# US 2020/0399787 A1 · Graphene composite ultra-high molecular weight polyethylene fiber and preparation method thereof > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2020/0399787 A1 - Document ID: US20200399787A1 - Status: Published application - Kind: A1 - Application number: 17/010,469 - Filed: 2020-09-02 - Published: 2020-12-24 - Earliest claimed: 2018-01-08 - Assignees: Jiangsu Hanvo Safety Product Co., Ltd - Applicants: Jiangsu Hanvo Safety Product Co., Ltd - Inventors: Chonghua OU; Shendong REN; Ming ZHANG; Xianhua WANG - Web page: https://patentgrep.com/patent/US20200399787A1 ## CPC - D01D 1/02: Preparation of spinning solutions - D01D 5/088: Cooling filaments, threads or the like, leaving the spinnerettes - D01F 1/10: Other agents for modifying properties - D01F 6/04: from polyolefins - D01F 8/06: with at least one polyolefin as constituent - D01F 9/08: of inorganic material (working or processing of metal wire B21F; from softened glass, minerals or slags C03B37/00) - D10B 2401/063: high strength - D01D: MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS - D01F: CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS - D10B: INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES ## Abstract The present invention provides a composite ultra-high molecular weight polyethylene fiber and a preparation method thereof, wherein the method comprises mixing glass fiber, graphene slurry, UHMWPE powder and white oil, and then swelling to a molten state, then cooling into a gel-spun, and finally making the fiber from the gel-spun. The method of the present disclosure not only can solve the problem that the glass fiber has poor dispersibility in the case of high viscoelasticity of the ultra-high molecular weight polyethylene, but also can improve the cut resistance of the ultra-high molecular weight polyethylene fiber on the basis of ensuring the flexibility of the yarn. ## Claims ### Claim 1 A method for preparing a composite ultra-high molecular weight polyethylene fiber, comprising: preparing a glass fiber premix: dispersing glass fiber in a first white oil to obtain the glass fiber premix containing 5 wt % to 30 wt % of glass fiber; preparing a graphene slurry premix: grinding graphene slurry, filtering, then adding the filter residue to a second white oil, and then adding a first UHMWPE to the second white oil containing the graphene filter residue, heating the premix to a first temperature, raising the first temperature to a second temperature after the same was not bubbled, and maintaining the second temperature; preparing a spinning mixture: mixing the glass fiber premix, the graphene slurry premix, a second UHMWPE, an antioxidant, and a third white oil to obtain the spinning mixture; swelling and mixing the spinning mixture to form a molten state; extruding the spinning mixture which is in the molten state; cooling to form a gel-spun; and obtaining the composite ultra-high molecular weight polyethylene fiber from the gel-spun. ### Claim 2 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein the glass fiber premix contains 10 wt % to 25 wt % of glass fiber. ### Claim 3 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein the dispersing method for dispersing the glass fiber in the first white oil comprises: first pouring the glass fiber into the first white oil, premixing, and then stirring at a high speed with an emulsifier to form a homogeneous slurry; the emulsifier has a stirring speed of 3000 rpm to 10000 rpm; and a stirring time of 5 min to 60 min. ### Claim 4 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein the glass fiber is modified with a coupling agent, and then used to prepare the glass fiber premix; the specific treatment method for modifying the glass fiber with the coupling agent is as follows: dissolving the coupling agent in anhydrous ethanol, and then the glass fiber is added to mix homogeneously, impregnating, drying, grinding, and filtering by 100 mesh; wherein, the amount of the coupling agent is 0.1% to 3% of the total mass of the glass fiber, and the impregnation time of the glass fiber in the coupling agent ethanol solution is 10 min to 5 h, and the drying temperature is 50° C. to 180° C., and the drying time is 1 h to 6 h. ### Claim 5 (depends on 4) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 4, wherein the coupling agent is a silane coupling agent, and the silane coupling agent is one or a mixture of two or more of A-150, A-151, A-171, KH-550, KH-560, KH-570, KH-580, KH-590, KH-902, or KH-792. ### Claim 6 (depends on 4) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 4, the coupling agent is added in an amount of 0.2% to 2% of the total mass of the glass fiber, the impregnation time of the glass fiber in the coupling agent ethanol solution is 30 min to 2 h, the drying temperature is 80° C. to 130° C., and the drying time is 2 h to 3 h. ### Claim 7 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein the graphene slurry is a mixture of graphene-anhydrous ethanol, the graphene slurry has a graphene concentration of 1 wt % to 8 wt %, and the graphene is a single-layer or multi-layer structure graphene powder. ### Claim 8 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein the graphene slurry has a graphene concentration of 5 wt %. ### Claim 9 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein the single-layer or multi-layer structure graphene has a sheet diameter of 0.5 μm to 5 μm and a thickness of 0.5 nm to 30 nm; and the single-layer or multi-layer structure graphene has a specific surface area of 200 m2/g to 1000 m2/g. ### Claim 10 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein in the method for preparing the graphene slurry premix, the grinding uses a sand mill to grind the graphene-anhydrous ethanol mixture for 3 h to 4 h to a graphene particle size of D99<7 μm, wherein the grinding uses grinding medium of zirconia bead having a particle diameter of 0.6 mm to 0.8 mm, the sand mill has a rotation speed of 1500 rpm to 2800 rpm; the first UHMWPE is added to the second white oil contained the graphene filter residue under a condition of high-speed stirring, the high-speed stirring has a stirring speed of 1800 rpm to 2000 rpm; and the high-speed stirring has a stirring time of 5 min to 20 min; the first temperature is 80° C. to 90° C.; the second temperature is 135° C. to 170° C.; after heating to the second temperature, the second temperature is maintained for 2.5 h to 4.5 h. ### Claim 11 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein in the method for preparing the graphene slurry premix, the first UHMWPE has a viscosity average molecular weight of (2-6)×106 g/mol, the graphene slurry premix has a graphene concentration of 1 wt % to 8 wt %, and the first UHMWPE has a mass fraction of 0.1 wt % to 0.3 wt %. ### Claim 12 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein in the method for preparing the graphene slurry premix, the graphene slurry premix has a graphene concentration of 5 wt % and the first UHMWPE has a mass fraction of 0.2 wt %. ### Claim 13 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, the second UHMWPE has a viscosity average molecular weight of (2-6)×106 g/mol and the antioxidant is one or a combination of two or more of antioxidant 1010, antioxidant 1076, antioxidant CA, antioxidant 164, antioxidant DNP, antioxidant DLTP or antioxidant TNP. ### Claim 14 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein in the method for preparing the spinning mixture, the glass fiber premix and the graphene slurry premix are first mixed at a high speed in an emulsifier, then added to a swelling kettle containing the second UHMWPE and the third white oil, and the antioxidant is further added to form the spinning mixture; wherein the second UHMWPE:the third white oil has a mass ratio of 6:94, and the glass fiber in the glass fiber premix:the graphene in the graphene slurry premix:the antioxidant has a mass ratio of (0.2-10):(0.01-3):(0.01-1). ### Claim 15 (depends on 14) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 14, wherein the glass fiber in the glass fiber premix:the graphene in the graphene slurry premix:the antioxidant has a mass ratio of (1-6):(0.05):(0.1-0.5). ### Claim 16 (depends on 1) The method for preparing the composite ultra-high molecular weight polyethylene fiber according to claim 1, wherein the swelling and mixing step is carried out by heating to 100° C. to 140° C. in a swelling kettle and holding for 1 h to 3 h.