CN108315833A - The preparation method of graphene ultra-high molecular weight polyethylene composite fibre - Google Patents
The preparation method of graphene ultra-high molecular weight polyethylene composite fibre Download PDFInfo
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- CN108315833A CN108315833A CN201810036884.4A CN201810036884A CN108315833A CN 108315833 A CN108315833 A CN 108315833A CN 201810036884 A CN201810036884 A CN 201810036884A CN 108315833 A CN108315833 A CN 108315833A
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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 present invention provides a kind of preparation methods of graphene ultra-high molecular weight polyethylene composite fibre comprising following steps：S1：In a solvent using the method dispersion being blended by polyvinyl resin with super-high molecular weight and filler, uniform resin dispersion liquid is formed；S2：Graphene powder is added in dispersant, after being heated to certain temperature, emulsifier is added, carries out emulsification treatment, obtains graphene dispersing solution；S3：The graphene dispersing solution is added in the resin dispersion liquid, agitating and heating obtains spinning solution；S4：The spinning solution is subjected to spinning, precursor standing and hot gas spring, obtains graphene ultra-high molecular weight polyethylene composite fibre.The present invention adds filler material and graphene to enhance the intensity of superhigh molecular weight polyethylene fibers in superhigh molecular weight polyethylene fibers, and final strength reaches 30~45cN/dtex, while the composite fibre also has the performances such as excellent uvioresistant, anti-cutting.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene ultra-high molecular weight polyethylene composite fibre, belong to fibrous material skill
Art field.
Background technology
Ultra-high molecular weight polyethylene is a kind of thermoplastic engineering plastic with Good All-around Property, in modernized war and
The fields such as Aeronautics and Astronautics, marine site defence equipment play very important effect.Ultra-high molecular weight polyethylene has fire retardant, anti-
Chemical attack, it is wear-resisting, electrical insulating property is excellent and mechanical strength is higher the advantages that, be widely used in each field, be in the world
The maximum engineering plastics of yield.
It is also mostly insufficient although ultra-high molecular weight polyethylene has many excellent characteristics：Since its strand is very long, pole
When easily generation chain entanglement melts, melt viscosity is up to 108Pas；And critical shear speed is low, and melt fracture easily occurs, and adds to molding
Work brings difficulty；Separately there are the scarce limits such as case hardness is low, wear-resistant grain wear resistance difference is low with thermal deformation.In order to enable it in condition
It is required that high certain fields need to carry out ultra-high molecular weight polyethylene performance suitably modified to application.Modified purpose is：In not shadow
On the basis of ringing UHMW-PE performances, fluidity of molten is improved, or for ultra-high molecular weight polyethylene self performance the shortcomings that is compound
Modified (such as fluidity of molten, heat resistance, case hardness).
It is by superelevation to introduce high cut resistant superhigh molecular weight polyethylene fibers application No. is 201410474250.9 patent
Molecular weight polyethylene and the inorganic ultrafine micro mist of nanocrystalline structure form are constituted.Inorganic ultrafine micro mist is aluminium, titanium, silicon, boron zirconium
The one or more combination of oxide, carbide, nitride, this cut resistant superhigh molecular weight polyethylene fibers tensile strength are
19-21cN/dtex, stretch modulus are 750-850cN/dtex, can be used as anti-cutting gloves application.
It is by supra polymer to introduce ultra-high molecular weight polyethylene composite material application No. is 201410814002.4 patent
Weight northylen, lubricant, filler material, reinforcing fiber, nano-inorganic filler.Wherein filler material is glass microballoon, ceramic microsphere, oxygen
Change one or more of aluminium, silicon carbide, boron carbide.Gained composite material has excellent impact resistance, wear-resistant, self-lubricating
The performances such as property, resistant to chemical etching.
The present invention is in order to further improve the intensity, wearability, heat resistance of superhigh molecular weight polyethylene fibers, in superelevation point
In sub- weight polyethylene fiber, inorganic filler is not only added, while being added to graphene powder, finally obtained with compared with high-tenacity
The compound superhigh molecular weight polyethylene fibers of functional form.
Invention content
For the defects in the prior art, the object of the present invention is to provide a kind of graphene ultra-high molecular weight polyethylene is compound
The preparation method of fiber.
The present invention is achieved by the following technical solutions：
The present invention provides a kind of preparation methods of graphene ultra-high molecular weight polyethylene composite fibre comprising following step
Suddenly：
S1：In a solvent using the method dispersion being blended by polyvinyl resin with super-high molecular weight and filler, it is formed uniform
Resin dispersion liquid；
S2：The graphene dispersing solution is added in the resin dispersion liquid, agitating and heating obtains spinning solution；
S3：The spinning solution is subjected to spinning, precursor standing and hot gas spring, it is multiple to obtain graphene ultra-high molecular weight polyethylene
Condensating fiber.
Preferably, the weight average molecular weight of the ultra-high molecular weight polyethylene is 4.0 × 106~6.0 × 106。
Preferably, the dosage of the filler is the 5~20% of polyvinyl resin with super-high molecular weight weight.
Preferably, the graphene dispersing solution is added in dispersant by graphene powder, and after heating, breast is added
Agent obtains after carrying out emulsification treatment；
Preferably, the filler is selected from silicon carbide, diamond, glass microballoon, ceramic fibre, glass fibre, profound
At least one of military rock fiber and metallic fiber.
Preferably, in the filler, silicon carbide, diamond, glass microballoon average grain diameter be 100~400nm.
Preferably, in the filler, ceramic fibre, glass fibre, basalt fibre and metallic fiber diameter
In 1~100um, draw ratio is 8~20.
Preferably, the weight ratio of the polyvinyl resin with super-high molecular weight and solvent is (1~8):(10~15).
Preferably, the solvent is selected from naphthane, decahydronaphthalene, normal heptane, n-hexane, hexamethylene, paraffin oil, white
It is one or more in oil, kerosene, vegetable oil, animal oil.
Preferably, the dosage of the graphene is the 0.5~10% of polyvinyl resin with super-high molecular weight weight.
Preferably, the thickness of the graphene is 0.4~5nm, and piece diameter is 0.01~6 μm, specific surface area 500
~1000m2/g；The graphene be selected from coupling agent modified graphene oxide, cationic surfactant modified graphene oxide,
In few layer graphene of few layer graphene, the preparation of electrochemical stripping method prepared by halogenated hydrocarbons modified graphene oxide, ball-milling method
It is one or more of.
Preferably, the speed that the high speed shear is blended is 1500~2800r/min, and mixing time is 4~6h；
The temperature of the spinning is 110~180 DEG C, and spinning process is dry spinning method or wet spinning process.
Compared with prior art, the present invention has following advantageous effect：
1, it is poly- to enhance super high molecular weight to add filler material and graphene in superhigh molecular weight polyethylene fibers by the present invention
The intensity of vinyl fiber, final strength reaches 30~45cN/dtex, while the composite fibre also has excellent uvioresistant, prevents cutting
The performances such as cut；
2, graphene is modified by the present invention, can well be dissolved in organic solvent, and this method is instead of multiple
Miscellaneous graphene and ultra-high molecular weight polyethylene ball milling blending technology, and modified graphene can easily and super high molecular weight
Polyethylene is compound, to ensure that the content of graphene in finished fiber, it is ensured that its performance；
3, the heat shock resistance function that the present invention utilizes graphene excellent, it is compound with ultra-high molecular weight polyethylene, it obtains
The excellent composite fibre of thermal shock resistance, greatly improved the heat resistance of superhigh molecular weight polyethylene fibers, to expand
Its big application range；
4, graphene ultra-high molecular weight polyethylene composite fibre of the invention can be used for rope, hawser, supertanker, sea
The guard shield cover etc. of foreign operating platform, flak jackets, parachute, warship armor protective plate, radar.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
Present embodiments provide a kind of preparation method of graphene ultra-high molecular weight polyethylene composite fibre, specifically include as
Lower step：
S1：Polyvinyl resin with super-high molecular weight 100kg and 5kg silicon carbide is dispersed in using the method that high speed shear is blended
In white oil, the rotating speed that control high speed shear is blended is 1500~2800r/min, forms uniform resin dispersion in a heated condition
Liquid；
S2：Graphene dispersing solution containing 0.5kg graphene powders is added in the resin dispersion liquid, agitating and heating
Obtain spinning solution；
S3：The spinning solution is subjected to dry spinning at 110 DEG C, then using precursor standing and hot gas spring, is obtained
Graphene ultra-high molecular weight polyethylene composite fibre.
Embodiment 2
Present embodiments provide a kind of preparation method of graphene ultra-high molecular weight polyethylene composite fibre, specifically include as
Lower step：
S1：The method point that polyvinyl resin with super-high molecular weight 100kg and 20kg bortz powder is blended using high speed shear
It is dispersed in naphthane, the rotating speed that control high speed shear is blended is 1500~2800r/min, forms uniform tree in a heated condition
Fat dispersion liquid；
S2：Graphene dispersing solution containing 10kg graphene powders is added in the resin dispersion liquid, agitating and heating
Obtain spinning solution；
S3：The spinning solution is subjected to dry spinning at 110 DEG C, then using precursor standing and hot gas spring, is obtained
Graphene ultra-high molecular weight polyethylene composite fibre.
Embodiment 3
Present embodiments provide a kind of preparation method of graphene ultra-high molecular weight polyethylene composite fibre, specifically include as
Lower step：
S1：The method point that polyvinyl resin with super-high molecular weight 100kg and 10kg ceramic fibre is blended using high speed shear
It is dispersed in decahydronaphthalene, the rotating speed that control high speed shear is blended is 1500~2800r/min, forms uniform tree in a heated condition
Fat dispersion liquid；
S2：Graphene dispersing solution containing 5kg graphene powders is added in the resin dispersion liquid, agitating and heating obtains
To spinning solution；
S3：The spinning solution is subjected to dry spinning at 110 DEG C, then using precursor standing and hot gas spring, is obtained
Graphene ultra-high molecular weight polyethylene composite fibre.
Embodiment 4
Present embodiments provide a kind of preparation method of graphene ultra-high molecular weight polyethylene composite fibre, specifically include as
Lower step：
S1：The method point that polyvinyl resin with super-high molecular weight 100kg and 15kg glass fibre is blended using high speed shear
It is dispersed in normal heptane, the rotating speed that control high speed shear is blended is 1500~2800r/min, forms uniform tree in a heated condition
Fat dispersion liquid；
S2：Graphene dispersing solution containing 1kg graphene powders is added in the resin dispersion liquid, agitating and heating obtains
To spinning solution；
S3：The spinning solution is subjected to dry spinning at 110 DEG C, then using precursor standing and hot gas spring, is obtained
Graphene ultra-high molecular weight polyethylene composite fibre.
Comparative example 1
The preparation method of this comparative example is not added with filler with differing only in for embodiment 1 in resin dispersion liquid.
Comparative example 2
The preparation method of this comparative example is not added with graphene dispersing solution with differing only in for embodiment 1.
Comparative example 3
The preparation method of this comparative example is not added with filler with differing only in for embodiment 1 in resin dispersion liquid, also not
Add graphene dispersing solution.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (12)
1. a kind of preparation method of graphene ultra-high molecular weight polyethylene composite fibre, which is characterized in that include the following steps：
S1：In a solvent using the method dispersion being blended by polyvinyl resin with super-high molecular weight and filler, uniform resin is formed
Dispersion liquid；
S2：The graphene dispersing solution is added in the resin dispersion liquid, agitating and heating obtains spinning solution；
S3：The spinning solution is subjected to spinning, precursor standing and hot gas spring, obtains the compound fibre of graphene ultra-high molecular weight polyethylene
Dimension.
2. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1, which is characterized in that institute
The weight average molecular weight for stating ultra-high molecular weight polyethylene is 4.0 × 106~6.0 × 106。
3. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1, which is characterized in that institute
The dosage for stating filler is the 5~20% of polyvinyl resin with super-high molecular weight weight.
4. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1, which is characterized in that stone
Black alkene dispersion liquid is added in dispersant by graphene powder, after heating, emulsifier is added, is obtained after progress emulsification treatment.
5. the preparation method of the graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1 or 3, feature exist
In the filler is selected from silicon carbide, diamond, glass microballoon, ceramic fibre, glass fibre, basalt fibre and metallic fiber
At least one of.
6. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as claimed in claim 5, which is characterized in that institute
The grain size for stating silicon carbide, diamond and glass microballoon is 100~400nm.
7. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as claimed in claim 5, the ceramic fibre,
A diameter of 1~100um of glass fibre, basalt fibre and metallic fiber, draw ratio are 8~20.
8. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1, which is characterized in that institute
The weight ratio for stating polyvinyl resin with super-high molecular weight and solvent is (1~8)：(10~15).
9. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1 or 6, feature exist
In the solvent is selected from naphthane, decahydronaphthalene, normal heptane, n-hexane, hexamethylene, paraffin oil, white oil, kerosene, vegetable oil, moves
It is one or more in object oil.
10. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1, which is characterized in that
The dosage of the graphene is the 0.5~10% of polyvinyl resin with super-high molecular weight weight.
11. the preparation method of the graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1 or 10, feature exist
In the thickness of the graphene is 0.4~5nm, and piece diameter is 0.01~6 μm, and specific surface area is 500~1000m2/g；The stone
Black alkene is selected from coupling agent modified graphene oxide, cationic surfactant modified graphene oxide, the modified oxidized stone of halogenated hydrocarbons
One or more of few layer graphene of few layer graphene, the preparation of electrochemical stripping method prepared by black alkene, ball-milling method.
12. the preparation method of graphene ultra-high molecular weight polyethylene composite fibre as described in claim 1, which is characterized in that
The blending method is high speed shear, and it is 1500~2800r/min that speed, which is blended, and mixing time is 4~6h；The temperature of the spinning
Degree is 110~180 DEG C, and spinning process is dry spinning method or wet spinning process；The dispersant is selected from SDS, SDBS, PSS,
PVP, Span-60 and Span-80's is one or more.
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| CN109355726A (en) * | 2018-09-20 | 2019-02-19 | 江苏恒辉安防股份有限公司 | Polymer fiber and preparation method thereof |
| 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 |
| CN109467814A (en) * | 2018-09-20 | 2019-03-15 | 中山德盛塑料有限公司 | A kind of compound mineral fiber filling polypropylene composite material 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 |
| CN109629028A (en) * | 2018-11-15 | 2019-04-16 | 南通强生安全防护科技股份有限公司 | A kind of graphene ultra-high molecular weight polyethylene composite fibre and preparation method thereof |
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| CN109881283A (en) * | 2019-01-16 | 2019-06-14 | 江苏恒辉安防股份有限公司 | A kind of graphene/UHMWPE composite conducting fiber and preparation method thereof |
| CN109881281A (en) * | 2019-01-14 | 2019-06-14 | 常州兴烯石墨烯科技有限公司 | Anti- cutting graphite alkene ultra-high molecular weight polyethylene composite fibre and preparation method thereof |
| CN109912873A (en) * | 2019-02-28 | 2019-06-21 | 常州兴烯石墨烯科技有限公司 | Anti- cutting graphite alkene ultra-high molecular weight polyethylene laminated film and preparation method thereof |
| CN111041588A (en) * | 2019-12-31 | 2020-04-21 | 江苏锵尼玛新材料股份有限公司 | Novel high-cutting-resistance ultra-high molecular weight polyethylene fiber and preparation method thereof |
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