CN105970331A - Graphene-alumina composite modified UHMWPE (Ultrahigh Molecular Weight Polyethylene) fiber and preparation method thereof - Google Patents
Graphene-alumina composite modified UHMWPE (Ultrahigh Molecular Weight Polyethylene) fiber and preparation method thereof Download PDFInfo
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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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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- 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
- D01D5/06—Wet spinning methods
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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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/00—Applications
- C08L2203/12—Applications used for fibers
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/068—Ultra high molecular weight polyethylene
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Abstract
The invention discloses a graphene-alumina composite modified UHMWPE (Ultrahigh Molecular Weight Polyethylene) fiber. The graphene-alumina composite modified UHMWPE fiber is characterized by further comprising 2 to 5 parts of graphene, and 0.05 to 2 parts of alumina according to 100 parts of UHMWPE in parts by weight in the composite modified UHMWPE fiber. The mechanical strength of the UHMWPE composite fiber modified by the graphene and alumina provided by the invention is obviously improved, the tensile strength of the UHMWPE composite fiber modified by the graphene and alumina can reach 32cN/dtex, and the tensile modulus of the UHMWPE composite fiber modified by the graphene and alumina can reach 1600cN/dtex. The modified UHMWPE composite fiber prepared by the invention can be used as a high-performance cutting resistant material to prepare anti-cutting gloves, and the anti-cutting level can reach the level 5 of international certification.
Description
Technical field
The present invention relates to a kind of superhigh molecular weight polyethylene fibers being added with Graphene and aluminium oxide, belong to polymeric material field.
Background technology
As one of big high-performance fiber in the world today three, ultra-high molecular weight polyethylene (UHMWPE) fiber has specific strength and the specific modulus of excellence, there is in terms of light composite material great advantage, play very important effect in modernized war and the field such as Aeronautics and Astronautics, marine site defence equipment.The end of the seventies in last century, DSM N. V. of Holland developed UHMWPE gel spinning technology the earliest so that the intensity of UHMWPE and modulus obtain revolutionary progress, and have applied for first part of patent preparing UHMWPE fiber about gel spinning.The Toyobo company of the Honeywell company of the U.S. and Japan developed the technology of preparing commercially producing high-performance UHMWPE fiber successively later, and had applied for substantial amounts of patent.
Anti-cutting, anti-puncture articles for use (such as various military applications, clothing, trick set etc.) are big applications of high-performance UHMWPE fiber, enjoy the concern of domestic and international industry always.In order to pursue optimal anti-puncture effect, research both at home and abroad has put into great effort to this, is concentrated mainly on two aspects: on the one hand by process modification or compound by the way of promote the anti-cutting performance of fiber itself, be on the other hand the weaving manner of improvement fiber.Patent CN 102037169A (Toyobo) discloses the radical polymerization being caused lower molecular weight polyethylene by cross-linking agent, forms network structure thus reaches the purpose strengthened.Patent CN 18092292A (Dupont) discloses the composite fibre of a kind of high-strength aromatic polymer and band cladodification polyethylene blend.Patent CN 102277669A (DSM) discloses a kind of rotation spray spinning technique, and by UHMWPE and the staple fibre such as composite spinning such as glass fibre, mineral rock fibre or metallic fiber with certain draw ratio, anti-cutting performance is obviously improved.But the production technology that said method is used for preparing UHMWPE composite fibre is extremely complex, and production cost increases.Additionally, cause end article body-sensing to be deteriorated because adding the hard reinforcing material such as inorganic metal, glass fibre, wearing comfort degree declines, and the most hyperbaric filler does not meets the light-weighted requirement of weaponry yet.Accordingly, it is desirable to provide a kind of new reinforcing material solves the purpose of the problems referred to above.
Graphene is a kind of by monolayer sp2The cellular two-dimensional structure of hexagonal lattice that hydbridized carbon atoms is constituted, has the most excellent mechanical strength (intensity: 130GPa, Young's modulus: 1TPa), is widely used in the activeness and quietness of composite.Additionally, the material that Graphene is the lightest, specific surface area is up to 2630m2/ g, meets the light-weighted design requirement of composite.Graphene particle diameter is little, the model ylid bloom action power that sheet interlayer is the strongest owing to conjugated structure is formed so that lamella easily stacks, it is difficult to dispersion.Traditional melt blending complex method uses the mode that graphene powder directly feeds intake, the polymer wrapped that the height being melted due to Graphene is viscous, system cannot fully spread, thus effective dispersion of Graphene cannot be ensured so that the excellent properties of Graphene fails to be not fully exerted.Therefore, whether Graphene can disperse mixing in UHMWPE fiber, becomes the key issue of restriction graphene composite material development.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of have the Graphene of high belt cutting-resisting property, the UHMWPE fiber of alumina composite modification；
It is a further object of the present invention to provide the preparation method of the UHMWPE fiber of above-mentioned Graphene, alumina composite modification.
The purpose of the present invention implements by the following technical programs:
The UHMWPE fiber that a kind of Graphene, alumina composite are modified, in described composite modified UHMWPE fiber, is 100 parts of meters according to the weight portion of contained UHMWPE, also includes the Graphene of 2-5 part, the aluminium oxide of 0.05-2 part.
Preferably, the UHMWPE fiber that above-mentioned Graphene, alumina composite are modified, by weight, UHMWP100 part, Graphene 3.5 parts, the aluminium oxide of 0.8 part.
Preferably, the molecular weight of described UHMWPE powder is 340-370 ten thousand.
Preferably, size d50 of described aluminium oxide is 0.1～0.8um, preferably 0.3～0.4um.
Preferably, described Graphene is the graphene powder of single or multiple lift structure, and its sheet footpath is 0.5～5um, and thickness is 0.5～30nm, and specific surface area is 200～1000m2/g；Preferably, described graphene film footpath is 3-4um, and thickness is 3.2～4nm, and specific surface area is 300～600m2/g。
The preparation method of the UHMWPE fiber that above-mentioned Graphene, alumina composite are modified, it is characterised in that: comprise the steps:
1) Graphene powder, alumina powder, UHMWPE sphere of powder mill premix
Graphene powder, alumina powder, UHMWPE powder put into ball grinder, and weigh stainless steel ball by ball material mass ratio 10:1, then add and seal dissolved with after the white oil of dispersant, ball mill grinds 12h, drum's speed of rotation is 600-1000rpm, obtains Graphene/aluminium oxide/UHMWPE composite granule；
3) preparation of liquid is spun in advance
Graphene/aluminium oxide/UHMWPE composite granule after ball milling is completely dissolved in white oil, is slowly heated to while stirring form mixed uniformly spinning solution；
3) spinning, extraction, drawing-off
To step 2) spinning solution that obtains uses gel spinning method to carry out spinning, then through solvent extraction, drawing-off, obtains Graphene/UHMWPE composite fibre.
Preferably, described step 1) in, described dispersant uses described dispersant to use one or more the mixing in PSS, SDBS, SDS, BYK dispersant or AFCONA dispersant.
Preferably, dispersant: the mass ratio of UHMWPE powder is (0.05-0.15): 100, preferably 0.1:100.
Preferably, described step 1) in, described steel ball uses the mixing steel ball of a diameter of 5mm, 12mm, 15mm 3:1:1 by volume.
Preferably, described step 1) in, described white oil addition is the 1/20 of UHMWPE opaque amount；Described step 2) in, white oil consumption: the mass ratio of UHMWPE powder is 9:2.
The invention has the beneficial effects as follows:
The present invention provides the modified UHMWPE composite fibre mechanical strength through Graphene and aluminium oxide to promote substantially, and hot strength is up to 32cN/dtex, and stretch modulus is up to 1600cN/dtex.Modified UHMWPE composite fibre prepared by the present invention can be used as high-performance cut resistant material and prepares anti-cutting gloves, and anti-cutting grade is up to International Certification 5 grades.Why the present invention can reach the effect above, is based primarily upon following advantage:
1) being combined with ball milling feature by the research of the mechanics of materials, utilize the distribution of ball milling steel ball, by Graphene powder, aluminium oxide, dispersant, UHMWPE carries out strict ball-milling treatment can be finely ground by material, fully mixes.Add after a small amount of white oil can moistening UHMWPE powder surface, by dispersant and the common effect of aluminium oxide, make Graphene and aluminium oxide uniform adsorption at each UHMWPE particle surface.
2) after ball milling, graphene powder and aluminium oxide particles uniformly wrap up at UHMWPE particle surface, during later stage rising temperature for dissolving, high thermal conductivity coefficient due to Graphene, system heat transfer is fast, being heated evenly, UHMWPE powder is progressively dissolved into and forms uniform spinning liquid without the macromolecular chain returned and the graphene film being wrapped in its outer layer.
3) complex method that the present invention uses does not changes traditional gel spinning technique, and combination process is simple, and production cost aspect only increases the cost of limited Graphene, and cost performance is high.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred embodiment described herein is merely to illustrate and explains the present invention, is not intended to limit the present invention.
Embodiment 1:
The technological process of modified UHMWPE composite fibre sees Fig. 1, comprises the steps:
1) being dissolved in 5 parts of white oils by 0.1 part of dispersant, (monolayer, sheet footpath is 3um, and thickness is 3.4nm, and specific surface area is 800m with 3.5 parts of Graphene powder2/ g), 0.8 part of alumina powder (size d50 is 0.1～0.8um, preferably 0.3～0.4um), UHMWPE powder (molecular weight is 340-370 ten thousand) obtain puddling uniform powder body after (using the mixing steel ball of a diameter of 5mm, 12mm, 15mm 3:1:1 by volume) in ball mill and grinding 12h；
2) powder body after ball milling is completely dissolved in 450 parts of white oils, is slowly heated to while stirring form homogeneous mixture solotion；
3) the UHMWPE/ Graphene mixed solution fully dissolved uses gel spinning method to carry out spinning, and spinning temperature controls at 240 DEG C, and spinning, through solvent extraction, drawing-off, obtains highly directional Graphene/UHMWPE composite fibre.
Embodiment 2:
The technological process of modified UHMWPE composite fibre sees Fig. 1, comprises the steps:
1) 0.05 part of dispersant is dissolved in 5 parts of white oils, then (monolayer, sheet footpath is 4um, and thickness is 4nm, and specific surface area is 700m with 2 parts of Graphene powder2/ g), 2 parts of alumina powders (size d50 is 0.1～0.8um, preferably 0.3～0.4um), 100 parts of UHMWPE powder (molecular weight is 340-370 ten thousand) obtain puddling uniform powder body after grinding 12h in ball mill (using the mixing steel ball of a diameter of 5mm, 12mm, 15mm 3:1:1 by volume)；
2) powder body after ball milling is completely dissolved in 450 parts of white oils, is slowly heated to while stirring form homogeneous mixture solotion；
3) the UHMWPE/ Graphene mixed solution fully dissolved uses gel spinning method to carry out spinning, and spinning temperature controls at 240 DEG C, and spinning, through solvent extraction, drawing-off, obtains highly directional Graphene/UHMWPE composite fibre.
Embodiment 3:
1) technological process of modified UHMWPE composite fibre sees Fig. 1, comprises the steps:
0.15 part of dispersant is dissolved in 5 parts of white oils, then (10 layers, sheet footpath is 5um, and thickness is 30nm, and specific surface area is 1000m with 5 parts of Graphenes2/ g), 0.05 part of alumina powder (size d50 is 0.1～0.8um, preferably 0.3～0.4um), 100 parts of UHMWPE powder (molecular weight is 340-370 ten thousand) obtain puddling uniform powder body after grinding 12h in ball mill (using the mixing steel ball of a diameter of 5mm, 12mm, 15mm 3:1:1 by volume)；
2) powder body after ball milling is completely dissolved in 450 parts of white oils, is slowly heated to while stirring form homogeneous mixture solotion；
3) the UHMWPE/ Graphene mixed solution fully dissolved uses gel spinning method to carry out spinning, and spinning temperature controls at 240 DEG C, and spinning, through solvent extraction, drawing-off, obtains highly directional Graphene/UHMWPE composite fibre.
Embodiment 4:
The technological process of modified UHMWPE composite fibre sees Fig. 1, comprises the steps:
1) 0.1 part of dispersant is dissolved in 5 parts of white oils, then (2 layers, sheet footpath is 0.5um, and thickness is 0.5nm, and specific surface area is 200m with 3 parts of Graphene powder2/ g), 1.5 parts of alumina powders (size d50 is 0.1～0.8um, preferably 0.3～0.4um), 100 parts of UHMWPE powder (molecular weight is 340-370 ten thousand) obtain puddling uniform powder body after grinding 12h in ball mill (using the mixing steel ball of a diameter of 5mm, 12mm, 15mm 3:1:1 by volume)；
2) powder body after ball milling is completely dissolved in 450 parts of white oils, is slowly heated to while stirring form homogeneous mixture solotion；
3) the UHMWPE/ Graphene mixed solution fully dissolved uses gel spinning method to carry out spinning, and spinning temperature controls at 240 DEG C, and spinning, through solvent extraction, drawing-off, obtains highly directional Graphene/UHMWPE composite fibre.
Embodiment 5:
1) technological process of modified UHMWPE composite fibre sees Fig. 1, comprises the steps:
0.15 part of dispersant is dissolved in 5 parts of white oils, then (6 layers, sheet footpath is 2um, and thickness is 15nm, and specific surface area is 700m with 4 parts of Graphene powder2/ g), 1 part of alumina powder (size d50 is 0.1～0.8um, preferably 0.3～0.4um), 100 parts of UHMWPE powder (molecular weight is 340-370 ten thousand) obtain puddling uniform powder body after grinding 12h in ball mill (using the mixing steel ball of a diameter of 5mm, 12mm, 15mm 3:1:1 by volume)；
2) powder body after ball milling is completely dissolved in 900 parts of white oils, is slowly heated to while stirring form homogeneous mixture solotion；
3) the UHMWPE/ Graphene mixed solution fully dissolved uses gel spinning method to carry out spinning, and spinning temperature controls at 240 DEG C, and spinning, through solvent extraction, drawing-off, obtains highly directional Graphene/UHMWPE composite fibre.
The foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention, although the present invention being described in detail with reference to previous embodiment, for a person skilled in the art, technical scheme described in foregoing embodiments still can be modified by it, or wherein portion of techniques feature is carried out equivalent.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (10)
1. a Graphene, the UHMWPE fiber of alumina composite modification, it is characterised in that: described composite modified UHMWPE
In fiber, it is 100 parts of meters according to the weight portion of contained UHMWPE, also includes the Graphene of 2-5 part, the oxidation of 0.05-2 part
Aluminum.
The UHMWPE fiber that Graphene the most according to claim 1, alumina composite are modified, it is characterised in that: by weight
Amount part meter, UHMWP 100 parts, Graphene 3.5 parts, the aluminium oxide of 0.8 part.
The UHMWPE fiber that Graphene the most according to claim 1 and 2, alumina composite are modified, it is characterised in that:
The molecular weight of described UHMWPE powder is 340-370 ten thousand.
The UHMWPE fiber that Graphene the most according to claim 1 and 2, alumina composite are modified, it is characterised in that:
Size d50 of described aluminium oxide is 0.1～0.8um, preferably 0.3～0.4um.
The UHMWPE fiber that Graphene the most according to claim 1 and 2, alumina composite are modified, it is characterised in that:
Described Graphene is the graphene powder of single or multiple lift structure, and its sheet footpath is 0.5～5um, and thickness is 0.5～30nm, compares table
Area is 200～1000m2/g.Preferably, described graphene film footpath is 3-4um, and thickness is 3.2～4nm, and specific surface area is
300～600m2/g。
6. according to the Graphene described in any one of claim 1-5, the preparation method of the UHMWPE fiber of alumina composite modification,
It is characterized in that: comprise the steps:
1) Graphene powder, alumina powder, UHMWPE sphere of powder mill premix
Graphene powder, alumina powder, UHMWPE powder put into ball grinder, and weigh stainless steel ball by ball material mass ratio 10:1,
Then adding and seal dissolved with after the white oil of dispersant, grind 12h on ball mill, drum's speed of rotation is 600-1000rpm,
Obtain Graphene/aluminium oxide/UHMWPE composite granule；
2) preparation of liquid is spun in advance
Graphene/aluminium oxide/UHMWPE composite granule after ball milling is completely dissolved in white oil, is slowly heated to while stirring
Form mixed uniformly spinning solution；
3) spinning, extraction, drawing-off
To step 2) spinning solution that obtains uses gel spinning method to carry out spinning, then through solvent extraction, drawing-off, obtains stone
Ink alkene/UHMWPE composite fibre.
The preparation method of the UHMWPE fiber that Graphene the most according to claim 6, alumina composite are modified, its feature
It is: described step 1) in, described dispersant uses described dispersant to use PSS, SDBS, SDS, BYK dispersant
Or the mixing of one or more in AFCONA dispersant.
The preparation method of the UHMWPE fiber that Graphene the most according to claim 6, alumina composite are modified, its feature
It is: dispersant: the mass ratio of UHMWPE powder is (0.05-0.15): 100, preferably 0.1:100.
The preparation method of the UHMWPE fiber that Graphene the most according to claim 6, alumina composite are modified, its feature
It is: described step 1) in, described steel ball uses the mixing steel of a diameter of 5mm, 12mm, 15mm 3:1:1 by volume
Ball.
The preparation method of the UHMWPE fiber that Graphene the most according to claim 6, alumina composite are modified, it is special
Levy and be: described step 1) in, described white oil addition is the 1/20 of UHMWPE opaque amount；Described step 2) in, white oil
Consumption: the mass ratio of UHMWPE powder is 9:2.
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| CN107419354A (en) * | 2017-08-21 | 2017-12-01 | 江苏九九久科技有限公司 | High cut resistant high-strength high-modulus polyethylene long filament and preparation method thereof |
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