CN113718527A - High-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber and preparation method thereof - Google Patents
High-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber and preparation method thereof Download PDFInfo
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- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 title claims abstract description 60
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims abstract description 20
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims abstract description 12
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- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims description 2
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 1
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- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 2
- 229940043264 dodecyl sulfate Drugs 0.000 description 2
- LLDIZGVRYGOOLU-UHFFFAOYSA-L dodecyl sulfate;iron(2+) Chemical compound [Fe+2].CCCCCCCCCCCCOS([O-])(=O)=O.CCCCCCCCCCCCOS([O-])(=O)=O LLDIZGVRYGOOLU-UHFFFAOYSA-L 0.000 description 2
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- 239000004698 Polyethylene Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 229920010741 Ultra High Molecular Weight Polyethylene (UHMWPE) Polymers 0.000 description 1
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- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
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- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/262—Sulfated compounds thiosulfates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
Abstract
The invention relates to a high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber and a preparation method thereof, wherein the ultrahigh molecular weight polyethylene fiber is connected with a poly (3, 4-ethylenedioxythiophene) conducting layer through alkyl ferric sulfate, the preparation method comprises the following steps of cleaning and drying the ultrahigh molecular weight polyethylene fiber, coating and wrapping an alcohol solution of alkyl ferric sulfate on the ultrahigh molecular weight polyethylene fiber, removing redundant solution, then placing the ultrahigh molecular weight polyethylene fiber in steam containing 3, 4-ethylenedioxythiophene monomers, removing unreacted substances after gas phase polymerization reaction is finished, and drying to obtain the high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber; the conductive effect is good and the strength is high.
Description
Technical Field
The invention belongs to the technical field of ultra-high molecular weight polyethylene fibers, and particularly relates to a high-strength high-conductivity ultra-high molecular weight polyethylene composite fiber and a preparation method thereof.
Background
Traditional macromolecular material body armor has light in weight and the good advantage of travelling comfort, but does not have fine radiation protection and electromagnetic shield function, can't solve the problem that electromagnetic radiation harms military personnel health in the war. Ultrahigh molecular weight polyethylene (UHMWPE), also known as high-strength high-modulus polyethylene fiber, is the fiber with the highest specific strength and specific modulus in the world at present, and is mainly used in military fields such as body armor, bulletproof helmets, bulletproof armor for military facilities and equipment, aerospace, and the like.
In order to improve the conductivity of the ultra-high molecular weight polyethylene fiber, a conductive material is usually added to the ultra-high molecular weight polyethylene, and a patent with a patent publication number of CN 102720066A discloses a preparation method of the ultra-high molecular weight polyethylene/polyaniline composite conductive fiber, which comprises the following specific implementation processes: placing the fiber in an aniline monomer for 0.5-2 h, taking out the fiber and uniformly extruding, wherein the mass ratio of the fiber to the aniline monomer is controlled to be 1: 1-1: 1.3; and (3) placing the fiber in a reaction solution, wherein the temperature of the reaction solution is 10-35 ℃, and reacting for 0.5-3 h to prepare the fiber with the uniform and continuous polyaniline conducting layer on the surface. The composite fiber with good conductivity is obtained by the technical scheme, can be made into textiles or fiber reinforced composite materials with antistatic, conductive and electromagnetic shielding functions, and is applied to the fields of individual protection, military industry, electronic and electric appliances, petrochemical industry, machinery and the like. The conductive polymer composite layer adopted by the scheme is polyaniline, and the conductivity of the polyaniline is low, so that the conductivity of the prepared conductive composite fiber is poor. In addition, due to the special chemical structure of the surface of the ultra-high molecular weight polyethylene, the adsorption effect on aniline is not ideal, and polymerization is not uniform, so that the surface treatment of the fiber surface is required, and the complexity of the process is increased.
Poly (3, 4-ethylenedioxythiophene) (PEDOT) is a good conductive polymer, has the characteristics of low cost, high flexibility, good environmental stability, high conductivity and the like, and in order to apply the PEDOT to fibers, the method generally adopted is that polyvinyl alcohol (PVA) is used as a spinning matrix, poly (3, 4-ethylenedioxythiophene) and polystyrene sulfonic acid (PEDOT: PSS) aqueous solution are used as a blending agent, dimethyl sulfoxide (DMSO) is used as a doping agent to improve the conductivity of the PEDOT: PSS, and the PVA/PEDOT: PSS/DMSO nanofibers are prepared through electrostatic spinning. However, if the polyvinyl alcohol is replaced by the ultra-high molecular weight polyethylene, and the ultra-high molecular weight polyethylene fiber with the PEDOT attached is prepared by the method, because the PEDOT: PSS related in the commonly adopted method is an aqueous dispersion and is used as a blending agent of the water-soluble PVA, the spinning solvent adopted by the ultra-high molecular weight polyethylene is an organic solvent, and the polyethylene is a hydrophobic material, and the blending of the PEDOT: PSS in the ultra-high molecular weight polyethylene fiber can damage the structure of the fiber and reduce the strength of the fiber.
Disclosure of Invention
The invention aims to provide a high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber and a preparation method thereof, which have the advantages of high conductivity effect and high strength.
The invention comprises a high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber, wherein the ultrahigh molecular weight polyethylene composite fiber is connected with a poly (3, 4-ethylenedioxythiophene) conductive layer through alkyl ferric sulfate, namely the poly (3, 4-ethylenedioxythiophene) is wrapped on the ultrahigh molecular weight polyethylene composite fiber.
The number of carbon atoms of the alkyl ferric sulfate is 5-18, and dodecyl ferric sulfate is more preferable.
The diameter of the ultra-high molecular weight polyethylene fiber is 2-4 microns.
The invention provides a preparation method of the high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber, which comprises the following steps,
the preparation method comprises the following steps of cleaning the ultrahigh molecular weight polyethylene fibers (preferably, the cleaning method is that the ultrahigh molecular weight polyethylene fibers are placed into ethanol (preferably pure ethanol) for ultrasonic cleaning to remove solid particles on the surfaces of the fibers), drying, then coating and wrapping alcohol solution of alkyl ferric sulfate on the ultrahigh molecular weight polyethylene fibers to remove redundant solution, then placing the ultrahigh molecular weight polyethylene fibers into steam containing 3, 4-ethylenedioxythiophene monomers, removing unreacted substances after gas phase polymerization reaction is finished, and drying to obtain the high-strength high-conductivity ultrahigh molecular weight polyethylene composite fibers.
Preferably, the solvent of the alcoholic solution of the alkyl ferric sulfate is an organic alcohol having 1 to 4 carbon atoms, and is preferably methanol, ethanol, n-propanol or n-butanol.
Preferably, the alcoholic solution of ferric alkyl sulfate is coated on the ultra-high molecular weight polyethylene fiber in a manner that the alcoholic solution of ferric alkyl sulfate is dropwise added on the ultra-high molecular weight polyethylene fiber.
Preferably, the excess solution is removed by scraping the excess solution with a spatula and then air drying.
Preferably, after removing the excess solution, the ultra-high molecular weight polyethylene fiber coated with the alkyl ferric sulfate is placed in a gas phase synthesis reaction chamber containing 3, 4-ethylenedioxythiophene monomer, the temperature is controlled to be 30-80 ℃, the humidity is controlled to be 40-60%, and the polymerization reaction is carried out for 30-120 min.
Preferably, the non-reacted materials are removed and dried by adding the materials after the polymerization reaction to a solvent (preferably an alcohol solution, more preferably a methanol or ethanol solution), soaking, then taking out, and drying in an oven at 80 ℃.
Compared with the prior art, the conductive polymer poly (3, 4-ethylenedioxythiophene) with better conductivity and more stability is synthesized by the technology, in addition, the alkyl ferric sulfate with the characteristics of the surfactant and the oxidant is innovatively adopted by the technology, the problem that the surface of the ultra-high molecular weight polyethylene fiber is not easy to coat is solved, so that the fiber can be directly coated and synthesized without any fiber surface treatment, and the fiber surface can not be damaged to damage the strength of the fiber surface due to the surface treatment.
Drawings
Fig. 1 is an SEM image of untreated ultra high molecular weight polyethylene fibers.
Fig. 2 is an SEM image of the high-strength high-conductivity ultra-high molecular weight polyethylene composite fiber of the present invention.
FIG. 3 is a Raman spectrum of the high-strength high-conductivity ultra-high molecular weight polyethylene composite fiber of the present invention.
Detailed Description
Example 1
A preparation method of high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber comprises the following steps,
the method comprises the steps of ultrasonically cleaning an ultra-high molecular weight polyethylene fiber bundle (40 fiber yarns with the diameter of 2-4 microns) in pure ethanol to remove solid particles on the surface of the fiber, drying the fiber after cleaning, fixing the fiber bundle on a glass support table after drying, dripping a methanol solution (with the mass concentration of 20 wt%) of lauryl ferric sulfate on the ultra-high molecular weight polyethylene fiber (with the total length of 1.2 meters) by using a dropper, and scraping by using a cylindrical scraper with the diameter of 2cm, wherein the redundant methanol solution of the lauryl ferric sulfate can be scraped away from the ultra-high molecular weight polyethylene fiber, so that the methanol solution of the lauryl ferric sulfate can be uniformly coated on the surface of the ultra-high molecular weight polyethylene fiber.
The coated fibers were air dried in a fume hood for 5 minutes.
The dried fiber coated with the lauryl ferric sulfate is placed in a gas phase synthesis reaction chamber with 3, 4-ethylenedioxythiophene monomer for synthesis, the temperature (50 ℃) and the humidity (50%) are set in advance in the reaction chamber, and the reaction time is 60 min.
And taking out the synthesized product, and soaking the product in an ethanol solvent for 5 minutes to remove the unreacted alkyl ferric sulfate and 3, 4-ethylenedioxythiophene monomer.
And (3) drying the soaked product in an oven at 80 ℃ for 60min to obtain the final product.
The sample is tested by adopting a scanning electron microscope, an electron microscope, a conductivity testing instrument, Raman and the like. The conductivity of the sample was about 2.03X 103S/cm。
The present invention compares the conductivity, breaking strength and elongation properties of the untreated ultrahigh molecular weight polyethylene fiber and the high strength and high conductivity ultrahigh molecular weight polyethylene composite fiber of the present invention, and obtains the data shown in table 1.
TABLE 1 comparison of ultra-high molecular weight polyethylene fibers with composite fibers
To illustrate the effect of the various reaction conditions of the present application on product performance, the present application examined the effect of mass concentration of ferric dodecyl sulfate in a methanol solution of ferric dodecyl sulfate and reaction time on product in a gas phase synthesis reaction to obtain data as shown in tables 1-2.
TABLE 2 Effect of reaction time on conductivity and Strength (oxidant concentration 20 wt%)
| Reaction time/min | conductivity/(S.cm)-1) | Breaking strength/(cN/dTex) | Elongation/(%) |
| 30 | 3.12×103 | 31.10 | 2.38 |
| 60 | 2.03×103 | 30.98 | 2.41 |
| 90 | 1.58×103 | 30.88 | 2.52 |
| 120 | 1.32×103 | 30.62 | 2.72 |
TABLE 3 Effect of oxidant concentration on conductivity and Strength (reaction time 60min)
| Concentration of oxidant/(wt%) | conductivity/(S.cm)-1) | Breaking strength/(cN/dTex) | Elongation/(%) |
| 5 | Is not conductive | 30.96 | 2.27 |
| 20 | 2.03×103 | 30.98 | 2.41 |
| 30 | 1.29×103 | 30.76 | 2.48 |
| 50 | 0.93×103 | 30.38 | 2.53 |
Conductivity measurement method: the method comprises the following steps of adopting an ultra-high molecular weight polyethylene sheet as a substrate, synthesizing a poly (3, 4-ethylenedioxythiophene) film on the ultra-high molecular weight polyethylene sheet substrate under the condition of synthesizing conductive composite fibers, testing the resistance of the film by using a four-point probe method and testing the thickness of the film by using an ellipsometer, wherein the electric conductivity of the final film can be calculated by a formula (1):
wherein R issqThe surface resistance of the conductive film is expressed in Ω/sq, and t is the thickness of the conductive film (the thickness of the conductive film is 20nm to 1 μm). Therefore, the conductivity of the poly (3, 4-ethylenedioxythiophene) coating in the composite conductive fiber can be approximately equal to that of the film prepared under the same conditions.
The breaking strength and elongation can be tested with a fiber tensile instrument: firstly, fixing the conductive composite fiber with the length of 1.2 meters on a traction end, and drawing and stretching the composite fiber under the operation of a computer program until program software obtains complete stretching data.
Comparative example 1
Compared with example 1, the other reaction steps were the same as in example 1 except that the methanol solution of iron dodecyl sulfate (mass concentration of 20 wt%) was replaced with the butanol solution of iron dodecyl sulfate (mass concentration of 20 wt%).
The properties of the product were measured to obtain the data shown in Table 4.
Table 4 performance test data for comparative example 1
| Substance(s) | conductivity/(S.cm)-1) | Breaking strength/(cN/dTex) | Elongation/(%) |
| Comparative example 1 | 2.13×103 | 31.02 | 2.42 |
Compared with other alcoholic solutions of ferric sulfate, the invention has obviously better conductivity than the comparative example 1.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, is limited to these examples; within the spirit of the present disclosure, features from the above embodiments or from different embodiments may also be combined, steps may be implemented in any order, and there are many other variations of different aspects of one or more embodiments in this application as described above, which are not provided in detail for the sake of brevity.
It is intended that the one or more embodiments of the present application embrace all such alternatives, modifications and variations as fall within the broad scope of the appended claims. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of one or more embodiments of the present disclosure are intended to be included within the scope of the present disclosure.
Claims (10)
1. The high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber is characterized in that the ultrahigh molecular weight polyethylene fiber is connected with a poly (3, 4-ethylenedioxythiophene) conductive layer through alkyl ferric sulfate.
2. The high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber according to claim 1, wherein the carbon number of the alkyl ferric sulfate is 5 to 18.
3. The high-strength high-conductivity ultrahigh molecular weight polyethylene composite fiber according to claim 2, wherein the alkyl ferric sulfate is dodecyl ferric sulfate.
4. The high strength high conductivity ultra high molecular weight polyethylene composite fiber according to claim 1, wherein the diameter of the ultra high molecular weight polyethylene fiber is 2 to 4 μm.
5. A method for preparing a high-strength high-conductivity ultra-high molecular weight polyethylene composite fiber according to any one of claims 1 to 4, comprising the steps of,
cleaning and drying the ultrahigh molecular weight polyethylene fibers, then coating and wrapping alcoholic solution of alkyl ferric sulfate on the ultrahigh molecular weight polyethylene fibers, removing redundant solution, then placing the ultrahigh molecular weight polyethylene fibers in steam containing 3, 4-ethylenedioxythiophene monomers, removing unreacted substances after the gas-phase polymerization reaction is finished, and drying to obtain the high-strength high-conductivity ultrahigh molecular weight polyethylene composite fibers.
6. The method according to claim 5, wherein the solvent of the alcoholic solution of iron alkyl sulfate is an organic alcohol having 1 to 4 carbon atoms.
7. The method of claim 5, wherein the alcoholic solution of ferric alkyl sulfate is coated and wrapped on the ultra-high molecular weight polyethylene fiber in a manner that the alcoholic solution of ferric alkyl sulfate is dropped on the ultra-high molecular weight polyethylene fiber.
8. The method according to claim 5, wherein the excess solution is removed by scraping the excess solution with a spatula and then air-drying.
9. The preparation method as set forth in any one of claims 5 to 8, wherein after removing the surplus solution, the ultra high molecular weight polyethylene fiber coated with the ferric alkylsulfate is placed in a gas phase synthesis reaction chamber containing 3, 4-ethylenedioxythiophene monomer, and polymerization is carried out while controlling the temperature at 30 to 80 ℃ and the humidity at 40 to 60%.
10. The preparation process as claimed in claim 5, wherein the non-reacted substances are removed and dried by adding the substances after completion of the polymerization reaction to a solution of methanol or ethanol, soaking, taking out, and drying in an oven at 80 ℃.
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| CN114575009A (en) * | 2022-01-28 | 2022-06-03 | 江苏九九久科技有限公司 | Heat-resistant ultra-high molecular weight polyethylene fiber product and preparation method thereof |
| CN114575009B (en) * | 2022-01-28 | 2023-06-06 | 九州星际科技有限公司 | Heat-resistant ultra-high molecular weight polyethylene fiber product and preparation method thereof |
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