CN108315833B - Preparation method of graphene ultra-high molecular weight polyethylene composite fiber - Google Patents
Preparation method of graphene ultra-high molecular weight polyethylene composite fiber Download PDFInfo
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- CN108315833B CN108315833B CN201810036884.4A CN201810036884A CN108315833B CN 108315833 B CN108315833 B CN 108315833B CN 201810036884 A CN201810036884 A CN 201810036884A CN 108315833 B CN108315833 B CN 108315833B
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- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- 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
- D01F1/10—Other agents for modifying properties
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Abstract
The invention provides a preparation method of a graphene ultra-high molecular weight polyethylene composite fiber, which comprises the following steps: s1: dispersing the ultra-high molecular weight polyethylene resin and the filler in a solvent by adopting a blending method to form uniform resin dispersion liquid; s2: adding graphene powder into a dispersing agent, heating to a certain temperature, adding an emulsifying agent, and performing emulsification treatment to obtain a graphene dispersion liquid; s3: adding the graphene dispersion liquid into the resin dispersion liquid, stirring and heating to obtain a spinning solution; s4: and spinning, precursor standing and hot drafting are carried out on the spinning solution to obtain the graphene ultrahigh molecular weight polyethylene composite fiber. According to the invention, the filler and the graphene are added into the ultra-high molecular weight polyethylene fiber to enhance the strength of the ultra-high molecular weight polyethylene fiber, the final strength reaches 30-45 cN/dtex, and meanwhile, the composite fiber has excellent ultraviolet resistance, cutting resistance and other properties.
Description
Technical Field
The invention relates to a preparation method of a graphene ultra-high molecular weight polyethylene composite fiber, and belongs to the technical field of fiber materials.
Background
The ultra-high molecular weight polyethylene is thermoplastic engineering plastic with excellent comprehensive performance, and plays a very important role in the fields of modern war, aviation, aerospace, sea defense equipment and the like. The ultra-high molecular weight polyethylene has the advantages of flame retardancy, chemical corrosion resistance, wear resistance, excellent electrical insulation, higher mechanical strength and the like, is widely applied to various fields, and is engineering plastic with the largest yield in the world.
Although ultra-high molecular weight polyethylene has many excellent properties, it is also deficient: because the molecular chain is very long, the melt viscosity is as high as 108 Pa.s when the chain is easy to be entangled and melted; the critical shearing speed is low, the melt is easy to break, and the forming processing is difficult; in addition, the method has the defects of low surface hardness, poor wear resistance of wear-resistant particles, low thermal deformation and the like. In order to make it possible to use it in certain fields where the conditions are critical, the properties of the ultrahigh molecular weight polyethylene have to be modified appropriately. The purpose of the modification is: on the basis of not influencing the performance of UHMW-PE, the melt fluidity is improved, or the defects of the self performance of the ultra-high molecular weight polyethylene (such as melt fluidity, heat resistance, surface hardness and the like) are compositely modified.
The patent application No. 201410474250.9 describes that the high cut-resistant ultra-high molecular weight polyethylene fiber is composed of ultra-high molecular weight polyethylene and inorganic ultra-fine powder with nanocrystalline structure. The inorganic superfine powder is one or the combination of several of oxides, carbides and nitrides of aluminum, titanium, silicon and boron zirconium, the tensile strength of the cutting-resistant ultra-high molecular weight polyethylene fiber is 19-21cN/dtex, the tensile modulus is 750-850cN/dtex, and the cutting-resistant ultra-high molecular weight polyethylene fiber can be used as a cutting-proof glove.
The patent application No. 201410814002.4 discloses that the composite material of ultra-high molecular weight polyethylene is prepared from ultra-high molecular weight polyethylene, lubricant, filler, reinforcing fiber and nano inorganic filler. Wherein the filler is one or more of glass beads, ceramic beads, aluminum oxide, silicon carbide and boron carbide. The obtained composite material has excellent performances of impact resistance, abrasion resistance, self-lubrication, chemical corrosion resistance and the like.
In order to further improve the strength, wear resistance and heat resistance of the ultrahigh molecular weight polyethylene fiber, the inorganic filler and the graphene powder are added into the ultrahigh molecular weight polyethylene fiber, so that the functional composite ultrahigh molecular weight polyethylene fiber with higher strength is finally obtained.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a graphene ultra-high molecular weight polyethylene composite fiber.
The invention is realized by the following technical scheme:
the invention provides a preparation method of a graphene ultra-high molecular weight polyethylene composite fiber, which comprises the following steps:
s1: dispersing the ultra-high molecular weight polyethylene resin and the filler in a solvent by adopting a blending method to form uniform resin dispersion liquid;
s2: adding the graphene dispersion liquid into the resin dispersion liquid, stirring and heating to obtain a spinning solution;
s3: and spinning, precursor standing and hot drafting are carried out on the spinning solution to obtain the graphene ultrahigh molecular weight polyethylene composite fiber.
Preferably, the ultra-high molecular weight polyethylene has a weight average molecular weight of 4.0 × 106～6.0×106。
Preferably, the amount of the filler is 5-20% of the weight of the ultrahigh molecular weight polyethylene resin.
Preferably, the graphene dispersion liquid is obtained by adding graphene powder into a dispersing agent, heating, adding an emulsifying agent, and performing emulsification treatment;
preferably, the filler is at least one selected from the group consisting of silicon carbide, diamond, glass beads, ceramic fiber, glass fiber, basalt fiber, and metal fiber.
Preferably, in the filler, the average grain diameter of the silicon carbide, the diamond and the glass bead is 100-400 nm.
Preferably, in the filler, the diameters of the ceramic fiber, the glass fiber, the basalt fiber and the metal fiber are 1-100 um, and the length-diameter ratio is 8-20.
Preferably, the weight ratio of the ultra-high molecular weight polyethylene resin to the solvent is (1-8) to (10-15).
Preferably, the solvent is selected from one or more of tetrahydronaphthalene, decalin, n-heptane, n-hexane, cyclohexane, paraffin oil, white oil, kerosene, vegetable oil and animal oil.
Preferably, the amount of the graphene is 0.5-10% of the weight of the ultra-high molecular weight polyethylene resin.
Preferably, the thickness of the graphene is 0.4-5 nm, the sheet diameter is 0.01-6 mu m, and the specific surface area is 500-1000 m2(ii)/g; the graphene is selected from one or more of coupling agent modified graphene oxide, cationic surfactant modified graphene oxide, halogenated hydrocarbon modified graphene oxide, few-layer graphene prepared by a ball milling method and few-layer graphene prepared by an electrochemical stripping method.
Preferably, the high-speed shearing and blending speed is 1500-2800 r/min, and the stirring time is 4-6 h; the spinning temperature is 110-180 ℃, and the spinning method is a dry spinning method or a wet spinning method.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the filler and the graphene are added into the ultra-high molecular weight polyethylene fiber to enhance the strength of the ultra-high molecular weight polyethylene fiber, the final strength reaches 30-45 cN/dtex, and meanwhile, the composite fiber has excellent ultraviolet resistance, cutting resistance and other properties;
2. according to the invention, graphene is modified, so that the graphene can be well dissolved in an organic solvent, the method replaces a complex ball milling and blending process of graphene and ultra-high molecular weight polyethylene, and the modified graphene can be easily compounded with the ultra-high molecular weight polyethylene, so that the content of the graphene in finished fibers is ensured, and the performance of the finished fibers is ensured;
3. according to the invention, the graphene is compounded with the ultra-high molecular weight polyethylene by utilizing the excellent thermal shock resistance function of the graphene to obtain the composite fiber with excellent thermal shock resistance, so that the thermal resistance of the ultra-high molecular weight polyethylene fiber is greatly improved, and the application range of the composite fiber is expanded;
4. the graphene ultra-high molecular weight polyethylene composite fiber can be used for ropes, cables, super oil tankers, ocean operation platforms, body armor, parachutes, ship armor protection plates, radar protection outer covers and the like.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment provides a preparation method of a graphene ultra-high molecular weight polyethylene composite fiber, which specifically comprises the following steps:
s1: dispersing 100kg of ultra-high molecular weight polyethylene resin and 5kg of silicon carbide in white oil by adopting a high-speed shearing and blending method, controlling the rotating speed of the high-speed shearing and blending to be 1500-2800 r/min, and forming uniform resin dispersion liquid under the heating condition;
s2: adding a graphene dispersion liquid containing 0.5kg of graphene powder into the resin dispersion liquid, stirring and heating to obtain a spinning solution;
s3: and (3) carrying out dry spinning on the spinning solution at 110 ℃, and then carrying out protofilament standing and hot drafting to obtain the graphene ultrahigh molecular weight polyethylene composite fiber.
Example 2
The embodiment provides a preparation method of a graphene ultra-high molecular weight polyethylene composite fiber, which specifically comprises the following steps:
s1: dispersing 100kg of ultra-high molecular weight polyethylene resin and 20kg of diamond powder in tetralin by a high-speed shearing and blending method, controlling the rotating speed of the high-speed shearing and blending to be 1500-2800 r/min, and forming uniform resin dispersion liquid under the heating condition;
s2: adding a graphene dispersion liquid containing 10kg of graphene powder into the resin dispersion liquid, stirring and heating to obtain a spinning solution;
s3: and (3) carrying out dry spinning on the spinning solution at 110 ℃, and then carrying out protofilament standing and hot drafting to obtain the graphene ultrahigh molecular weight polyethylene composite fiber.
Example 3
The embodiment provides a preparation method of a graphene ultra-high molecular weight polyethylene composite fiber, which specifically comprises the following steps:
s1: dispersing 100kg of ultrahigh molecular weight polyethylene resin and 10kg of ceramic fiber in decahydronaphthalene by a high-speed shearing and blending method, controlling the rotating speed of the high-speed shearing and blending to be 1500-2800 r/min, and forming uniform resin dispersion liquid under the heating condition;
s2: adding a graphene dispersion liquid containing 5kg of graphene powder into the resin dispersion liquid, stirring and heating to obtain a spinning solution;
s3: and (3) carrying out dry spinning on the spinning solution at 110 ℃, and then carrying out protofilament standing and hot drafting to obtain the graphene ultrahigh molecular weight polyethylene composite fiber.
Example 4
The embodiment provides a preparation method of a graphene ultra-high molecular weight polyethylene composite fiber, which specifically comprises the following steps:
s1: dispersing 100kg of ultrahigh molecular weight polyethylene resin and 15kg of glass fiber in n-heptane by adopting a high-speed shearing and blending method, controlling the rotating speed of the high-speed shearing and blending to be 1500-2800 r/min, and forming uniform resin dispersion liquid under the heating condition;
s2: adding a graphene dispersion liquid containing 1kg of graphene powder into the resin dispersion liquid, stirring and heating to obtain a spinning solution;
s3: and (3) carrying out dry spinning on the spinning solution at 110 ℃, and then carrying out protofilament standing and hot drafting to obtain the graphene ultrahigh molecular weight polyethylene composite fiber.
Comparative example 1
The preparation method of this comparative example differs from example 1 only in that no filler is added to the resin dispersion.
Comparative example 2
The preparation method of this comparative example differs from example 1 only in that no graphene dispersion is added.
Comparative example 3
The preparation method of this comparative example differs from example 1 only in that no filler is added to the resin dispersion, nor is the graphene dispersion added.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (7)
1. A preparation method of graphene ultra-high molecular weight polyethylene composite fibers is characterized by comprising the following steps:
s1: dispersing the ultra-high molecular weight polyethylene resin and the filler in a solvent by adopting a blending method to form uniform resin dispersion liquid;
s2: adding the graphene dispersion liquid into the resin dispersion liquid, stirring and heating to obtain a spinning solution; the graphene dispersion liquid is prepared by adding graphene powder into a dispersing agent, heating, adding an emulsifying agent, and emulsifyingObtained after treatment; the thickness of the graphene is 0.4-5 nm, the sheet diameter is 0.01-6 mu m, and the specific surface area is 500-1000 m2(ii)/g; the amount of the graphene is 0.5-10% of the weight of the ultra-high molecular weight polyethylene resin; the amount of the filler is 5-20% of the weight of the ultrahigh molecular weight polyethylene resin; the graphene is selected from one or more of cationic surfactant modified graphene oxide, halogenated hydrocarbon modified graphene oxide, few-layer graphene prepared by a ball milling method and few-layer graphene prepared by an electrochemical stripping method; the filler is selected from at least one of silicon carbide, diamond, glass beads, ceramic fiber, glass fiber, basalt fiber and metal fiber;
s3: and spinning, precursor standing and hot drafting are carried out on the spinning solution to obtain the graphene ultra-high molecular weight polyethylene composite fiber, and the final strength reaches 30-45 cN/dtex.
2. The method of preparing graphene ultra-high molecular weight polyethylene composite fibers according to claim 1, wherein the ultra-high molecular weight polyethylene has a weight average molecular weight of 4.0 × 106～6.0×106。
3. The method for preparing the graphene ultra-high molecular weight polyethylene composite fiber according to claim 1, wherein the particle size of the silicon carbide, the diamond and the glass beads is 100-400 nm.
4. The preparation method of the graphene ultra-high molecular weight polyethylene composite fiber according to claim 1, wherein the diameters of the ceramic fiber, the glass fiber, the basalt fiber and the metal fiber are 1-100 um, and the length-diameter ratio is 8-20.
5. The preparation method of the graphene ultra-high molecular weight polyethylene composite fiber according to claim 1, wherein the weight ratio of the ultra-high molecular weight polyethylene resin to the solvent is (1-8): (10-15).
6. The method for preparing the graphene ultra-high molecular weight polyethylene composite fiber according to claim 1 or 5, wherein the solvent is selected from one or more of tetrahydronaphthalene, decahydronaphthalene, n-heptane, n-hexane, cyclohexane, paraffin oil, white oil, kerosene, vegetable oil, and animal oil.
7. The preparation method of the graphene ultra-high molecular weight polyethylene composite fiber according to claim 1, wherein the blending mode is high-speed shearing, the blending speed is 1500-2800 r/min, and the stirring time is 4-6 h; the spinning temperature is 110-180 ℃, and the spinning method is a dry spinning method or a wet spinning method; the dispersant is selected from one or more of SDS, SDBS, PSS, PVP, Span-60 and Span-80.
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| CN109440220A (en) * | 2018-09-11 | 2019-03-08 | 江苏恒辉安防股份有限公司 | Cut resistant fibers and preparation method thereof |
| CN109468699A (en) * | 2018-09-11 | 2019-03-15 | 江苏恒辉安防股份有限公司 | Compound ultra high molecular weight polyethylene fiber and preparation method thereof |
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| CN102618955B (en) * | 2012-03-22 | 2013-12-04 | 中国人民解放军总后勤部军需装备研究所 | Preparation method and application of ultrahigh molecular weight polyethylene/graphene composite fiber |
| CN104762683A (en) * | 2015-04-09 | 2015-07-08 | 江苏九九久科技股份有限公司 | Graphene composite modified high-strength polyethylene fiber and preparation method thereof |
| CN105483848A (en) * | 2016-01-21 | 2016-04-13 | 青岛大学 | Preparation method of graphene ultra-high molecular weight polyethylene hybrid fiber |
| CN106222780B (en) * | 2016-06-23 | 2018-11-09 | 常州第六元素材料科技股份有限公司 | A kind of graphene/UHMWPE composite fibres and its preparation method and application |
| CN106149085B (en) * | 2016-06-30 | 2018-10-26 | 常州第六元素材料科技股份有限公司 | A kind of cut resistant superhigh molecular weight polyethylene fibers and its preparation process |
| CN106222781B (en) * | 2016-07-25 | 2018-08-14 | 江苏锵尼玛新材料股份有限公司 | UHMWPE compositions and its high abrasion of preparation, high cut resistant fibers |
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