofiber, but efficient is lower; The spinning process method should be the most promising method of scale preparation polymer nanofiber, and the spinning process method mainly comprises method of electrostatic spinning, meltblown, flash method, composite spinning method etc.Method of electrostatic spinning is to prepare the most frequently used method of micro nanometer fiber at present, and right method of electrostatic spinning is strict to solution properties and machined parameters, and method of electrostatic spinning is primarily aimed at the solvent spinning system in addition.Though the fusion electrospinning can not be subjected to the restriction of solvent, because the diameter of the fiber that high viscosity obtains of molten high polymer is difficult to less than 500nm.Meltblown can prepare hybrid microscale and the very little superfine fibre of ultra micro meter ruler, mainly collects with the form of nonwoven fabric.Dong Li company adopts " indefinite island " composite spinning technology to prepare micrometer fibers, be " island " component mainly with polyamide, polyester etc., alkali soluble polyester is " sea " component, control by technology can obtain designed micro nanometer fiber after alkali lye dissolving " sea " component, applied for Chinese invention patent (200380105030.9).U.S. Hills company utilizes " deciding the island " composite spinning method to prepare micro nanometer fiber, the spinneret design complex process of " deciding the island " composite spinning method.
Summary of the invention
Technical problem to be solved by this invention provides a kind of thermoplastic polymer micro-nanometer fiber and preparation method thereof, and this method is simply efficient, and thermoplastic, polymeric materials is had the characteristic of universality, is easy to accomplish scale production.
A kind of thermoplastic polymer micro-nanometer fiber of the present invention, its component comprises: 100% thermoplastic polymer, described thermoplastic polymer is one or more the blend in polyethylene, polypropylene, polyamide, polytrimethylene terephthalate, the polybutylene terephthalate, or polyethylene to graft glycidyl methacrylate, polypropylene grafted maleic anhydride etc.
The diameter range of described thermoplastic polymer micro-nanometer fiber is 50～1000nm.
The preparation method of a kind of thermoplastic polymer micro-nanometer fiber of the present invention comprises:
(1) be (1-40) with mass ratio: thermoplastic polymer (60-99) and matrix blend mutually, melt extrude through the twin-screw spinning machine, be wound into fibre, form thermoplastic polymer/matrix phase multicomponent blended fiber;
(2) above-mentioned blended fiber is dissolved in the solvent, removes matrix phase PLA and polyhydroxy-alkanoate, promptly get thermoplastic polymer micro-nanometer fiber;
Described matrix is PLA or polyhydroxy-alkanoate mutually.
Described thermoplastic polymer is one or more the blend in polyethylene, polypropylene, polyamide, polyethylene terephthalate, polytrimethylene terephthalate, the polybutylene terephthalate, or polyethylene to graft glycidyl methacrylate, polypropylene grafted maleic anhydride etc.
Blending temperature in the described step (1) is 180 ℃-260 ℃.
Blending temperature in the described step (1) is: 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃ or 260 ℃.
Solvent in the described step (2) is carrene or chloroform.
In thermal plasticity high polymer of the present invention and PLA or the polyhydroxy-alkanoate melting process thermoplastic polymer as decentralized photo because the existence of inherent restraining factors such as external force field such as shear tension and temperature and ratio of component, ratio of viscosities can assemble in situ form micro nanometer fiber.
Beneficial effect
(1) diameter of thermoplastic polymer micro-nanometer fiber of the present invention is 50～1000nm;
(2) preparation method of the present invention is simply efficient, and thermoplastic, polymeric materials is had the characteristic of universality, has overcome different materials and has adopted different technology paths and cause complex process, equipment investment to require high weak point, is easy to accomplish scale production.
Description of drawings
Fig. 1 iPP/PLA blend composite fiber (mass ratio is 0.5: 9.5) is removed PLA back gained iPP micro nanometer fiber mutually;
Fig. 2 iPP/PLA blend composite fiber (mass ratio is 10: 90) is removed PLA back gained iPP micro nanometer fiber mutually;
Fig. 3 iPP/PLA blend composite fiber (mass ratio is 20: 80) is removed PLA back gained iPP micro nanometer fiber mutually;
Fig. 4 PE/PLA blend composite fiber (mass ratio is 20: 80) is removed PLA back gained PE micro nanometer fiber mutually;
Fig. 5 PTT/PLA blend composite fiber (mass ratio is 20: 80) is removed PLA back gained PTT micro nanometer fiber mutually.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
It is polypropene blended that the 1900 gram dried PLAs of vacuum drying oven and 100 restrain, and melt extrudes to reel through the twin-screw spinning machine again to obtain the polypropylene blended fiber.Processing temperature: 180 ℃, matrix phase constituent PLA in the blended fiber adopts chloroform to dissolve removal in Soxhlet extractor, promptly obtains polypropylene micro nanometer fiber material, is 50～500nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 2
Poly butyric ester after the 1950 gram vacuumizes and 50 gram polypropylene melt extrude the acquisition polypropylene/poly butyric ester blended fiber of reeling through twin-screw machine, and processing temperature is 180 ℃.Poly butyric ester in the blended fiber adopts the chloroform dissolving to obtain polypropylene micro nanometer fiber material, is 50～500nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 3
It is polypropene blended that the 1800 gram dried PLAs of vacuum drying oven and 200 restrain, and melt extrudes to reel through the twin-screw spinning machine again to obtain polypropylene blended fiber, processing temperature: 190 ℃.By the chloroform dissolving of heat, promptly obtaining polypropylene micro nanometer fiber material in the matrix phase constituent PLA in the blended fiber, is 50～600nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 4
Poly butyric valerate after the 1400 gram vacuumizes and 600 gram polypropylene melt extrude the acquisition polypropylene/poly butyric valerate blended fiber of reeling through twin-screw machine, and processing temperature is 190 ℃.Poly butyric valerate in the blended fiber adopts the chloroform dissolving promptly to obtain polypropylene micro nanometer fiber material, is 100～700nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 5
It is polypropene blended that the 1600 gram dried PLAs of vacuum drying oven and 400 restrain, and melt extrudes to reel through the twin-screw spinning machine again to obtain polypropylene blended fiber, processing temperature: 200 ℃.PLA matrix in the blended fiber through the dissolving of 60 ℃ of chloroforms, promptly obtains polypropylene micro nanometer fiber material in dissolution kettle, be 100～600nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 6
Poly butyric valerate after the 1600 gram vacuumizes and 400 gram polyethylene blends melt extrude reel acquisition polyethylene/poly butyric and hydroxyl valerate blended fiber through twin-screw machine, and processing temperature is 200 ℃.Poly butyric valerate in the blended fiber is through carrene dissolving back acquisition polyethylene micro nanometer fiber material, is 100～800nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 7
Poly butyric valerate after the 1800 gram vacuumizes and 200 gram polyethylene to graft glycidyl methacrylate melt extrude the acquisition polyethylene to graft glycidyl methacrylate/poly butyric valerate blended fiber of reeling through twin-screw machine, and processing temperature is 210 ℃.Poly butyric valerate in the blended fiber adopts chloroform dissolving back to obtain polyethylene to graft glycidyl methacrylate micro nanometer fiber material, is 100～700nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 8
1600 gram dried PLAs of vacuum drying oven and 400 gram polyethylene blends melt extrude the acquisition polyethylene/polylactic acid blend fiber of reeling through the twin-screw spinning machine again.Processing temperature: 180 ℃, the PLA matrix phase constituent in the blended fiber by the dichloromethane solvent room temperature condition down dissolving remove, promptly obtain polyethylene micro nanometer fiber material, be 100～600nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 9
The PLA of 1800 gram vacuumizes and 200 gram polyethylene to graft glycidyl methacrylate blend melt extrude the acquisition polyethylene to graft glycidyl methacrylate/polylactic acid blend fiber of reeling through the twin-screw spinning machine again.Processing temperature: 200 ℃, PLA matrix under the room temperature condition in the blended fiber is removed by the carrene dissolving, promptly obtaining polyethylene to graft glycidyl methacrylate micro nanometer fiber material, is 100～600nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 10
After the polyamide 6 difference vacuum drying oven drying of the PLA of 1600 grams and 400 grams, melt extrude the acquisition polyamide 6/polylactic acid blend fiber of reeling through the twin-screw spinning machine.Processing temperature: 230 ℃, communicated chloroform dissolving of the PLA matrix under the room temperature condition in the blended fiber is removed, and promptly obtains polyamide 6 micro nanometer fiber material, is 50～500nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 11
After 1600 gram poly butyric esters and the 400 gram polyamide 6s difference dryings, melt extrude acquisition polyamide 6/poly butyric ester blended fiber through twin-screw machine, processing temperature is 230 ℃.Poly butyric ester in the blended fiber adopts chloroform dissolving back to obtain polyamide 6 micro nanometer fiber material, is 100～900nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 12
After the poly butyric capronate of 1600 grams and the 400 gram polyethylene terephthalate difference dryings, melt extrude acquisition polyethylene terephthalate/poly butyric capronate blended fiber through twin-screw machine, processing temperature is 240 ℃.Poly butyric capronate in the blended fiber adopts carrene dissolving back to obtain polyethylene terephthalate micro nanometer fiber material, is 100～1000nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 13
1800 gram PLAs and 200 gram polytrimethylene terephthalate blend after the vacuum drying oven drying melt extrude the acquisition polytrimethylene terephthalate/polylactic acid blend fiber of reeling through the twin-screw spinning machine again.Processing temperature: 230 ℃, room temperature condition adopts the PLA matrix phase constituent in the chloroform dissolution with solvents removal blended fiber down, promptly obtaining polytrimethylene terephthalate micro nanometer fiber material, is 100～600nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 14
After the poly butyric ester of 1800 grams and the 200 gram polytrimethylene terephthalates difference dryings, melt extrude acquisition terephthalic acid (TPA) propylene diester/poly butyric ester blended fiber through twin-screw machine, processing temperature is 220 ℃.It is 100～800nm through the diameter range of scanning electron microscopic observation micro nanometer fiber that poly butyric ester in the blended fiber adopts carrene dissolving back to obtain polytrimethylene terephthalate micro nanometer fiber material.
Embodiment 15
After the poly butyric ester of 1600 grams and the 400 gram polybutylene terephthalates difference dryings, melt extrude acquisition terephthalic acid (TPA) propylene diester/poly butyric ester blended fiber through twin-screw machine, processing temperature is 240 ℃.Poly butyric ester in the blended fiber adopts carrene dissolving back to obtain polybutylene terephthalate micro nanometer fiber material, is 100～700nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 16
1600 gram PLAs and 400 gram polybutylene terephthalate blend after the vacuum drying oven drying melt extrude the acquisition polytrimethylene terephthalate/polylactic acid blend fiber of reeling through the twin-screw spinning machine again.Processing temperature: 240 ℃, room temperature condition adopts the PLA matrix phase constituent in the dichloromethane solvent dissolving removal blended fiber down, promptly obtaining polybutylene terephthalate micro nanometer fiber material, is 100～700nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Embodiment 17
1600 gram dried PLAs of vacuum drying oven and 400 gram polypropylene grafted maleic anhydride blend melt extrude the acquisition polypropylene maleic anhydride/polylactic acid blend fiber of reeling through the twin-screw spinning machine again.Processing temperature: 190 ℃, PLA matrix phase constituent in the blended fiber is by the dissolving removal down of chloroform solvent room temperature condition, promptly obtaining polypropylene maleic anhydride micro nanometer fiber material, is 100～700nm through the diameter range of scanning electron microscopic observation micro nanometer fiber.
Claims (7)
1. thermoplastic polymer micro-nanometer fiber, its component comprises: 100% thermoplastic polymer; Described thermoplastic polymer is one or more the blend in polyethylene, polypropylene, polyamide, polyethylene terephthalate, polytrimethylene terephthalate, the polybutylene terephthalate, or polyethylene to graft glycidyl methacrylate, polypropylene grafted maleic anhydride.
2. a kind of thermoplastic polymer micro-nanometer fiber according to claim 1 is characterized in that: the diameter range of micro nanometer fiber is 50～1000nm.
3. the preparation method of a thermoplastic polymer micro-nanometer fiber comprises:
(1) be (1-40) with mass ratio: described thermoplastic polymer of claim 1 (60-99) and matrix blend mutually, melt extrude coiling through the twin-screw spinning machine, form thermoplastic polymer/matrix phase multicomponent blended fiber;
(2) above-mentioned blended fiber is dissolved in the solvent, removes the matrix phase, promptly get thermoplastic polymer micro-nanometer fiber;
Described matrix is PLA or polyhydroxy-alkanoate mutually.
4. the preparation method of a kind of thermoplastic polymer micro-nanometer fiber according to claim 3, it is characterized in that: described polyhydroxy-alkanoate is poly butyric ester PHB, poly butyric valerate PHBV or poly butyric capronate PHBHHx.
5. the preparation method of a kind of thermoplastic polymer micro-nanometer fiber according to claim 3, it is characterized in that: the blending temperature in the described step (1) is 180 ℃-270 ℃.
6. the preparation method of a kind of thermoplastic polymer micro-nanometer fiber according to claim 3, it is characterized in that: the blending temperature in the described step (1) is: 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃ or 270 ℃.
7. the preparation method of a kind of thermoplastic polymer micro-nanometer fiber according to claim 3, it is characterized in that: the solvent in the described step (2) is carrene or chloroform.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102154734A (en) * | 2011-03-09 | 2011-08-17 | 宁波大发化纤有限公司 | Blend fiber of poly(ethylene terephthalate) and polypropylene and preparation method thereof |
| CN102154733A (en) * | 2011-03-09 | 2011-08-17 | 宁波大发化纤有限公司 | Blended fiber of polyethylene terephthalate and polyethylene and preparation method thereof |
| CN103952784A (en) * | 2014-05-09 | 2014-07-30 | 浙江省纺织测试研究院 | Method for preparing polypropylene nanofiber on large scale |
| CN104294403A (en) * | 2014-10-20 | 2015-01-21 | 湖州市菱湖石淙永盛丝织厂 | Preparation method of stretch-proof mixed fibers |
| CN104630925A (en) * | 2015-02-05 | 2015-05-20 | 江苏科技大学 | Reactive extrusion preparation method of polyamide micro/nano fiber |
| CN108532016A (en) * | 2017-03-03 | 2018-09-14 | 长丰纺织科技股份有限公司 | Thermoplastic polymer nanofiber fiber and its manufacturing method |
| CN110479122A (en) * | 2019-09-03 | 2019-11-22 | 贵州省材料产业技术研究院 | A kind of preparation method of porous polymer in-situ micro-fibril water-oil separating material |
| TWI684619B (en) * | 2017-01-03 | 2020-02-11 | 長豐紡織科技股份有限公司 | Thermoplastic polymer nanofiber and method for producing the same |
| CN113512290A (en) * | 2021-07-28 | 2021-10-19 | 南京禾素时代抗菌材料科技有限公司 | Biological-based material PHBV and polyamide modified antibacterial, deodorizing and antiviral master batch |
| CN114808162A (en) * | 2022-04-28 | 2022-07-29 | 上海迅江科技有限公司 | Flash spinning/electrostatic spinning composite superfine nanofiber material and preparation method thereof |
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| CN101012577A (en) * | 2007-02-09 | 2007-08-08 | 北京特斯顿新材料技术发展有限公司 | Extraction and desiccation method in preparing process of polyvinyl fibre with super high molecular weight |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102154734A (en) * | 2011-03-09 | 2011-08-17 | 宁波大发化纤有限公司 | Blend fiber of poly(ethylene terephthalate) and polypropylene and preparation method thereof |
| CN102154733A (en) * | 2011-03-09 | 2011-08-17 | 宁波大发化纤有限公司 | Blended fiber of polyethylene terephthalate and polyethylene and preparation method thereof |
| CN102154733B (en) * | 2011-03-09 | 2013-07-03 | 宁波大发化纤有限公司 | Blended fiber of polyethylene terephthalate and polyethylene and preparation method thereof |
| CN103952784A (en) * | 2014-05-09 | 2014-07-30 | 浙江省纺织测试研究院 | Method for preparing polypropylene nanofiber on large scale |
| CN104294403A (en) * | 2014-10-20 | 2015-01-21 | 湖州市菱湖石淙永盛丝织厂 | Preparation method of stretch-proof mixed fibers |
| CN104630925A (en) * | 2015-02-05 | 2015-05-20 | 江苏科技大学 | Reactive extrusion preparation method of polyamide micro/nano fiber |
| TWI684619B (en) * | 2017-01-03 | 2020-02-11 | 長豐紡織科技股份有限公司 | Thermoplastic polymer nanofiber and method for producing the same |
| CN108532016A (en) * | 2017-03-03 | 2018-09-14 | 长丰纺织科技股份有限公司 | Thermoplastic polymer nanofiber fiber and its manufacturing method |
| CN110479122A (en) * | 2019-09-03 | 2019-11-22 | 贵州省材料产业技术研究院 | A kind of preparation method of porous polymer in-situ micro-fibril water-oil separating material |
| CN110479122B (en) * | 2019-09-03 | 2021-09-21 | 贵州省材料产业技术研究院 | Preparation method of porous polymer in-situ microfiber oil-water separation material |
| CN113512290A (en) * | 2021-07-28 | 2021-10-19 | 南京禾素时代抗菌材料科技有限公司 | Biological-based material PHBV and polyamide modified antibacterial, deodorizing and antiviral master batch |
| CN114808162A (en) * | 2022-04-28 | 2022-07-29 | 上海迅江科技有限公司 | Flash spinning/electrostatic spinning composite superfine nanofiber material and preparation method thereof |
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Application publication date: 20101020 |