CN102943315B - 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 ranks first in the world for 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, very critical role is accounted in national economy, and there is following problem in the development of domestic synthetic fiber at present: first, the development of synthetic fiber is subject to the restriction of shortage of resources, the raw material more than 90% of synthetic fiber relies on oil, and calculate with now explored oil total amount and depletion rate, after 50 years, fiber and relevant industries thereof will be in the situation of " cooking a meal without rice "; Secondly, the development of synthetic fiber is subject to the restriction of environmental pollution, and petroleum-based chemical fiber can not be degraded at occurring in nature, can bring very serious " white pollution ", have a strong impact on the quality of life of people.Therefore turn to the research and development of resource recyclable organism degradation material most important at the emphasis of synthetic fiber industrial research exploitation.Again, China's experimental branch line is still based on conventional fibre, and new high-tech fibers exploitation is delayed, and synthetic fiber output accounts for 2/3 of world's total amount, but functionalization ratio is less than 10%, far below the level of developed country more than 30%.Therefore, realize the functionalization of chemical fibre and high performance to improve the added value of fiber, enhance one's market competitiveness and meet the needs of China's chemical fibre development.
PLA resource is renewable, biodegradable, good biocompatibility, it is a kind of thermoplastic macromolecule material simultaneously, can directly carry out melt spinning and obtain 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, the problems such as the shortage of resources faced with the development solving synthetic fiber and environmental pollution.But, 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 realizing PLA fiber has certain necessity, and the current only graduate Petra of Dresden, Germany macromolecule
[
p., Kobashi, K., Villmow, T., Andres, T., Paiva, M.C., Covas, J.A.Liquid sensing properties of melt processed polypropylene/poly (e-caprolactone blendscontaining multiwalled carbon nanotubes.Composites Science and Technology 2011, 71, 1451-1460.] obtain PCL/PLA/MWNTs conductive fiber by the method for melt spinning, but the mechanical property of gained conductive fiber is poor, the fracture strength elongation at break of gained as-spun fibre is only 22MPa and 6.2% respectively, not there is actual application value at field of textiles.
Summary of the invention
The object of the invention is, for the few present situation of PLA fiber functionalization product, to develop a kind of PLA conductive fiber, and provide its preparation method.
A kind of PLA (PLA) conductive fiber, be made up of 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 L-lactic acid unit in PLA is: 0 ~ 10mol%;
Described PLA conductive fiber, is characterized in that conductive filler is the one in carbon black (CB), Single Walled Carbon Nanotube (SWCNTs), multi-walled carbon nano-tubes (MWCNTs), Graphene (GN), gas phase nano carbon fiber (VGCNFs), copper sulfide, cuprous sulfide and cuprous iodide;
Described PLA conductive fiber, is characterized in that the viscosity average molecular weigh of P (VAc-co-VA) is 5.0 × 10
4~ 1.0 × 10
6;
Described PLA conductive fiber, is characterized in that the ratio of the vinyl alcohol construction unit in P (VAc-co-VA) is 9mol% ~ 80mol%;
The preparation method of described PLA conductive fiber, comprises the steps:
(1) in advance the baking temperature of PLA, P (VAc-co-VA) and conductive filler dry 8 ~ 48h, PLA, P (VAc-co-VA) and conductive filler in vacuum drying oven is respectively 50 ~ 120 DEG C, 25 ~ 55 DEG C and 50 ~ 120 DEG C;
(2) get PLA50 ~ 80 part, P (VAc-co-VA) 20 ~ 50 parts and conductive filler 0.05 ~ 8 part to put in super mixer and be dry mixed 3 ~ 5 minutes, then blended granulation in twin-screw blender, obtain PLA conductive agglomerate, prilling temperature is 160 ~ 220 DEG C, rotating speed is 50 ~ 150rmp, and the melt blending time is 3 ~ 8 minutes; Or first get 20 ~ 50 parts of P (VAc-co-VA) and 0.05 ~ 8 part of conductive agglomerate to put in super mixer and be dry mixed 3 ~ 5 minutes, then blended granulation in twin-screw blender, obtain P (VAc-co-VA) conductive agglomerate, melt blending temperature is 160 ~ 220 DEG C, rotating speed is 50 ~ 150rmp, the melt blending time is 3 ~ 6 minutes, then get P (VAc-co-VA) conductive agglomerate of 50 ~ 80 parts of PLA and gained blended PLA conductive agglomerate, prilling temperature is 160 ~ 220 DEG C, rotating speed is 50 ~ 150rmp, and the melt blending time is 3 ~ 8 minutes;
(3) by the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity PLA as-spun fibre, spinning temperature is 170 ~ 220 DEG C, and winding speed is 1500 ~ 3000m/min;
(4) carry out drawing-off to as-spun fibre, obtain PLA conductive fiber, drawing temperature is 100 ~ 125 DEG C, and drafting multiple is 1 ~ 6 times.
Beneficial effect:
The method of the present invention's normal melt spinning achieves the conducting function of PLA fiber, easy to operate, and in addition, percolation threshold is low, and namely the consumption of conductive filler is few, and the good spinnability of fiber, 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%.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments only do not limit the scope of the invention for illustration of the present invention.In addition should be understood that those skilled in the art can to the various change of the present invention or amendment, and these equivalent form of values fall into claims limited range appended by the application equally after the content of having read the present invention's instruction.
Embodiment 1
(1) 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 dry 12 hours (80 DEG C), 48 hours (40 DEG C) and 8 hours (100 DEG C) in vacuum drying oven respectively are first taken, then they are put in super mixer and be dry mixed 3 minutes, blended granulation in twin-screw blender again, obtains PLA conductive agglomerate.Prilling temperature is 170 DEG C, and screw speed is 75rmp, and the melt blending time is 8 minutes.
(2) by the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity PLA as-spun fibre, spinning temperature is 190 DEG C, and winding speed is 1500m/min;
(3) carry out drawing-off to as-spun fibre, obtain PLA conductive fiber, drawing temperature is 110 DEG C, 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) 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 dry 15 hours (70 DEG C), 36 hours (45 DEG C) and 8 hours (110 DEG C) in vacuum drying oven respectively are first taken, then they are put in super mixer and be dry mixed 4 minutes, blended granulation in twin-screw blender again, obtains PLA conductive agglomerate.Prilling temperature is 180 DEG C, and screw speed is 60rmp, and the melt blending time is 7 minutes.
(2) by the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity PLA as-spun fibre, spinning temperature is 200 DEG C, and winding speed is 3000m/min;
(3) carry out drawing-off to as-spun fibre, obtain PLA conductive fiber, drawing temperature is 100 DEG C, 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) 65 parts of PLA (content of L-lactic acid unit is 1.0mol%) are first taken, 35 parts of P (VAc-co-VA) and 2.5 parts of SWCNTs dry 12 hours (90 DEG C) in vacuum drying oven respectively, 48 hours (40 DEG C) and 12 hours (100 DEG C), the P (VAc-co-VA) of drying and conductive agglomerate are put in super mixer and is dry mixed 3 minutes, blended granulation in twin-screw blender again, then blended granulation in twin-screw blender, obtain P (VAc-co-VA) conductive agglomerate, melt blending temperature is 170 DEG C, rotating speed is 75rmp, the melt blending time is 6 minutes, put in super mixer by P (VAc-co-VA) conductive agglomerate of the PLA of drying and gained and be dry mixed 3 minutes, melt blending obtains PLA conductive agglomerate, and temperature is 190 DEG C, and rotating speed is 80rmp, and the melt blending time is 6 minutes, obtains PLA conductive agglomerate.
(2) by the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity PLA as-spun fibre, spinning temperature is 190 DEG C, and winding speed is 2000m/min;
(3) carry out drawing-off to as-spun fibre, obtain PLA conductive fiber, drawing temperature is 100 DEG C, 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) 60 parts of PLA (content of L-lactic acid unit is 2.5mol%) are first taken, 40 parts of P (VAc-co-VA) and 6 parts of carbon blacks dry 12 hours (90 DEG C) in vacuum drying oven respectively, 48 hours (40 DEG C) and 12 hours (100 DEG C), the P (VAc-co-VA) of drying and conductive agglomerate are put in super mixer and is dry mixed 4 minutes, blended granulation in twin-screw blender again, then blended granulation in twin-screw blender, obtain P (VAc-co-VA) conductive agglomerate, melt blending temperature is 170 DEG C, rotating speed is 75rmp, the melt blending time is 6 minutes, put in super mixer by P (VAc-co-VA) conductive agglomerate of the PLA of drying and gained and be dry mixed 4 minutes, melt blending obtains PLA conductive agglomerate, and temperature is 190 DEG C, and rotating speed is 80rmp, and the melt blending time is 6 minutes, obtains PLA conductive agglomerate.
(2) by the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity PLA as-spun fibre, spinning temperature is 190 DEG C, and winding speed is 1500m/min;
(3) carry out drawing-off to as-spun fibre, obtain PLA conductive fiber, drawing temperature is 100 DEG C, 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 (2)
1. PLA (PLA) conductive fiber, be made up of 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;
Wherein the viscosity average molecular weigh of PLA is: 6.0 × 10
4~ 3.0 × 10
5;
In PLA, the content of L-lactic acid unit is: 0 ~ 10mol%;
Conductive filler is the one in carbon black (CB), Single Walled Carbon Nanotube (SWCNTs), multi-walled carbon nano-tubes (MWCNTs), Graphene (GN), gas phase nano carbon fiber (VGCNFs), copper sulfide, cuprous sulfide and cuprous iodide;
The viscosity average molecular weigh of P (VAc-co-VA) is 5.0 × 10
4~ 1.0 × 10
6;
The ratio of the vinyl alcohol construction unit in P (VAc-co-VA) is 9mol% ~ 80mol%.
2. the preparation method of PLA conductive fiber according to claim 1, comprises the steps:
(1) in advance the baking temperature of PLA, P (VAc-co-VA) and conductive filler dry 8 ~ 48h, PLA, P (VAc-co-VA) and conductive filler in vacuum drying oven is respectively 50 ~ 120 DEG C, 25 ~ 55 DEG C and 50 ~ 120 DEG C;
(2) get PLA50 ~ 80 part, P (VAc-co-VA) 20 ~ 50 parts and conductive filler 0.05 ~ 8 part to put in super mixer and be dry mixed 3 ~ 5 minutes, then blended granulation in twin-screw blender, obtain PLA conductive agglomerate, prilling temperature is 160 ~ 220 DEG C, rotating speed is 50 ~ 150rmp, and the melt blending time is 3 ~ 8 minutes; Or first get 20 ~ 50 parts of P (VAc-co-VA) and 0.05 ~ 8 part of conductive agglomerate to put in super mixer and be dry mixed 3 ~ 5 minutes, then blended granulation in twin-screw blender, obtain P (VAc-co-VA) conductive agglomerate, melt blending temperature is 160 ~ 220 DEG C, rotating speed is 50 ~ 150rmp, the melt blending time is 3 ~ 6 minutes, then get P (VAc-co-VA) conductive agglomerate of 50 ~ 80 parts of PLA and gained blended PLA conductive agglomerate, prilling temperature is 160 ~ 220 DEG C, rotating speed is 50 ~ 150rmp, and the melt blending time is 3 ~ 8 minutes;
(3) by the spinning on melt spinning machine of PLA conductive agglomerate, must conduct electricity PLA as-spun fibre, spinning temperature is 170 ~ 220 DEG C, and winding speed is 1500 ~ 3000m/min;
(4) carry out drawing-off to as-spun fibre, obtain PLA conductive fiber, drawing temperature is 100 ~ 125 DEG C, and drafting multiple is 1 ~ 6 times.
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| 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 |
| CN106676679A (en) * | 2016-11-08 | 2017-05-17 | 江南大学 | Preparation method of polylactic acid conductive fibers |
| 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 |
| CN106609400B (en) * | 2017-01-04 | 2018-04-20 | 苏州金泉新材料股份有限公司 | A kind of preparation method of multi-functional acid fiber by polylactic |
| CN108593719B (en) * | 2018-06-26 | 2020-06-19 | 浙江大学 | Immunosensor based on flexible electrode |
| PL440577A1 (en) | 2022-03-08 | 2023-09-11 | Politechnika Gdańska | Method of obtaining an electrode |
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