CN102943315A - PLA (polylactic acid) conductive fiber and preparation method thereof - Google Patents
PLA (polylactic acid) conductive fiber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a PLA (polylactic acid) conductive fiber and a preparation method thereof. The fiber comprises the following raw materials in parts by weight: 50-80 parts of PLA, 20-50 parts of P (VAc-co-VA) and 0.05-8 parts of conductive filler. The preparation method of the PLA conductive fiber comprises the following steps of: (1) weighing the dried PLA, P (VAc-co-VA) and conductive filler according to the proportions, premixing, and granulating in a blending way to obtain conductive master batches of the PLA; or firstly, weighing the P (VAc-co-VA) and the conductive filler according to the proportions, premixing, granulating in a blending way to obtain conductive master batches of the P (VAc-co-VA), and then blending with the PLA to obtain conductive master batches of the PLA; and (2) carrying out melt spinning-drafting on the conductive master batches of the PLA to obtain PLA conductive fiber. The conductive fiber can be taken as an electrode material, an anti-static material, a low-temperature heating material, an electromagnetic shielding material, a heat-sensitive material, a gas-sensitive material and the like.
Description
Technical field
The present invention relates to polymeric material field, be specifically related to PLA (PLA) conductive fiber and preparation method thereof.
Background technology
China is procedure of fibre production big country, synthetic fiber output ranked first in the world in continuous 15 years, the total output value of fiber and textiles thereof accounts for about 10% of China GDP, foreign exchange earning accounts for 1/4, in national economy, account for very critical role, and there is following problem in the development of domestic synthetic fiber at present: at first, the development of synthetic fiber is subject to the restriction of shortage of resources, the raw material of synthetic fiber relies on oil more than 90%, and calculate with now explored oil total amount and depletion rate, fiber and relevant industries thereof will be in the situation of " cooking a meal without rice " after 50 years; Secondly, the development of synthetic fiber is subject to the restriction of environmental pollution, and the petroleum base chemical fibre can not be degraded at occurring in nature, can bring very serious " white pollution ", has a strong impact on people's quality of life.Therefore turn to the emphasis of synthetic fiber industrial research exploitation the research and development of resource recyclable organism degradation material most important.Again, China's chemical fibre production is still take conventional fibre as main, and the new high-tech fibers exploitation lags behind, and synthetic fiber output accounts for 2/3 of world's total amount, but functionalization ratio less than 10%, far below the level of developed country more than 30%.Therefore, the functionalization of realization chemical fibre and high performance are to improve the added value of fiber, to enhance one's market competitiveness the needs that meet China's chemical fibre development.
The PLA resource is renewable, biodegradable, good biocompatibility, it is a kind of thermoplastic macromolecule material simultaneously, can directly carry out melt spinning and make fiber, at present, the melt spinning technology of PLA is ripe, PLA is expected the raw material that petroleum replacing based high molecular material becomes chemical fibre, with problems such as the shortage of resources that development was faced that solves synthetic fiber and environmental pollutions.Yet, the research-and-development activity of PLA fiber functionalization is less, and the conducting function of fiber turns to the emphasis of the R and D of industrial circle and academia, therefore, the conducting function of realizing the PLA fiber has certain necessity, and the present graduate Petra of Dresden, Germany macromolecule only
[
P.; Kobashi, K.; Villmow, T.; Andres, T.; Paiva, M.C.; Covas, J.A.Liquid sensing properties of melt processed polypropylene/poly (ε-caprolactone blends containing multiwalled carbon nanotubes.Composites Science and Technology 2011,71,1451-1460.] made the PCL/PLA/MWNTs conductive fiber with the method for melt spinning, but the mechanical property of gained conductive fiber is relatively poor, the fracture strength elongation at break of gained as-spun fibre only is 22MPa and 6.2% respectively, does not have actual application value at field of textiles.
Summary of the invention
The objective of the invention is to develop a kind of PLA conductive fiber, and its preparation method is provided for the few present situation of PLA fiber functionalization product.
A kind of PLA (PLA) conductive fiber, made by the raw material of following parts by mass:
PLA:50～80 part;
Poly-(vinylacetate-co-vinyl alcohol) (P (VAc-co-VA)): 20～50 parts;
Conductive filler: 0.05～8 part;
Described PLA conductive fiber is characterized in that the viscosity average molecular weigh of PLA is: 6.0 * 10
4～3.0 * 10
5
Described PLA conductive fiber is characterized in that the content of dextrorotation lactic acid units among the PLA is: 0～10mol%;
Described PLA conductive fiber is characterized in that conductive filler is carbon black (CB), single ancient piece of jade, round, flat and with a hole in its centre CNT (SWCNTs), many ancient piece of jade, round, flat and with a hole in its centres CNT (MWCNTs), Graphene (GN), gas phase nano carbon fiber (VGCNFs), copper sulfide, cuprous sulfide and cuprous iodide etc.;
Described PLA conductive fiber, the viscosity average molecular weigh that it is characterized in that P (VAc-co-VA) is 5.0 * 10
4～1.0 * 10
6
Described PLA conductive fiber, the ratio that it is characterized in that the vinyl alcohol construction unit among the P (VAc-co-VA) is 9mol%～80mol%;
The preparation method of described PLA conductive fiber comprises the steps:
(1) in advance with PLA, P (VAc-co-VA) and conductive filler dry 8～48h in vacuum drying oven, the baking temperature of PLA, P (VAc-co-VA) and conductive filler is respectively 50～120 ℃, 25～55 ℃ and 50～120 ℃;
(2) getting 0.05～8 part of PLA50～80 part, 20～50 parts of P (VAc-co-VA) and conductive filler puts into and is dry mixed 3～5 minutes in the super mixer, then blend granulation in the twin-screw blender, get the PLA conductive agglomerate, prilling temperature is 160～220 ℃, rotating speed is 50～150rmp, and the melt blending time is 3～8 minutes; Perhaps getting first 20～50 parts of P (VAc-co-VA) and 0.05～8 part of conductive agglomerate puts into and is dry mixed 3～5 minutes in the super mixer, then blend granulation in the twin-screw blender, get P (VAc-co-VA) conductive agglomerate, the melt blending temperature is 160～220 ℃, rotating speed is 50～150rmp, the melt blending time is 3～6 minutes, P (VAc-co-VA) the conductive agglomerate blend of then getting 50～80 parts of PLA and gained gets the PLA conductive agglomerate, prilling temperature is 160～220 ℃, rotating speed is 50～150rmp, and the melt blending time is 3～8 minutes;
(3) with the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity the PLA as-spun fibre, spinning temperature is 170～220 ℃, winding speed is 1500～3000m/min;
(4) as-spun fibre is carried out drawing-off, get the PLA conductive fiber, drawing temperature is 100～125 ℃, and drafting multiple is 1～6 times.
Beneficial effect:
The present invention has realized the conducting function of PLA fiber with the method for common melt spinning, and easy to operate, in addition, percolation threshold is low, and namely the consumption of conductive filler is few, the good spinnability of fiber, and cost is low.The conductance of gained PLA conductive fiber can reach 2.5S/m, and fracture strength is 2.0～6.0cN/dtex, and elongation at break is 20%～80%.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are used for the present invention being described and not limiting the scope of the invention.Should be understood that in addition those skilled in the art can be to the various changes of the present invention or modification after the content of having read the present invention's instruction, these equivalent form of values fall into the appended claims limited range of the application equally.
Embodiment 1
(1) at first takes by weighing 50 parts of PLA (content of L-lactic acid unit is 2.1mol%), 50 parts of P (VAc-co-VA) and 4 parts of carbon blacks respectively dry 12 hours (80 ℃), 48 hours (40 ℃) and 8 hours (100 ℃) in vacuum drying oven, then they are put into and be dry mixed 3 minutes in the super mixer, again blend granulation in the twin-screw blender gets the PLA conductive agglomerate.Prilling temperature is 170 ℃, and screw speed is 75rmp, and the melt blending time is 8 minutes.
(2) with the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity the PLA as-spun fibre, spinning temperature is 190 ℃, winding speed is 1500m/min;
(3) as-spun fibre is carried out drawing-off, get the PLA conductive fiber, drawing temperature is 110 ℃, and drafting multiple is 3 times.The conductance of gained PLA conductive fiber is 1.52S/m, and fracture strength is 2.5cN/dtex, and elongation at break is 50.5%.
Embodiment 2
(1) at first takes by weighing 60 parts of PLA (content of L-lactic acid unit is 0.5mol%), 40 parts of P (VAc-co-VA) and 3 parts of MWCNTs respectively dry 15 hours (70 ℃), 36 hours (45 ℃) and 8 hours (110 ℃) in vacuum drying oven, then they are put into and be dry mixed 4 minutes in the super mixer, again blend granulation in the twin-screw blender gets the PLA conductive agglomerate.Prilling temperature is 180 ℃, and screw speed is 60rmp, and the melt blending time is 7 minutes.
(2) with the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity the PLA as-spun fibre, spinning temperature is 200 ℃, winding speed is 3000m/min;
(3) as-spun fibre is carried out drawing-off, get the PLA conductive fiber, drawing temperature is 100 ℃, and drafting multiple is 4 times.The conductance of gained PLA conductive fiber is 1.78S/m, and fracture strength is 3.0cN/dtex, and elongation at break is 30.8%.
Embodiment 3
(1) at first takes by weighing 65 parts of PLA (content of L-lactic acid unit is 1.0mol%), 35 parts of P (VAc-co-VA) and 2.5 parts of SWCNTs be dry 12 hours (90 ℃) in vacuum drying oven respectively, 48 hours (40 ℃) and 12 hours (100 ℃), the P (VAc-co-VA) of drying and conductive agglomerate put into be dry mixed 3 minutes in the super mixer, again blend granulation in the twin-screw blender, then blend granulation in the twin-screw blender, get P (VAc-co-VA) conductive agglomerate, the melt blending temperature is 170 ℃, rotating speed is 75rmp, and the melt blending time is 6 minutes; The PLA of drying and the P of gained (VAc-co-VA) conductive agglomerate put into be dry mixed 3 minutes in the super mixer, melt blending gets the PLA conductive agglomerate, and temperature is 190 ℃, and rotating speed is 80rmp, and the melt blending time is 6 minutes, gets the PLA conductive agglomerate.
(2) with the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity the PLA as-spun fibre, spinning temperature is 190 ℃, winding speed is 2000m/min;
(3) as-spun fibre is carried out drawing-off, get the PLA conductive fiber, drawing temperature is 100 ℃, and drafting multiple is 2.5 times.The conductance of gained conductive fiber is 1.45S/m, and fracture strength is 2.0cN/dtex, and elongation at break is 80.9%.
Embodiment 4
(1) at first takes by weighing 60 parts of PLA (content of L-lactic acid unit is 2.5mol%), 40 parts of P (VAc-co-VA) and 6 parts of carbon blacks be dry 12 hours (90 ℃) in vacuum drying oven respectively, 48 hours (40 ℃) and 12 hours (100 ℃), the P (VAc-co-VA) of drying and conductive agglomerate put into be dry mixed 4 minutes in the super mixer, again blend granulation in the twin-screw blender, then blend granulation in the twin-screw blender, get P (VAc-co-VA) conductive agglomerate, the melt blending temperature is 170 ℃, rotating speed is 75rmp, and the melt blending time is 6 minutes; The PLA of drying and the P of gained (VAc-co-VA) conductive agglomerate put into be dry mixed 4 minutes in the super mixer, melt blending gets the PLA conductive agglomerate, and temperature is 190 ℃, and rotating speed is 80rmp, and the melt blending time is 6 minutes, gets the PLA conductive agglomerate.
(2) with the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity the PLA as-spun fibre, spinning temperature is 190 ℃, winding speed is 1500m/min;
(3) as-spun fibre is carried out drawing-off, get the PLA conductive fiber, drawing temperature is 100 ℃, and drafting multiple is 5 times.The conductance of gained conductive fiber is 2.01S/m, and fracture strength is 3.8cN/dtex, and elongation at break is 25.7%.
Claims (7)
1. a PLA (PLA) conductive fiber, made by the raw material of following parts by mass:
PLA:50～80 part;
Poly-(vinylacetate-co-vinyl alcohol) (P (VAc-co-VA)): 20～50 parts;
Conductive filler: 0.05～8 part.
2. PLA conductive fiber according to claim 1 is characterized in that the viscosity average molecular weigh of PLA is: 6.0 * 1
04～3.0 * 10
5
3. PLA conductive fiber according to claim 1 is characterized in that the content of dextrorotation lactic acid units among the PLA is: 0～10mol%.
4. PLA conductive fiber according to claim 1 is characterized in that conductive filler is carbon black (CB), single ancient piece of jade, round, flat and with a hole in its centre CNT (SWCNTs), many ancient piece of jade, round, flat and with a hole in its centres CNT (MWCNTs), Graphene (GN), gas phase nano carbon fiber (VGCNFs), copper sulfide, cuprous sulfide and cuprous iodide etc.
5. PLA conductive fiber according to claim 1, the viscosity average molecular weigh that it is characterized in that P (VAc-co-VA) is 5.0 * 10
4～1.0 * 10
6
6. PLA conductive fiber according to claim 1, the ratio that it is characterized in that the vinyl alcohol construction unit among the P (VAc-co-VA) is 9mol%～80mol%.
7. the preparation method of each described PLA conductive fiber comprises the steps: according to claim 1～6
(1) in advance with PLA, P (VAc-co-VA) and conductive filler dry 8～48h in vacuum drying oven, the baking temperature of PLA, P (VAc-co-VA) and conductive filler is respectively 50～120 ℃, 25～55 ℃ and 50～120 ℃;
(2) getting 0.05～8 part of PLA50～80 part, 20～50 parts of P (VAc-co-VA) and conductive filler puts into and is dry mixed 3～5 minutes in the super mixer, then blend granulation in the twin-screw blender, get the PLA conductive agglomerate, prilling temperature is 160～220 ℃, rotating speed is 50～150rmp, and the melt blending time is 3～8 minutes; Perhaps getting first 20～50 parts of P (VAc-co-VA) and 0.05～8 part of conductive agglomerate puts into and is dry mixed 3～5 minutes in the super mixer, then blend granulation in the twin-screw blender, get P (VAc-co-VA) conductive agglomerate, the melt blending temperature is 160～220 ℃, rotating speed is 50～150rmp, the melt blending time is 3～6 minutes, P (VAc-co-VA) the conductive agglomerate blend of then getting 50～80 parts of PLA and gained gets the PLA conductive agglomerate, prilling temperature is 160～220 ℃, rotating speed is 50～150rmp, and the melt blending time is 3～8 minutes;
(3) with the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity the PLA as-spun fibre, spinning temperature is 170～220 ℃, winding speed is 1500～3000m/min;
(4) as-spun fibre is carried out drawing-off, get the PLA conductive fiber, drawing temperature is 100～125 ℃, and drafting multiple is 1～6 times.
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Cited By (8)
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| WO2015170344A1 (en) | 2014-05-09 | 2015-11-12 | Council Of Scientific & Industrial Research | An improved next generation off-laboratory polymer chip electrode |
| CN105694395A (en) * | 2016-04-28 | 2016-06-22 | 苏州新区华士达工程塑胶有限公司 | Degradable antistatic plastic |
| CN106433057A (en) * | 2016-10-21 | 2017-02-22 | 天津大学 | Preparation method of 3D (three-dimensional) printed conductive wire |
| CN106592203A (en) * | 2016-12-21 | 2017-04-26 | 常州二维碳素科技股份有限公司 | Graphene conductive fabric, preparation method and application thereof |
| CN106609400A (en) * | 2017-01-04 | 2017-05-03 | 苏州金泉新材料股份有限公司 | Preparation method of multifunctional polylactic acid fiber |
| CN106676679A (en) * | 2016-11-08 | 2017-05-17 | 江南大学 | Preparation method of polylactic acid conductive fibers |
| CN108593719A (en) * | 2018-06-26 | 2018-09-28 | 浙江大学 | A kind of immunosensor based on flexible electrode |
| EP4242648A1 (en) | 2022-03-08 | 2023-09-13 | Politechnika Gdanska | Composite electrodes for nitroexplosive detection comprising a nanodiamond foil (ndf) or a layer of nanodiamond powder (ndp) deposited on a graphene-doped polylactic acid (g-pla) |
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| CN106433057A (en) * | 2016-10-21 | 2017-02-22 | 天津大学 | Preparation method of 3D (three-dimensional) printed conductive wire |
| CN106676679A (en) * | 2016-11-08 | 2017-05-17 | 江南大学 | Preparation method of polylactic acid conductive fibers |
| CN106592203A (en) * | 2016-12-21 | 2017-04-26 | 常州二维碳素科技股份有限公司 | Graphene conductive fabric, preparation method and application thereof |
| CN106592203B (en) * | 2016-12-21 | 2019-06-07 | 常州二维碳素科技股份有限公司 | Graphene conductive cloth, preparation method and its usage |
| CN106609400A (en) * | 2017-01-04 | 2017-05-03 | 苏州金泉新材料股份有限公司 | Preparation method of multifunctional polylactic acid fiber |
| CN108593719A (en) * | 2018-06-26 | 2018-09-28 | 浙江大学 | A kind of immunosensor based on flexible electrode |
| EP4242648A1 (en) | 2022-03-08 | 2023-09-13 | Politechnika Gdanska | Composite electrodes for nitroexplosive detection comprising a nanodiamond foil (ndf) or a layer of nanodiamond powder (ndp) deposited on a graphene-doped polylactic acid (g-pla) |
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