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CN101864611B - Polylactic acid nano fiber and preparation method thereof - Google Patents

Polylactic acid nano fiber and preparation method thereof Download PDF

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Publication number
CN101864611B
CN101864611B CN2010101954907A CN201010195490A CN101864611B CN 101864611 B CN101864611 B CN 101864611B CN 2010101954907 A CN2010101954907 A CN 2010101954907A CN 201010195490 A CN201010195490 A CN 201010195490A CN 101864611 B CN101864611 B CN 101864611B
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polylactic acid
water
fiber
soluble polyester
preparation
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CN101864611A (en
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肖茹
刘鹏
欧阳炀
江霄汉
顾莉琴
王华平
孙刚
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Donghua University
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Donghua University
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Abstract

本发明涉及一种聚乳酸微纳米纤维及其制备方法,组分包括:100%聚乳酸;制备包括:(1)将聚乳酸与水溶性聚酯共混,经双螺杆纺丝机熔融挤出卷绕,形成聚乳酸/水溶性聚酯共混纤维;(2)将上述共混纤维溶解在溶剂中,去除水溶性聚酯,即得。本发明的纤维的直径范围为50~500nm;制备方法简单高效,易于实现规模化生产。

Figure 201010195490

The invention relates to a polylactic acid micro-nano fiber and a preparation method thereof. The components include: 100% polylactic acid; the preparation includes: (1) blending polylactic acid and water-soluble polyester, and melting and extruding the polylactic acid through a twin-screw spinning machine Winding to form polylactic acid/water-soluble polyester blended fibers; (2) dissolving the above-mentioned blended fibers in a solvent and removing the water-soluble polyester to obtain the product. The diameter range of the fiber of the invention is 50-500nm; the preparation method is simple and efficient, and it is easy to realize large-scale production.

Figure 201010195490

Description

Polylactic acid nano fiber and preparation method thereof
Technical field
The invention belongs to micro nanometer fiber and preparation field thereof, particularly relate to a kind of polylactic acid nano 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 application fields and huge commercial value.
The method for preparing nanofiber has: compound vapor deposition, masterplate polymerization and MOLECULE DESIGN method and spinning process method etc.Wherein 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.People such as the Jin Xiangyu of Donghua University prepare a kind of ultra-fine acid fiber by polylactic non-woven fabric material, and its average fibre diameter is 2.7~9.1 μ m, have applied for Chinese invention patent (200410017776.0).Toray Fiber Research Institute (China) Co., Ltd. has prepared a kind of polylactic acid fibre of separating property of fire resistant water resistant, and its technical characterstic comprises terminal carboxyl group blockade back spinning, and uses the processing and sorting liquid that contains water-soluble crosslinking agent to handle.It is all bigger than normal that but these methods obtain the acid fiber by polylactic diameter, hindered the further Application and Development of poly-lactic acid material.
Summary of the invention
Technical problem to be solved by this invention provides a kind of polylactic acid nano fiber and preparation method thereof, and this method is simple, and efficient is high, and environmentally safe is easy to accomplish scale production.
A kind of polylactic acid nano fiber of the present invention, its component comprises: 100% PLA.
The diameter of said nanofiber is 50~500nm.
The preparation method of a kind of polylactic acid nano fiber of the present invention comprises:
(1) be (1-50) with mass ratio: PLA (50-99) and water-soluble polyester (co-PET) (EastONE S85030Copolyester) blend, melt extrude through the twin-screw spinning machine, be wound into fibre, form PLA/water-soluble polyester blended fiber;
(2) above-mentioned blended fiber is dissolved in the solvent, removes water-soluble polyester, promptly get polylactic acid nano fiber.
PLA in the said step (1) is PLA and copolymer or their blends.
Blending temperature in the said step (1) is 170-220 ℃.
Blending temperature in the said step (1) is: 170 ℃, 180 ℃, 190 ℃, 200 ℃, 210 ℃ or 220 ℃ etc.
Solvent in the said step (2) is a water.
Be decentralized photo with the PLA in PLA of the present invention and the water-soluble polyester melting process, because the existence of inherent restraining factors such as co-mixing system ratio of component, ratio of viscosities and external force fields such as shear tension and temperature can assemble in situ form micro nanometer fiber.
Beneficial effect
(1) diameter range of polylactic acid nano fiber of the present invention is 50~500nm;
(2) preparation method of the present invention is simple, and efficient is high, is easy to accomplish scale production; Do not use toluene, xylene and other alkaline solutions etc. to be prone to environment is produced the solvent that pollutes, help resource conservation.
Description of drawings
Fig. 1 PLA/co-PET blend composite fiber (mass ratio is 10: 90) is removed co-PET back gained PLA micro nanometer fiber mutually;
Fig. 2 PLA/co-PET blend composite fiber (mass ratio is 20: 80) is removed co-PET back gained PLA micro nanometer fiber mutually;
Fig. 3 PLA/co-PET blend composite fiber (mass ratio is 30: 70) is removed co-PET back gained PLA micro nanometer fiber mutually;
Fig. 4 PLA/co-PET blend composite fiber (mass ratio is 40: 60) is removed co-PET back gained PLA 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 the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to 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
The PLA of 1800 gram water-soluble polyester co-PET and 200 grams is dry back blend in vacuum drying oven, melt extrudes to reel through the twin-screw spinning machine again to obtain PLA/water-soluble polyester blended fiber.Processing temperature: 180 ℃; Matrix phase constituent water-soluble polyester in the blended fiber is removed after in 85 ℃ of pure water, dissolving 15min; Promptly obtaining the polylactic acid nano fiber material, is 50~350nm through the diameter range of scanning electron microscopic observation micro nanometer fiber, and average diameter is about 198nm.
Embodiment 2
After the vacuum drying oven dried, 1600 gram water-soluble polyester co-PET and 400 gram polylactic acid blends melt extrude the acquisition PLA/water-soluble polyester blended fiber of reeling through the twin-screw spinning machine.Processing temperature: 190 ℃; Matrix phase constituent water-soluble polyester in the blended fiber is removed after in 85 ℃ of pure water, dissolving 20min; Promptly obtaining the polylactic acid nano fiber material, is 50~400nm through the diameter range of scanning electron microscopic observation micro nanometer fiber, and average diameter is about 239nm.
Embodiment 3
Dried 1400 gram water-soluble polyester co-PET of vacuum drying oven and 600 gram polylactic acid blends melt extrude the acquisition PLA/water-soluble polyester blended fiber of reeling through the twin-screw spinning machine again.Processing temperature: 200 ℃; Matrix phase constituent water-soluble polyester in the blended fiber is removed after in 85 ℃ of pure water, dissolving 20min; Promptly obtaining the polylactic acid nano fiber material, is 100~450nm through the diameter range of scanning electron microscopic observation micro nanometer fiber, and average diameter is about 284nm.
Embodiment 4
The PLA of 1000 gram water-soluble polyester co-PET and 1000 grams is dry back blend in vacuum drying oven, melt extrudes to reel through the twin-screw spinning machine again to obtain PLA/water-soluble polyester blended fiber.Processing temperature: 170 ℃; Water-soluble polyester matrix in the blended fiber is removed after in 85 ℃ of pure water, dissolving 30min; Promptly obtaining the polylactic acid nano fiber material, is 200~500nm through the diameter range of scanning electron microscopic observation micro nanometer fiber, and average diameter is about 320nm.
Embodiment 5
Dried 1200 gram water-soluble polyester co-PET of vacuum drying oven and 800 gram polylactic acid blends melt extrude the acquisition PLA/water-soluble polyester blended fiber of reeling through the twin-screw spinning machine again.Processing temperature: 210 ℃; Water-soluble polyester matrix in the blended fiber is removed after in 85 ℃ of pure water, dissolving 25min; Promptly obtaining the polylactic acid nano fiber material, is 150~500nm through the diameter range of scanning electron microscopic observation micro nanometer fiber, and average diameter is about 282nm.
Embodiment 6
Dried 1980 gram water-soluble polyester co-PET of vacuum drying oven and 20 gram polylactic acid blends melt extrude the acquisition PLA/water-soluble polyester blended fiber of reeling through the twin-screw spinning machine again.Processing temperature: 220 ℃; Matrix phase constituent water-soluble polyester in the blended fiber is removed after in 85 ℃ of pure water, dissolving 20min; Promptly obtaining the polylactic acid nano fiber material, is 100~350nm through the diameter range of scanning electron microscopic observation micro nanometer fiber, and average diameter is about 200nm.

Claims (4)

1.一种聚乳酸微纳米纤维的制备方法,包括:1. A preparation method of polylactic acid micro-nano fibers, comprising: (1)将质量比为(1-50)∶(50-99)的聚乳酸与水溶性聚酯co-PET共混,经双螺杆纺丝机熔融挤出,卷绕成纤,形成聚乳酸/水溶性聚酯共混纤维;(1) Blend polylactic acid with a mass ratio of (1-50): (50-99) and water-soluble polyester co-PET, melt and extrude it through a twin-screw spinning machine, and wind it into fibers to form polylactic acid /Water-soluble polyester blended fiber; (2)将上述共混纤维溶解在溶剂中,去除水溶性聚酯,即得聚乳酸微纳米纤维。(2) Dissolving the above-mentioned blended fiber in a solvent to remove the water-soluble polyester to obtain the polylactic acid micro-nano fiber. 2.根据权利要求1所述的一种聚乳酸微纳米纤维的制备方法,其特征在于:所述步骤(1)中的共混温度为170℃-220℃。2. A method for preparing polylactic acid micro-nano fibers according to claim 1, characterized in that: the blending temperature in the step (1) is 170°C-220°C. 3.根据权利要求1所述的一种聚乳酸微纳米纤维的制备方法,其特征在于:所述步骤(1)中的共混温度为:170℃、180℃、190℃、200℃、210℃或220℃。3. A method for preparing polylactic acid micro-nano fibers according to claim 1, characterized in that: the blending temperature in the step (1) is: 170°C, 180°C, 190°C, 200°C, 210°C °C or 220 °C. 4.根据权利要求1所述的一种聚乳酸微纳米纤维的制备方法,其特征在于:所述步骤(2)中的溶剂为水。4. The preparation method of a kind of polylactic acid micro-nano fiber according to claim 1, characterized in that: the solvent in the step (2) is water.
CN2010101954907A 2010-06-08 2010-06-08 Polylactic acid nano fiber and preparation method thereof Expired - Fee Related CN101864611B (en)

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CN102532833A (en) * 2011-12-16 2012-07-04 奇瑞汽车股份有限公司 Nanometer high polymer polylactic acid composite material and preparation method thereof
CN103541040B (en) * 2012-07-09 2015-11-18 北京服装学院 The preparation method of PLA superfine fibre and PLA superfine fibre
CN108486715B (en) * 2018-05-03 2019-04-26 广东护康宝农林生物科技有限公司 A kind of Tea Saponin washes clean bag and its application method
CN116988185B (en) * 2023-09-21 2023-12-05 苏州宝丽迪材料科技股份有限公司 Preparation method of light-absorbing and heat-generating polylactic acid fiber

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CN101563391A (en) * 2006-12-15 2009-10-21 金伯利-克拉克环球有限公司 Biodegradable polylactic acids for use in forming fibers

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101563391A (en) * 2006-12-15 2009-10-21 金伯利-克拉克环球有限公司 Biodegradable polylactic acids for use in forming fibers

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