CN116770458A - Bi-component conductive monofilament and preparation method thereof - Google Patents
Bi-component conductive monofilament and preparation method thereof Download PDFInfo
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- CN116770458A CN116770458A CN202311080234.7A CN202311080234A CN116770458A CN 116770458 A CN116770458 A CN 116770458A CN 202311080234 A CN202311080234 A CN 202311080234A CN 116770458 A CN116770458 A CN 116770458A
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- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000009987 spinning Methods 0.000 claims abstract description 35
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000011231 conductive filler Substances 0.000 claims abstract description 23
- 239000000835 fiber Substances 0.000 claims abstract description 22
- 239000004626 polylactic acid Substances 0.000 claims description 85
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 83
- 229920000520 poly(3-hydroxybutyrate-co-3-hydroxyvalerate) Polymers 0.000 claims description 47
- 238000002156 mixing Methods 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 35
- 208000012886 Vertigo Diseases 0.000 claims description 32
- 239000000155 melt Substances 0.000 claims description 23
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 22
- 238000009998 heat setting Methods 0.000 claims description 17
- 238000004804 winding Methods 0.000 claims description 17
- 238000001125 extrusion Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- REKYPYSUBKSCAT-UHFFFAOYSA-N 3-hydroxypentanoic acid Chemical compound CCC(O)CC(O)=O REKYPYSUBKSCAT-UHFFFAOYSA-N 0.000 claims description 14
- 239000000498 cooling water Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 2
- 238000005325 percolation Methods 0.000 abstract description 9
- 239000002861 polymer material Substances 0.000 abstract description 4
- 238000010276 construction Methods 0.000 abstract 1
- 238000007580 dry-mixing Methods 0.000 description 19
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 description 15
- 229920002994 synthetic fiber Polymers 0.000 description 13
- 239000012209 synthetic fiber Substances 0.000 description 13
- 238000011161 development Methods 0.000 description 9
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 description 8
- 239000006229 carbon black Substances 0.000 description 8
- 238000007306 functionalization reaction Methods 0.000 description 8
- 229920013724 bio-based polymer Polymers 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 239000002048 multi walled nanotube Substances 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 238000003912 environmental pollution Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012827 research and development Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229930182843 D-Lactic acid Natural products 0.000 description 2
- 239000002134 carbon nanofiber Substances 0.000 description 2
- 229940022769 d- lactic acid Drugs 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000002074 melt spinning Methods 0.000 description 2
- 229920000070 poly-3-hydroxybutyrate Polymers 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 229910021595 Copper(I) iodide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 description 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000005014 poly(hydroxyalkanoate) Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
Abstract
The invention relates to the technical field of high polymer materials. The invention discloses a bi-component conductive monofilament and a preparation method thereof, wherein the bi-component conductive monofilament is prepared by combining a composite spinning method and a method for constructing a double-percolation structure, so that the problems of poor spinnability, poor mechanical property and the like existing in the construction of only the double-percolation structure are solved, and a non-conductive component in the composite spinning has good spinnability and can ensure that the conductive monofilament has good mechanical property; in addition, the double-percolation structure is constructed in the conductive component of the bi-component conductive monofilament, so that the content of conductive filler in the conductive fiber prepared by the conventional composite spinning method is further reduced, and the cost is reduced.
Description
Technical Field
The disclosure relates to the technical field of high polymer materials, in particular to a bi-component conductive monofilament and a preparation method thereof.
Background
The yield of the synthetic fiber in 2021 China is 6152.4 ten thousand tons, the first time of the stable living is the world, the synthetic fiber and products thereof occupy very important position in national economy, and the development of the synthetic fiber in China at present has the following problems: firstly, the development of the synthetic fiber is limited by resource shortage, more than 90% of raw materials of the synthetic fiber depend on petroleum, and the raw materials are calculated according to the total amount and the consumption speed of the petroleum which are ascertained, and the fiber and the related industries thereof are in a 'no-rice cooking' state after 50 years; secondly, the development of the synthetic fiber is limited by environmental pollution, and petroleum-based chemical fiber cannot be degraded in the nature, so that the petroleum-based chemical fiber can bring about serious white pollution and seriously influence the life quality of people. Therefore, the focus of research and development of the synthetic fiber industry is turned to the research and development of renewable biodegradable materials as resources. Again, the production of the synthetic fibers in our country is still based on conventional fibers, the development of high and new technology fibers is lagged, the yield of the synthetic fibers is 2/3 of the total world, but the functionalization ratio is not high. Therefore, the functionalization and high performance of the chemical fiber are realized to improve the added value of the fiber, and the market competitiveness is enhanced to meet the needs of the development of the synthetic fiber in China.
Polylactic acid (PLA) and Polyhydroxyalkanoate (PHA), wherein the two most important commercial varieties are poly (3-hydroxybutyrate) (PHB) or poly (3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV), are two very important resources which are renewable, biodegradable and good in biocompatibility, and are thermoplastic polymer materials, and can be directly melt-spun to prepare fibers, and at present, the melt-spinning technology of PLA is mature, and PLA is expected to replace petroleum-based polymer materials to be raw materials of chemical fibers so as to solve the problems of resource shortage, environmental pollution and the like faced by the development of synthetic fibers. However, currently, little research and development work is done on functionalization of PLA fibers. The conductive functionalization of common fibers is an important point of development and research in industry and academia, and thus, it is necessary to realize the conductive functionalization of PLA fibers. However, in the current study of PLA fiber conductive functionalization, two-phase polymers are incompatible, and more conductive fillers are needed to be added, so that the spinnability and mechanical properties of the fibers are greatly limited, and the industrialization process of the fibers is influenced.
Disclosure of Invention
In view of the above, the embodiments of the present disclosure provide a bicomponent conductive monofilament and a preparation method thereof, which address the problems of resource shortage, environmental pollution, low degree of functionalization, and the like faced by the development of the current synthetic fibers.
In a first aspect, embodiments of the present disclosure provide a two-component conductive monofilament comprising a component a and a component B, wherein:
the component A is a non-conductive component, and the component A is a blend of polylactic acid with the content of the dextrorotatory lactic acid structural unit of 0-10 mol% and poly (3-hydroxybutyrate-co-3-hydroxyvalerate) with the content of the 3-hydroxyvalerate of 0-100 mol%; the polylactic acid in the component A has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 The poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in component A has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 ；
The component B is a conductive component, and is a blend of polylactic acid, poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and a conductive filler, wherein the content of a dextrorotatory lactic acid structural unit in the polylactic acid in the component B is 0-100%, and the content of the 3-hydroxyvalerate in the poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component B is 0-100 mol%; the polylactic acid in the component B has a viscosity average molecular weight of 5.0X10 5 ~1.0×10 6 The poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in component B has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 。
According to a specific implementation mode of the embodiment of the disclosure, the mass percentage of the poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component A is 0-50%.
According to a specific implementation manner of the embodiment of the disclosure, the mass ratio of polylactic acid to poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component B is 40: 60-60: 40.
according to a specific implementation manner of the embodiment of the disclosure, the mass ratio of the conductive filler in the component B is 0.05-8% of the total polymer.
According to a specific implementation manner of the embodiment of the disclosure, the composite ratio of the component A to the component B is 90: 10-50: 50.
in addition, the invention also provides a preparation method of the bi-component conductive monofilament, which comprises the following steps:
(1) Pretreatment of materials: pretreating the needed poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and polylactic acid;
(2) Taking a proper amount of poly (3-hydroxybutyrate-co-3-hydroxyvalerate), polylactic acid and conductive filler, and carrying out mixing treatment and granulation treatment to obtain a conductive slice;
(3) Mixing and granulating proper amounts of polylactic acid and poly (3-hydroxybutyrate-co-3-hydroxyvalerate) to obtain a polylactic acid/poly (3-hydroxybutyrate-co-3-hydroxyvalerate) blend;
(4) Drying the obtained conductive slice and the blend of polylactic acid and poly (3-hydroxybutyrate-co-3-hydroxyvalerate);
(5) And weighing the polylactic acid/poly (3-hydroxybutyrate-co-3-hydroxyvalerate) blend and the conductive slice according to a proportion, respectively serving as a component A and a component B of the bi-component conductive monofilament, and carrying out melt composite spinning treatment on the component A and the component B to obtain the bi-component conductive monofilament.
The step of taking a proper amount of poly (3-hydroxybutyrate-co-3-hydroxyvalerate), polylactic acid and conductive filler, and carrying out mixing treatment and granulation treatment to obtain the conductive slice comprises the following steps:
(1) When the weight part of the polylactic acid is more than or equal to 50 parts, 40-50 parts of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and 0.05-8 parts of conductive filler are taken to be mixed and granulated to obtain poly (3-hydroxybutyrate-co-3-hydroxyvalerate) conductive master batch; blending and granulating 50-60 parts of polylactic acid and the obtained poly (3-hydroxybutyrate-co-3-hydroxyvalerate) conductive master batch to obtain conductive slices;
or (2) when the weight part of the polylactic acid is less than 50 parts, mixing 40-50 parts of the polylactic acid and 0.05-8 parts of the conductive filler, and granulating to obtain the polylactic acid conductive master batch; and (3) blending and granulating 50-60 parts of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and the obtained PLA conductive master batch to obtain the conductive slice.
According to a specific implementation manner of the embodiment of the disclosure, the melt composite spinning method includes: the component A and the component B are respectively subjected to the procedures of melt extrusion, water bath cooling, one-step steam stretching, two-step hot air stretching, heat setting and oiling winding to prepare the bi-component guide fiber.
The extrusion temperatures corresponding to the component A and the component B are 130-220 ℃, the temperatures corresponding to the spinning box body are 160-240 ℃, the temperature of a cooling water bath is 20-70 ℃, the winding speed of one roll is 1-25 m/min, the stretching temperature of one water bath is 50-95 ℃, the stretching multiple is 2-15 times, the stretching multiple of two hot air stretching temperatures are 70-135 ℃, the stretching multiple is 1-10 times, and the heat setting temperature is 100-135 ℃.
According to a specific implementation of an embodiment of the present disclosure, the weight percentages of component a and component B are 90: 10-50: 50.
the bicomponent conductive monofilament in the embodiment of the disclosure and the preparation method thereof have the beneficial effects that:
(1) The main raw materials of the conductive monofilament in the invention are PLA and P (3 HB-co-3 HV), which are renewable resources and biodegradable materials, and are environment-friendly materials.
(2) The invention combines the composite spinning and the method for constructing the double-percolation structure to prepare the conductive monofilament, overcomes the problems of poor spinnability, poor mechanical property and the like existing in the method for constructing the double-percolation structure only, ensures that the non-conductive component in the composite spinning has good spinnability and can ensure that the conductive monofilament has better mechanical property; in addition, the double-percolation structure is constructed in the conductive component of the bi-component conductive monofilament, so that the content of conductive filler in the conductive fiber prepared by the conventional composite spinning method is further reduced, and the cost is reduced.
Detailed Description
The present embodiment is described in detail below with reference to examples.
Other advantages and effects of the present disclosure will become readily apparent to those skilled in the art from the following disclosure, which describes embodiments of the present disclosure by way of specific examples. It will be apparent that the described embodiments are merely some, but not all embodiments of the present disclosure. The disclosure may be embodied or practiced in other different specific embodiments, and details within the subject specification may be modified or changed from various points of view and applications without departing from the spirit of the disclosure. It should be noted that the following embodiments and features in the embodiments may be combined with each other without conflict. All other embodiments, which can be made by one of ordinary skill in the art without inventive effort, based on the embodiments in this disclosure are intended to be within the scope of this disclosure.
It is noted that various aspects of the embodiments are described below within the scope of the following claims. It should be apparent that the aspects described herein may be embodied in a wide variety of forms and that any specific structure and/or function described herein is merely illustrative. Based on the present disclosure, one skilled in the art will appreciate that one aspect described herein may be implemented independently of any other aspect, and that two or more of these aspects may be combined in various ways. For example, an apparatus may be implemented and/or a method practiced using any number of the aspects set forth herein. In addition, such apparatus may be implemented and/or such methods practiced using other structure and/or functionality in addition to one or more of the aspects set forth herein.
In addition, in the following description, specific details are provided in order to provide a thorough understanding of the examples. However, it will be understood by those skilled in the art that the aspects may be practiced without these specific details.
Embodiments of the present disclosure provide a bicomponent conductive monofilament comprising component a and component B, wherein:
the component A is a non-conductive component, and the component A is a blend of polylactic acid with the content of the dextrorotatory lactic acid structural unit of 0-10 mol% and poly (3-hydroxybutyrate-co-3-hydroxyvalerate) with the content of the 3-hydroxyvalerate of 0-100 mol%; the polylactic acid in the component A has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 The poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in component A has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 ；
The component B is a conductive component, the component B is a blend of polylactic acid, poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and conductive filler,wherein the content of the structural unit of the D-lactic acid in the polylactic acid in the component B is 0-100%, and the content of the 3-hydroxyvalerate in the poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component B is 0-100 mol%; the polylactic acid in the component B has a viscosity average molecular weight of 5.01.0 ×10 5 ~1.0×10 6 The poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in component B has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 。
The main raw materials of the conductive monofilament in the invention are polylactic acid and poly (3-hydroxybutyrate-co-3-hydroxyvalerate), which are renewable resources and biodegradable, are environment-friendly materials, and solve the problems of resource shortage, environmental pollution, low functionalization degree and the like in the development of the existing synthetic fiber. The obtained conductive monofilament is a high-diameter bio-based polymer conductive monofilament with good mechanical properties.
Specifically, in the bicomponent conductive monofilament of the embodiment of the invention, the mass percentage of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component A is 0-50%; the mass ratio of polylactic acid to poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component B is 40: 60-60: 40. the mass ratio of the conductive filler in the component B is 0.05-8% of the total polymer. The composite ratio of the component A to the component B is 90: 10-50: 50;
the bicomponent conductive monofilament of the embodiment of the invention is formed in an optimal proportioning range, and is as follows:
the bicomponent conductive monofilament of this embodiment comprises a component a and a component B, wherein:
the component A is a non-conductive component and is a blend of polylactic acid (PLA) with 0-10 mol% of D-lactic acid structural unit (D-LA) and poly (3-hydroxybutyrate-co-3-hydroxyvalerate) (P (3 HB-co-3 HV)) with 0-100 mol% of 3-hydroxyvalerate, wherein the mass percentage of the P (3 HB-co-3 HV) is 0-50%; PLA had a viscosity-average molecular weight of 1.0X10 5 ~1.0×10 6 P (3 HB-co-3 HV) having a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 ；
Component B, which is a conductive component, is a blend of PLA, P (3 HB-co-3 HV) and a conductive fillerThe mixture comprises 0-100% of D-LA in PLA, 0-100 mol% of HV in P (3 HB-co-3 HV), and 40% of PLA and P (3 HB-co-3 HV) by mass: 60-60: 40, the conductive filler is 0.05-8% of the total polymer; wherein the conductive filler is one or two of MXene, carbon Black (CB), single-walled carbon nanotubes (SWCNTs), multi-walled carbon nanotubes (MWCNTs), graphene (GN), gas-phase carbon nanofibers (VGCNFs), fullerene, titanium carbide, copper sulfide, cuprous sulfide and cuprous iodide; PLA has a viscosity-average molecular weight of 5.0X10 5 ~1.0×10 6 P (3 HB-co-3 HV) having a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 ；
The composite ratio of the component A to the component B is 90: 10-50: 50.
in addition, the invention also provides a preparation method of the bi-component conductive monofilament, which comprises the following steps:
(1) PLA, P (3 HB-co-3 HV) and conductive filler are dried in a vacuum oven for 8 to 48 hours in advance, and the drying temperature is 50 to 120 ℃;
(2) When the weight part of PLA is not less than 50 parts, 40 to 50 parts of P (3 HB-co-3 HV) and 0.05 to 8 parts of conductive filler are taken and put into a high-speed mixer for dry mixing for 3 to 5 minutes, and then the mixture is blended and granulated in a double-screw blending machine to obtain P (3 HB-co-3 HV) conductive master batch, wherein the melt blending temperature is 130 to 220 ℃ and the rotating speed is 300 to 500rmp; putting 50-60 parts of PLA and the obtained P (3 HB-co-3 HV) conductive master batch into a high-speed mixer for dry mixing for 3-5 minutes, and then blending and granulating on a double-screw blender to obtain conductive slices, wherein the melt blending temperature is 130-220 ℃ and the rotating speed is 300-500 rmp;
if the weight part of PLA is less than 50 parts, taking 40-50 parts of PLA and 0.05-8 parts of conductive filler, putting into a high-speed mixer, dry mixing for 3-5 minutes, and then blending and granulating in a double-screw blender to obtain PLA conductive master batch, wherein the melt blending temperature is 130-220 ℃ and the rotating speed is 300-500 rmp; 50 to 60 parts of P (3 HB-co-3 HV) and the obtained PLA conductive master batch are put into a high-speed mixer to be dry mixed for 3 to 5 minutes, and then are mixed and granulated on a double-screw mixer to obtain conductive slices, wherein the melt blending temperature is 130 to 220 ℃ and the rotating speed is 300 to 500rmp;
(3) Taking 50-100 parts of PLA and 50-100 parts of P (3 HB-co-3 HV), putting into a high-speed mixer, dry mixing for 3-5 minutes, and then blending and granulating in a double-screw blender to obtain a PLA/P (3 HB-co-3 HV) blend, wherein the melt blending temperature is 160-220 ℃ and the rotating speed is 300-500 rmp;
(4) Drying the prepared conductive slice and PLA/P (3 HB-co-3 HV) blend in a vacuum oven for 8-48 h at the drying temperature of 50-120 ℃;
(5) The PLA/P (3 HB-co-3 HV) blend and the conductive slice are weighed according to a proportion and respectively used as a component A and a component B of the conductive fiber, the component A and the component B are respectively added into a hopper of a melt composite spinning device for melt composite spinning, and the two-component conductive monofilament is prepared through the procedures of melt extrusion, water bath cooling, one-step steam stretching, two-step hot air stretching, heat setting and oiling winding, wherein the screw extrusion temperatures corresponding to the component A and the component B are 130-220 ℃, the temperature corresponding to a spinning box is 160-240 ℃, the temperature of a cooling water bath is 20-70 ℃, the winding speed of one roll is 1-25 m/min, the temperature of one-step water bath stretching is 50-95 ℃, the stretching multiple is 2-15 times, the temperature of two-step hot air stretching is 70-135 ℃, the stretching multiple is 1-10 times, and the heat setting temperature is 100-135 ℃; the weight percentage of the component A and the component B is 90: 10-50: 50.
the invention combines the composite spinning and the method for constructing the double-percolation structure to prepare the conductive monofilament, overcomes the problems of poor spinnability, poor mechanical property and the like existing in the method for constructing the double-percolation structure only, ensures that the non-conductive component in the composite spinning has good spinnability and can ensure that the conductive monofilament has better mechanical property; in addition, the double-percolation structure is constructed in the conductive component of the bi-component conductive monofilament, so that the content of conductive filler in the conductive fiber prepared by the conventional composite spinning method is further reduced, and the cost is reduced.
The excellent properties of the bicomponent conductive monofilaments prepared by the process of the present invention will be described below with reference to specific examples.
Example 1:
(1) PLA (content of D-lactic acid unit was 2.0mol% and viscosity average molecular weight was 2.0' -10) 5 ) P (3 HB-co-3 HV) (HV unit content of 2.5%, viscosity average molecular weight of 3.9' -10) 5 ) And carbon black are dried in a vacuum oven for 12 hours respectively, and the temperature is 80 ℃; 50 parts of P (3 HB-co-3 HV) and 5 parts of carbon black are put into a high-speed mixer for dry mixing for 5 minutes, and then are blended and granulated in a double-screw blender to obtain P (3 HB-co-3 HV) conductive master batch, wherein the granulating temperature is 175 ℃, and the screw rotating speed is 420rmp; 50 parts of PLA and the obtained P (3 HB-co-3 HV) conductive master batch are put into a high-speed mixer to be dry mixed for 3 minutes, and then are mixed and granulated on a double-screw mixer to obtain conductive slices, wherein the melt blending temperature is 180 ℃, and the screw rotating speed is 420rmp.
(2) Putting 90 parts of PLA and 10 parts of P (3 HB-co-3 HV) into a high-speed mixer for dry mixing for 3 minutes, and then blending and granulating in a double-screw blender to obtain a PLA/P (3 HB-co-3 HV) blend, wherein the melt blending temperature is 180 ℃, and the screw rotating speed is 420rmp;
(3) The prepared conductive slice and PLA/P (3 HB-co-3 HV) blend were dried in a vacuum oven for 24 hours at 90 ℃;
(4) PLA/P (3 HB-co-3 HV) blend and conductive slices are weighed according to the proportion of 50:50 and respectively used as a component A and a component B of the conductive monofilament, the component A and the component B are respectively added into a hopper of a melt composite spinning device for melt composite spinning, and the conductive monofilament with the sheath-core structure high-strength diameter bio-based polymer, the component B of which is a sheath and the component A of which is a core, is prepared through the procedures of melt extrusion, water bath cooling, one-step hot air stretching, two-step hot air stretching, heat setting and oiling winding, the screw extrusion temperatures of the component A and the component B are 190 ℃, the spinning box temperature is 185 ℃, the temperature of a cooling water bath is 50 ℃, the winding speed of one roll is 20m/min, the temperature of one-step water bath stretching is 90 ℃, the stretching multiple is 6 times, the temperature of two-step hot air stretching is 120 ℃, the stretching multiple is 1.2 times, and the heat setting temperature is 130 ℃.
The conductivity of the obtained conductive monofilament was 1.32S/m, the diameter of the monofilament was 0.1mm, the breaking strength was 3.23cN/dtex, and the elongation at break was 23.8%.
Example 2:
(1) PLA (content of D-lactic acid unit was 2.5mol% and viscosity average molecular weight was 2.2' -10) 5 ) P (3 HB-co-3 HV) (HV unit content 5.7%, viscosity average molecular weight 2.9' -10) 5 ) And MWCNTs were dried in a vacuum oven for 36 hours at a temperature of 80 o C, performing operation; 40 parts of P (3 HB-co-3 HV) and 3.5 parts of MWCNTs are put into a high-speed mixer for dry mixing for 5 minutes, and then are blended and granulated in a double-screw blender to obtain the P (3 HB-co-3 HV) conductive master batch, wherein the granulating temperature is 170 o C, the rotating speed of the screw is 450rmp; taking 60 parts of PLA and the obtained P (3 HB-co-3 HV) conductive master batch, putting into a high-speed mixer, dry mixing for 5 minutes, and then blending and granulating on a double-screw blender to obtain conductive slices, wherein the melt blending temperature is 180 DEG C o C, the rotating speed of the screw is 450rmp;
(2) 95 parts of PLA and 5 parts of P (3 HB-co-3 HV) are put into a high-speed mixer for dry mixing for 5 minutes, and then blended and granulated in a double screw blender to obtain PLA/P (3 HB-co-3 HV) blend with the melt blending temperature of 180 DEG C o C, the rotating speed of the screw is 450rmp;
(3) Drying the prepared conductive slice and PLA/P (3 HB-co-3 HV) blend in a vacuum oven for 36h at 80 ℃;
(4) PLA/P (3 HB-co-3 HV) blend and conductive slices are weighed according to the ratio of 60:40 and respectively used as a component A and a component B of the conductive monofilament, the components are respectively added into a hopper of a melt composite spinning device for melt composite spinning, and the parallel high-strength high-diameter bio-based polymer conductive monofilament is prepared through the processes of melt extrusion, water bath cooling, one-step hot air stretching, two-step hot air stretching, heat setting and oiling winding, wherein the screw extrusion temperature of the component A and the component B is 185 ℃, the temperature of a spinning box is 185 ℃, the temperature of a cooling water bath is 45 ℃, the winding speed of one roll is 20m/min, the temperature of one-step water bath stretching is 90 ℃, the stretching multiple is 6.5 times, the temperature of two-step hot air stretching is 120 ℃, the stretching multiple is 1.2 times, and the heat setting temperature is 130 ℃. The conductivity of the obtained conductive monofilament was 1.29S/m, the diameter of the monofilament was 0.1mm, the breaking strength was 3.48cN/dtex, and the elongation at break was 19.2%.
Example 3:
(1) PLA (content of D-lactic acid unit was 1.5mol% and viscosity average molecular weight was 2.2' -10) 5 ) P (3 HB-co-3 HV) (HV unit content of 2.5%, viscosity average molecular weight of 5.0' -10) 5 ) And MXene fractionDrying in vacuum oven for 36 hr at 80 deg.C o C, performing operation; 40 parts of P (3 HB-co-3 HV) and 3.5 parts of MXene are put into a high-speed mixer for dry mixing for 5 minutes, and then are blended and granulated in a double-screw blender to obtain the P (3 HB-co-3 HV) conductive master batch, wherein the granulating temperature is 175 o C, the rotating speed of the screw is 450rmp; taking 60 parts of PLA and the obtained P (3 HB-co-3 HV) conductive master batch, putting into a high-speed mixer, dry mixing for 5 minutes, and then blending and granulating on a double-screw blender to obtain conductive slices, wherein the melt blending temperature is 185 o C, the rotating speed of the screw is 450rmp;
(2) Putting 90 parts of PLA and 10 parts of P (3 HB-co-3 HV) into a high-speed mixer for dry mixing for 5 minutes, and then blending and granulating in a double-screw blender to obtain PLA/P (3 HB-co-3 HV) blend with the melt blending temperature of 185 o C, the rotating speed of the screw is 450rmp;
(3) Drying the prepared conductive slice and PLA/P (3 HB-co-3 HV) blend in a vacuum oven for 36h at 80 ℃;
(4) PLA/P (3 HB-co-3 HV) blend and conductive slices are weighed according to the proportion of 70:30 and respectively used as a component A and a component B of conductive fibers, the components A and the B are respectively added into a hopper of a melt composite spinning device for melt composite spinning, and the parallel high-strength high-diameter bio-based polymer conductive monofilament is prepared through the processes of melt extrusion, water bath cooling, one-step hot air stretching, two-step hot air stretching, heat setting and oiling winding, wherein the screw extrusion temperature of the component A and the component B is 190 ℃, the temperature of a spinning box is 185 ℃, the temperature of a cooling water bath is 50 ℃, the winding speed of one roll is 20m/min, the temperature of one-step water bath stretching is 90 ℃, the stretching multiple is 6 times, the temperature of two-step hot air stretching is 120 ℃, the stretching multiple is 1.2 times, and the heat setting temperature is 130 ℃.
The conductivity of the obtained conductive monofilament was 1.52S/m, the diameter of the monofilament was 0.1mm, the breaking strength was 3.37cN/dtex, and the elongation at break was 26.5%.
Example 4:
(1) PLA (content of D-lactic acid unit was 2.0mol% and viscosity average molecular weight was 2.0' -10) 5 ) P (3 HB-co-3 HV) (content of HV unit was 8.5%, viscosity average molecular weight was 3.2' -10) 5 ) AndMWCNTs were dried in vacuum oven for 36 hours at 80℃respectively o C, performing operation; 40 parts of P (3 HB-co-3 HV) and 4 parts of MWCNTs are put into a high-speed mixer for dry mixing for 5 minutes, and then are blended and granulated in a double-screw blender to obtain the P (3 HB-co-3 HV) conductive master batch, wherein the granulating temperature is 170 o C, the rotating speed of the screw is 450rmp; taking 60 parts of PLA and the obtained P (3 HB-co-3 HV) conductive master batch, putting into a high-speed mixer, dry mixing for 5 minutes, and then blending and granulating on a double-screw blender to obtain conductive slices, wherein the melt blending temperature is 180 DEG C o C, the rotating speed of the screw is 450rmp;
(2) 95 parts of PLA and 5 parts of P (3 HB-co-3 HV) are put into a high-speed mixer for dry mixing for 5 minutes, and then blended and granulated in a double screw blender to obtain PLA/P (3 HB-co-3 HV) blend with the melt blending temperature of 180 DEG C o C, the rotating speed of the screw is 450rmp;
(3) Drying the prepared conductive slice and PLA/P (3 HB-co-3 HV) blend in a vacuum oven for 36h at 80 ℃;
(4) PLA/P (3 HB-co-3 HV) blend and conductive slices are weighed according to the proportion of 75:25 and respectively used as a component A and a component B of the conductive monofilament, the components are respectively added into a hopper of a melt composite spinning device for melt composite spinning, the component B is a sheath, the component A is a sheath-core structure high-strength high-diameter bio-based polymer conductive monofilament with a core, the screw extrusion temperature of the component A and the component B is 190 ℃, the temperature of a spinning box is 185 ℃, the temperature of a cooling water bath is 50 ℃, the winding speed of a roll is 20m/min, the temperature of the one-pass stretching is 90 ℃, the stretching multiple is 6 times, the temperature of the two-pass hot air stretching is 120 ℃, the stretching multiple is 1.2 times, and the heat setting temperature is 130 ℃.
The conductivity of the obtained conductive monofilament was 1.12S/m, the diameter of the monofilament was 0.1mm, the breaking strength was 3.83cN/dtex, and the elongation at break was 18.5%.
To address the superiority of the performance of the bicomponent conductive monofilaments obtained using the above examples, the present invention is illustrated with the following two comparative examples.
Comparative example 1
(1) PLA (content of D-lactic acid unit was 2.0mol% and viscosity average molecular weight was 2.0' -10) 5 ) P (3 HB-co-3 HV) (HV unit content of 2.5%, viscosity average molecular weight of 3.9' -10) 5 ) And carbon black are dried in a vacuum oven for 12 hours respectively, and the temperature is 80 ℃; 50 parts of P (3 HB-co-3 HV) and 5 parts of carbon black are put into a high-speed mixer for dry mixing for 5 minutes, and then are blended and granulated in a double-screw blender to obtain P (3 HB-co-3 HV) conductive master batch, wherein the granulating temperature is 175 ℃, and the screw rotating speed is 420rmp; putting 50 parts of PLA and the obtained P (3 HB-co-3 HV) conductive master batch into a high-speed mixer for dry mixing for 3 minutes, and then carrying out blending granulation on a double-screw blender to obtain conductive slices, wherein the melt blending temperature is 180 ℃, and the screw rotating speed is 420rmp;
(2) Drying the prepared conductive slice in a vacuum oven for 24 hours at 90 ℃;
(3) The high-strength large-diameter bio-based polymer conductive monofilament is prepared by taking conductive slices as raw materials for melt spinning through the procedures of melt extrusion, water bath cooling, one-step steam stretching, two-step hot air stretching, heat setting and oiling winding, wherein the temperature of a spinning box body is 185 ℃, the temperature of a cooling water bath is 50 ℃, the winding speed of a roller is 20m/min, the temperature of one-step water bath stretching is 90 ℃, the stretching multiple is 3 times, the temperature of two-step hot air stretching is 120 ℃, the stretching multiple is 1.1 times, and the heat setting temperature is 130 ℃.
The conductivity of the obtained conductive monofilament was 1.53S/m, the diameter of the monofilament was 0.1mm, the breaking strength was 2.39cN/dtex, and the elongation at break was 29.8%.
Comparison of comparative example 1 and example 1 shows that comparative example 1 is difficult to perform high-power drawing and spinning is difficult.
Comparative example 2
(1) PLA (content of D-lactic acid unit was 2.0mol% and viscosity average molecular weight was 2.0' -10) 5 ) P (3 HB-co-3 HV) (HV unit content of 2.5%, viscosity average molecular weight of 3.9' -10) 5 ) And carbon black are dried in a vacuum oven for 12 hours respectively, and the temperature is 80 ℃; 100 parts of P (3 HB-co-3 HV) and 5 parts of carbon black are taken and put into a high speed mixer for dry mixing for 5 minutes, and thenBlending and granulating in a double-screw blender to obtain P (3 HB-co-3 HV) conductive slices, wherein the granulating temperature is 175 ℃ and the screw rotating speed is 420rmp;
(2) Putting 90 parts of PLA and 10 parts of P (3 HB-co-3 HV) into a high-speed mixer for dry mixing for 3 minutes, and then blending and granulating in a double-screw blender to obtain a PLA/P (3 HB-co-3 HV) blend, wherein the melt blending temperature is 180 ℃, and the screw rotating speed is 420rmp;
(3) The prepared conductive slice and PLA/P (3 HB-co-3 HV) blend were dried in a vacuum oven for 24 hours at 90 ℃;
(4) PLA/P (3 HB-co-3 HV) blend and conductive slices are weighed according to the proportion of 50:50 and respectively used as a component A and a component B of the conductive monofilament, the component A and the component B are respectively added into a hopper of a melt composite spinning device for melt composite spinning, and the conductive monofilament with the sheath-core structure high-strength diameter bio-based polymer, the component B of which is a sheath and the component A of which is a core, is prepared through the procedures of melt extrusion, water bath cooling, one-step hot air stretching, two-step hot air stretching, heat setting and oiling winding, the screw extrusion temperatures of the component A and the component B are 190 ℃, the spinning box temperature is 185 ℃, the temperature of a cooling water bath is 50 ℃, the winding speed of one roll is 20m/min, the temperature of one-step water bath stretching is 90 ℃, the stretching multiple is 6 times, the temperature of two-step hot air stretching is 120 ℃, the stretching multiple is 1.2 times, and the heat setting temperature is 130 ℃.
The conductivity of the obtained conductive monofilament was 0.13S/m, the diameter of the monofilament was 0.1mm, the breaking strength was 3.45cN/dtex, and the elongation at break was 19.6%.
Comparison of comparative example 2 and example 1 shows that the conductive monofilaments produced in comparative example 2 have low conductivity.
The foregoing is merely specific embodiments of the disclosure, but the protection scope of the disclosure is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the disclosure are intended to be covered by the protection scope of the disclosure. Therefore, the protection scope of the present disclosure shall be subject to the protection scope of the claims.
Claims (10)
1. A bicomponent conductive monofilament, wherein the bicomponent conductive monofilament comprises a component a and a component B, wherein:
the component A is a non-conductive component, and the component A is a blend of polylactic acid with the content of the dextrorotatory lactic acid structural unit of 0-10 mol% and poly (3-hydroxybutyrate-co-3-hydroxyvalerate) with the content of the 3-hydroxyvalerate of 0-100 mol%; the polylactic acid in the component A has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 The poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in component A has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 ；
The component B is a conductive component, and is a blend of polylactic acid, poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and a conductive filler, wherein the content of a dextrorotatory lactic acid structural unit in the polylactic acid in the component B is 0-100%, and the content of the 3-hydroxyvalerate in the poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component B is 0-100 mol%; the polylactic acid in the component B has a viscosity average molecular weight of 5.0X10 5 ~1.0×10 6 The poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in component B has a viscosity average molecular weight of 1.0X10 5 ~1.0×10 6 。
2. The two-component conductive monofilament according to claim 1, wherein the mass percentage of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component a is 0-50%.
3. The two-component conductive monofilament according to claim 1, wherein the mass ratio of polylactic acid to poly (3-hydroxybutyrate-co-3-hydroxyvalerate) in the component B is 40: 60-60: 40.
4. the bicomponent conductive monofilament according to claim 1, wherein the mass ratio of the conductive filler in the component B is 0.05 to 8% of the total amount of the polymer.
5. The bicomponent conductive monofilament according to any one of claims 1 to 4, wherein the composite ratio of component a and component B is 90: 10-50: 50.
6. a method for preparing a bicomponent conductive monofilament, comprising:
(1) Pretreatment of materials: pretreating the needed poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and polylactic acid;
(2) Taking a proper amount of poly (3-hydroxybutyrate-co-3-hydroxyvalerate), polylactic acid and conductive filler, and carrying out mixing treatment and granulation treatment to obtain a conductive slice;
(3) Mixing and granulating proper amounts of polylactic acid and poly (3-hydroxybutyrate-co-3-hydroxyvalerate) to obtain a polylactic acid/poly (3-hydroxybutyrate-co-3-hydroxyvalerate) blend;
(4) Drying the obtained conductive slice and the blend of polylactic acid and poly (3-hydroxybutyrate-co-3-hydroxyvalerate);
(5) And weighing the polylactic acid/poly (3-hydroxybutyrate-co-3-hydroxyvalerate) blend and the conductive slice according to a proportion, respectively serving as a component A and a component B of the bi-component conductive monofilament, and carrying out melt composite spinning treatment on the component A and the component B to obtain the bi-component conductive monofilament.
7. The method for preparing the bicomponent conductive monofilament according to claim 6, wherein the step of taking a proper amount of poly (3-hydroxybutyrate-co-3-hydroxyvalerate), polylactic acid and conductive filler, mixing and granulating the mixture to obtain the conductive chips comprises the steps of:
(1) When the weight part of the polylactic acid is more than or equal to 50 parts, 40-50 parts of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and 0.05-8 parts of conductive filler are taken to be mixed and granulated to obtain poly (3-hydroxybutyrate-co-3-hydroxyvalerate) conductive master batch; blending and granulating 50-60 parts of polylactic acid and the obtained poly (3-hydroxybutyrate-co-3-hydroxyvalerate) conductive master batch to obtain conductive slices;
or (2) when the weight part of the polylactic acid is less than 50 parts, mixing 40-50 parts of the polylactic acid and 0.05-8 parts of the conductive filler, and granulating to obtain the polylactic acid conductive master batch; and (3) blending and granulating 50-60 parts of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) and the obtained polylactic acid conductive master batch to obtain the conductive slice.
8. The method for producing a bicomponent conductive monofilament according to claim 6, wherein the melt composite spinning method comprises: the component A and the component B are respectively subjected to the procedures of melt extrusion, water bath cooling, one-step steam stretching, two-step hot air stretching, heat setting and oiling winding to prepare the bi-component guide fiber.
9. The method for producing a bicomponent conductive monofilament according to claim 8, wherein the extrusion temperatures of the component a and the component B are 130 to 220 ℃, the temperatures of the spinning beams are 160 to 240 ℃, the temperatures of the cooling water baths are 20 to 70 ℃, the winding speed of one roll is 1 to 25m/min, the stretching temperature of one water bath is 50 to 95 ℃, the stretching multiple is 2 to 15 times, the stretching temperature of two hot air is 70 to 135 ℃, the stretching multiple is 1 to 10 times, and the heat setting temperature is 100 to 135 ℃.
10. The method for preparing the bi-component conductive monofilament according to claim 6-9, wherein the weight percentage of the component A and the component B is 90: 10-50: 50.
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| CN102936761A (en) * | 2012-12-11 | 2013-02-20 | 江南大学 | Resource-renewable and biodegradable conductive fiber and preparation method thereof |
| CN102942773A (en) * | 2012-12-11 | 2013-02-27 | 江南大学 | Tenacious, recyclable and biodegradable composite material and preparation method thereof |
| CN106400183A (en) * | 2016-09-22 | 2017-02-15 | 江南大学 | Poly-(3-polyhydroxybutyrate-co-3-polyhydroxybutyrate-hydroxyvalerate) multifilament and preparation method thereof |
| CN106948168A (en) * | 2017-03-07 | 2017-07-14 | 江苏中杰澳新材料有限公司 | Composite construction conductive fiber of carbon nano-tube coating and preparation method thereof |
| WO2017155043A1 (en) * | 2016-03-10 | 2017-09-14 | ナノサミット株式会社 | Conductive fiber and method for manufacturing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102936761A (en) * | 2012-12-11 | 2013-02-20 | 江南大学 | Resource-renewable and biodegradable conductive fiber and preparation method thereof |
| CN102942773A (en) * | 2012-12-11 | 2013-02-27 | 江南大学 | Tenacious, recyclable and biodegradable composite material and preparation method thereof |
| WO2017155043A1 (en) * | 2016-03-10 | 2017-09-14 | ナノサミット株式会社 | Conductive fiber and method for manufacturing same |
| CN106400183A (en) * | 2016-09-22 | 2017-02-15 | 江南大学 | Poly-(3-polyhydroxybutyrate-co-3-polyhydroxybutyrate-hydroxyvalerate) multifilament and preparation method thereof |
| CN106948168A (en) * | 2017-03-07 | 2017-07-14 | 江苏中杰澳新材料有限公司 | Composite construction conductive fiber of carbon nano-tube coating and preparation method thereof |
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