CN106854833A - A kind of antistatic superhigh molecular weight polyethylene fibers of lightweight and preparation method thereof - Google Patents
A kind of antistatic superhigh molecular weight polyethylene fibers of lightweight and preparation method thereof Download PDFInfo
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- 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
- D06M13/322—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 nitrogen
- D06M13/325—Amines
- D06M13/328—Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
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- 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
- D06M13/322—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 nitrogen
- D06M13/368—Hydroxyalkylamines; Derivatives thereof, e.g. Kritchevsky bases
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- 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
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Abstract
The present invention discloses antistatic superhigh molecular weight polyethylene fibers of a kind of lightweight and preparation method thereof.Fiber of the present invention includes high molecular weight polyethylene fiber basic unit, the dopamine active layer for investing substrate surface and the partial reduction graphene layer that dopamine activation layer surface is attached in lamella deployed condition.The present invention obtains the antistatic superhigh molecular weight polyethylene fibers of lightweight by the decentralized medium and dispersion liquid concentration of preferred graphene oxide, reducing agent species and dipping time.Using the characteristic of partial reduction Graphene：1) carbon oxygen atom ratio, appropriate oxy radical ensure that the partial reduction Graphene fiber modified with dopamine occurs sufficiently strong interaction, while providing enough electric conductivity；2) the lamella number of plies, influences its stabilization absorption on fiber；3) slice plane size, influences lamella in the coating of fiber surface, and conductive path.
Description
Technical field
The invention belongs to technical field of polymer materials, be related to a kind of antistatic superhigh molecular weight polyethylene fibers of lightweight and
Its preparation method.
Background technology
Ultra-high molecular weight polyethylene (UHMWPE) fiber and carbon fiber, aramid fiber and the referred to as big high-performance in the world three fibre
Dimension is most important in national defense industry and protective gear field.UHMWPE fibers in addition to high intensity, modulus, its density
Relatively low (about 0.97g/cm3), be that uniquely may float on the high-performance fiber on the water surface, at the same have shock resistance, it is corrosion-resistant,
It is wear-resistant to wait excellent properties.However, due to the dielectric constant of UHMWPE fibers low (2.4), resistance (＞ 10 high14Ω), in application
When antistatic property it is poor.UHMWPE fibers are in elevated chemical inertia, and surface is extremely smooth, and it is also this area that it is modified
One of great difficult problem.
Antistatic coating fiber type refers to, with fiber as matrix, to be solidificated in one layer of conduction of fiber surface absorption by coating and fill out
The fiber of material.Traditional conductive coating type is mainly metal (such as silver, copper, nickel), but metal coating often makes fibre density
Increase, thus brings the low shortcoming of unit resource benefit.The Chinese invention patent of Publication No. CN102277728 is (close using silver
It is 10.49g/cm to spend3) be conducting particles, with silver ammino solution as silver plating liquid, it is silver-plated it is preceding by fiber carry out slurry and surface active
Treatment, finally gives a kind of conductive UHMWPE fibers, wherein when line resistance is about 0.15 Ω/cm, fibre density is from
0.97g/cm before reason3It is changed into the about 1.92g/cm after treatment3(density increase about 95%).The China of Publication No. CN1693576
Patent of invention is deoiled to fabric, is roughened, striping, sensitization, after the pre-treatment such as activation, once being changed with nickel, copper as conducting particles
Nickel plating, electro-coppering and secondary chemical nickel plating or electronickelling are learned, a kind of high performance electromagnetism is obtained by the adjustment of technological parameter
Shielding conductive dacron fabric, the fabric face resistance is 0.03 Ω/, and conductive fabric surface density is from 55g/cm2Increase to
111g/cm2(density increase about 102%).
In order to obtain the benefit of same even more high from less resource, exploitation lightweight antistatic fibre just seems very
It is meaningful.And Graphene as a kind of New Type of Carbon nanometer super light material, with relatively low density (based on graphite：2.25g/cm3)、
Great specific surface area (2363m2/ g), fabulous electric conductivity (6 × 103S/cm) and be exceedingly fast electron transfer rate (2 ×
105cm2/ Vs), it is a kind of outstanding two-dimensional nano conductive material.When Graphene is used as conductive coating, can be in irreducible minimum
On the premise of degree changes density of material, the tremendous increase of electric conductivity is obtained.The Chinese invention patent of Publication No. CN102926207
In conductive fabric prepared using dip dyeing technique and its preparation method and application, fabric is carried out into base extraction, pretreatment, assisting-dyeing
Agent immersion and Graphene aqueous dispersions impregnate, and conducting particles are adsorbed onto into fabric face under ultrasonication, graphite in the fabric
The mass percent of alkene is 3.5%, and it is 3.6 × 10 that fabric is changed into electrical conductivity from insulating2S/cm.Publication No. CN103966844
Chinese invention patent provide a kind of preparation method of graphene conductive composite fibre, terylene (or cotton or viscose glue) fiber is made
After with silane coupler surface activation process, be immersed in the graphene aqueous solution containing dispersant (mass concentration be 0.1%~
5%), Graphene content is 1%~3% in composite fibre after drying, and the resistivity of Graphene composite fibre is 10~105Ω·
M, than conventional fibre resistivity (~1014Ω m) reduce by more than ten order of magnitude.
Metal coating is contrasted with graphite ene coatings for fiber or the improvement degree of fabric electric conductivity, it is seen that, stone
Black alkene can be more favorable for the lifting of materials conductive performance under the conditions of identical weightening, thus Graphene is to prepare the antistatic material of lightweight
That expects is preferred.But chemical inertness and interlayer van der Waals interaction due to Graphene, cause the difficult stripping of piece interlayer and coating is easy
Obscission, seriously hinders the performance of its electrical-conductive nanometer material advantage.Graphene is particularly applied to UHMWPE fibers
During surface treatment, because UHMWPE fibers are in elevated chemical inertia, surface is extremely smooth, causes graphene sheet layer to be difficult
UHMWPE fiber surfaces are evenly distributed and combine closely.Therefore, it is badly in need of the new material system of research and method is above-mentioned to solve
Problem, and the antistatic UHMWPE fibers of lightweight are produced in economically viable mode.
The content of the invention
First purpose of the invention is to provide a kind of antistatic superhigh molecular weight polyethylene fibers of lightweight.
The antistatic superhigh molecular weight polyethylene fibers of lightweight include that high molecular weight polyethylene fiber basic unit, dopamine live
Change layer and partial reduction graphene layer (being referred to as Graphene antistatic layer)；Wherein dopamine active layer is attached at basic unit's table
Face, partial reduction graphene layer is attached at dopamine activation layer surface in lamella deployed condition.
The density of the antistatic superhigh molecular weight polyethylene fibers of described lightweight is 0.97~1.03g/cm3, a diameter of 15
~25 μm, intensity is 30~40cN/dtex, and modulus is 800~1600cN/dtex, and elongation at break is 2.5%~4.5%, table
Surface resistivity is 103~1010Ω/cm, surface carbon oxygen atom ratio is 4: 1~10: 1；(surface carbon oxygen atom herein is than referring to
The carbon oxygen atom ratio of UHMWPE+ dopamines+Graphene)；
Described dopamine active layer mass content is 0.01%~1.0%, and carbon oxygen atom ratio is 4: 1~6: 1；
The mass content of described partial reduction graphene layer is 0.1%~5%, and carbon oxygen atom compares 5: 1~10: 1, lamella
Surface size is 0.1~2 μm, and the lamella number of plies is 1~10 layer；Described partial reduction graphene layer and the matter of dopamine active layer
Amount is than being 500: 1~0.1: 1；
After being cleaned by ultrasonic 2h in the antistatic superhigh molecular weight polyethylene fibers of described lightweight water at room temperature, its surface
Resistivity is 1~100 times before cleaning.
Second object of the present invention is to provide a kind of preparation method of the antistatic superhigh molecular weight polyethylene fibers of lightweight,
The method is comprised the concrete steps that：
Step (1), the preparation of graphene oxide dispersion：
Graphene oxide powder is added in decentralized medium under normal temperature, first 20~30min of mechanical agitation, stir speed (S.S.) is
500~800r/min, then ultrasonically treated 20~40min in ice-water bath, obtain uniform and stable graphene oxide dispersion；
Wherein graphene oxide powder is the 0.01%~1% of decentralized medium weight.
The carbon oxygen atom ratio of described graphene oxide is 2: 1~4: 1, and sheet surfaces size is 0.1~2 μm, and piece is layer by layer
Number is 1~10 layer；
Described decentralized medium is in water, ethylene glycol, 1-METHYLPYRROLIDONE (NMP) and dimethylformamide (DMF)
One or two mixture；
Preferably, the graphene oxide is the 0.05%~0.5% of decentralized medium weight；
Preferably, the pH value of described graphene oxide decentralized medium is 8~12；
Step (2), the cleaning of UHMWPE fibers：UHMWPE fibers are cleaned by ultrasonic 0.5 in a solvent at room temperature~
1.5h, takes out stand-by after drying；Described solvent is one or two the mixture in ethanol, acetone and tetrahydrofuran；
The molecular weight of described UHMWPE fibers is 100~3,000,000, and density is 0.97g/cm3, a diameter of 15~25 μm,
Intensity is 30~40cN/dtex, and modulus is 800~1600cN/dtex, and elongation at break is 2.5%~4.5%, sheet resistance
Rate is 1012~1016Ω/cm；Surface carbon oxygen atom ratio is 10: 1~1000: 1；
Preferably, a diameter of 20~23 μm of UHMWPE fibers, carbon oxygen atom ratio in surface is 100: 1~1000: 1；
Step (3), the preparation of activated fiber：In three (methylol) aminomethanes-hydrochloric acid (Tris-HCl) that pH is 8~11
Dopamine is added in cushioning liquid, dopamine solution is obtained；The fibre after step 2 treatment is added in above-mentioned dopamine solution again
Dimension, stands 8~24h of reaction, and washing obtains dopamine activation UHMWPE fibers after drying；
Described dopamine is one or two the mixture in catecholamines or hexichol quinones, structural formula
Such as (1), wherein R be with amino group-(CHy)x-NH2Or-(CHy)x-NH-(CHq)p-CH3Or-(CH2)x-NH-(CO)x-
(CH2)P-CH3Or-(CH2)x-NH-(CO)x-(CH2)P-C6H5Or-(CH2)x-NH2Or-(CHy)x-N(CHj)h-(CHq)p-(CH3)e
Or-CHOH-NH- (CH2)p-CH3Or-CHOH- (CH2)x-NH2, wherein x is 1~99 natural number, and p, h are 0~99 nature
Number, y, q, e are 1 or 2, j are 1,2 or 3；
Preferably, R is N is 1~10 natural number；
Preferably, the pH of the Tris-HCl cushioning liquid is 8~10；
Preferably, the mass concentration of the dopamine solution is 0.1%~0.3%；
Described UHMWPE fibers are 2%~10% with the mass ratio of dopamine solution；
The surface carbon oxygen atom ratio of described dopamine activation UHMWPE fibers is 4: 1~8: 1；(surface carbon oxygen is former herein
Carbon oxygen atom ratio of the son than reference UHMWPE+ dopamines)；
The preparation of step (4), the antistatic UHMWPE of lightweight：The activated fiber that step (3) is obtained is immersed in into step (1) to obtain
To graphene oxide dispersion in, add reducing agent, at 50~95 DEG C with the rotating speed of 100~500r/min stirring 1~
5h, then dries fiber wash, repeats this dipping reduction process 2~10 times, obtains partial reduction Graphene coating superelevation point
Sub- weight polyethylene fiber；
The reducing agent is in ammoniacal liquor, hydrazine hydrate, hydroiodic acid, sodium borohydride, ascorbic acid, sodium peroxydisulfate, glucose
One or two mixture.
The graphene oxide is 1: 0.5~1: 40 with the mass ratio of reducing agent；
In the Graphene coating superhigh molecular weight polyethylene fibers, Graphene content is 0.1%~5%, fiber surface
Carbon oxygen atom ratio is 4: 1~10: 1, and graphene sheet layer size is 0.1~2 μm, and the Graphene number of plies is 1~10 layer.
The present invention by the decentralized medium and dispersion liquid concentration of preferred graphene oxide, reducing agent species and dipping time,
Obtain the antistatic superhigh molecular weight polyethylene fibers of lightweight.Using the characteristic of partial reduction Graphene：1) carbon oxygen atom ratio, in right amount
Oxy radical ensure that the modified fiber of partial reduction Graphene and dopamine occurs sufficiently strong interaction, while
Enough electric conductivity is provided；2) the lamella number of plies, when the number of plies of partial reduction Graphene is too high, can reduce unit volume Graphene number
Amount, so be unfavorable for its on fiber stabilization absorption, and the number of plies of partial reduction Graphene it is too low when, then easily occur from roll up
Contract and be unfavorable for being fully extended in UHMWPE fiber surfaces, and then drop low-fiber electric conductivity；3) slice plane size, fits
Suitable slice plane size not only contributes to coating of the lamella in fiber surface, and is conducive to the formation of conductive path；4) divide
Powder, the oxy radical of graphene oxide makes it be uniformly dispersed in polar solvent, reduces the reunion between lamella, is beneficial to
It is fully contacted with fiber；In addition, reducing agent species is by influenceing reducing degree (the i.e. graphenic surface of graphene oxide
Carbon oxygen atom ratio), and then change Graphene and the adhesion size on activated fiber surface, finally influence the density and conduction of fiber
Performance.Meanwhile, dipping time determine fiber surface absorption Graphene quantity number, so also direct fibre property.In a word,
The present invention obtains the light of good antistatic property by the dispersion liquid of preferred graphene oxide, reducing agent species and dipping time
Matter ultra-high molecular weight fibers.
Brief description of the drawings
Fig. 1 is the electron microscope of superhigh molecular weight polyethylene fibers；
Fig. 2 is the electron microscope of activated fiber；
Fig. 3 is the electron microscope that Graphene coats superhigh molecular weight polyethylene fibers.
Specific embodiment
Technical scheme and effect are further described with reference to embodiment, it is to be understood that, these
Description is intended merely to further illustrate the features and advantages of the present invention, and they can not be interpreted as to the scope of the present invention
Limit.
The computational methods of fibre density described in the present embodiment are：UHMWPE fibre densities are 0.973g/cm3, it is a diameter of
15~25 μm, surface resistivity is 1012~1016The diameter (as shown in Figure 1) of Ω/cm, UHMWPE fiber is in activation (such as Fig. 2 institutes
Show) and Graphene coating (as shown in Figure 3) before and after be held essentially constant, by weigh a fixed length coat after fiber weight calculating
And obtain.
Comparative example 1：
The Tris-HCl cushioning liquid that 500mL pH are 10 is measured, 1g dopamines are added, UHMWPE is stirring evenly and then adding into
Fiber (through the ultrasonically treated 1h of acetone), stands reaction 24h, obtains activated fiber；Then dripped toward side in 1.0% silver nitrate solution
Ammonification waterside is stirred, and is become to solution and is clarified, afterwards by its potassium sodium tartrate solution with 5.0% by volume for 1: 1 mixing is equal
It is even, form silver plating liquid；Finally activated fiber is immersed in silver plating liquid, shading reaction 0.5h, obtains silver plated fiber at room temperature.
Fibre density prepared by the method is 1.053g/cm3, resistivity is 1010Ω/cm, fiber fastness is：Surpass at room temperature
Resistivity is changed into 10 after sound cleaning 2h13Ω/cm, that is, 1000 times before cleaning.It can be seen that, it is right using dopamine treatment UHMWPE fibers
Silver-plated afterwards, the resistivity of fiber reaches 10 after the usage amount of preferred silver makes treatment10Ω/cm, its density increases to 1.053g/
cm3, the usage amount of silver is further reduced, the density of fiber reduces after treatment, but resistivity is more than 1010Ω/cm。
Comparative example 2：
The Tris-HCl cushioning liquid that 500mL pH are 9 is measured, 1g dopamines are added, UHMWPE is stirring evenly and then adding into fine
Dimension stands reaction 24h (through the ultrasonically treated 1h of acetone), obtains activated fiber；Then it is added dropwise toward side in 3.8% silver nitrate solution
Ammoniacal liquor side is stirred, and is become to solution and is clarified, afterwards by its potassium sodium tartrate solution with 17% by volume for be well mixed at 1: 1,
Form silver plating liquid；Finally activated fiber is immersed in silver plating liquid, shading reaction 0.5h, obtains silver plated fiber at room temperature.
Fibre density prepared by the method is 1.102g/cm3, resistivity is 104Ω/cm, fiber fastness is：Surpass at room temperature
Resistivity is changed into 10 after sound cleaning 2h7Ω/cm, that is, 1000 times before cleaning.It can be seen that, it is right using dopamine treatment UHMWPE fibers
It is silver-plated afterwards, although to decline the resistivity of fiber, but fibre density is higher, and the fastness of silver coating is not enough.
Comparative example 3：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines are added, UHMWPE is stirring evenly and then adding into
Fiber (through the ultrasonically treated 1h of acetone), stands reaction 24h, obtains activated fiber；Then dripped toward side in 3.8% silver nitrate solution
Ammonification waterside is stirred, and is become to solution and is clarified, afterwards by its potassium sodium tartrate solution with 17% by volume for 1: 1 mixing is equal
It is even, form silver plating liquid；Finally activated fiber is immersed in silver plating liquid, shading reaction 8h, obtains silver plated fiber at room temperature.
Fibre density prepared by the method is 1.943g/cm3, resistivity is≤1.0 Ω/cm, and fiber fastness is：At room temperature
Resistivity is changed into 10 after being cleaned by ultrasonic 2h7Ω/cm, that is, before cleaning 107Times.It can be seen that, it is right using dopamine treatment UHMWPE fibers
Silver-plated afterwards, when the usage amount of silver is higher, although the resistivity of fiber is effectively declined, but fibre density is significantly raised, and plating
The fastness of silver layer is not enough.
Comparative example 4：
Take graphene oxide 1.25g to be added in 500mL deionized waters, mechanical agitation 30min, ultrasonically treated 30min；Will
In UHMWPE fibers (through the ultrasonically treated 1h of acetone) immersion graphene oxide dispersion, it is 9 to add ammoniacal liquor regulation pH, adds water
Hydrazine (graphene oxide is 10: 7 with the mass ratio of hydrazine hydrate) is closed, 3h is stirred with the rotating speed of 200r/min at 95 DEG C, complete stone
Black alkene coating, repeats this dipping reduction process 8 times, obtains Graphene coating UHMWPE fibers.
Fibre density prepared by the method is 0.976g/cm3, resistivity is 1011Ω/cm, fiber fastness is：Surpass at room temperature
Resistivity is changed into 10 after sound cleaning 2h14Ω, that is, 1000 times before cleaning.It can be seen that, UHMWPE fibers are coated using Graphene, although
Decline the resistivity of fiber, and density keeps relatively low, but the fastness of Graphene coat is not enough.
Embodiment 1：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,0.05g graphene oxides are added in 500mL deionized waters, mechanical agitation 20min, ultrasonically treated 20min；Afterwards
Will activated fiber immerse graphene oxide dispersion in, add ammoniacal liquor regulation pH be 9, add hydrazine hydrate (graphene oxide with
The mass ratio of hydrazine hydrate is 10: 5), 2h is stirred with the rotating speed of 100r/min at 50 DEG C, completes Graphene coating, washs drying
Afterwards, repeat this dipping reduction process 6 times, finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.976g/cm to fiber prepared by the method3, surface resistivity is 108Ω/cm, it is fine
Tieing up fastness is：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature9Ω/cm, that is, 10 times before cleaning.
Embodiment 2：
The Tris-HCl cushioning liquid that 500mL pH are 10 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,0.25g graphene oxides are added in 500mL deionized waters, mechanical agitation 20min, ultrasonically treated 20min；Afterwards
Will activated fiber immerse graphene oxide dispersion in, add ammoniacal liquor regulation pH be 9, add hydrazine hydrate (graphene oxide with
The mass ratio of hydrazine hydrate is 10: 5), 3h is stirred with the rotating speed of 100r/min at 70 DEG C, completes Graphene coating, washs drying
Afterwards, repeat this dipping reduction process 5 times, finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.977g/cm to fiber prepared by the method3, surface resistivity is 108Ω/cm,
Fiber fastness is：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature10Ω/cm, that is, 100 times before cleaning.
Embodiment 3：
The Tris-HCl cushioning liquid that 500mL pH are 9 is measured, 1g dopamines (as shown in table 2) is added, stirred, plus
Enter UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1, stand reaction 24h, obtain activated fiber；Then such as table 3
It is shown, 1.25g graphene oxides are added in 500mL ml deionized waters, mechanical agitation 30min, ultrasonically treated 30min；
Activated fiber is immersed in graphene oxide dispersion afterwards, it is 10 to add ammoniacal liquor regulation pH, adds hydrazine hydrate (graphite oxide
Alkene is 10 with the mass ratio of hydrazine hydrate: 7), 2h is stirred with the rotating speed of 300r/min at 85 DEG C, completes Graphene coating, washing
After drying, this dipping reduction process is repeated 7 times, finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.991g/cm to fiber prepared by the method3, surface resistivity is 106Ω/cm, it is fine
Tieing up fastness is：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 10 times before cleaning.
Embodiment 4：
The Tris-HCl cushioning liquid that 500mL pH are 10 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,2.50g graphene oxides are added in 500mL deionized waters, mechanical agitation 30min, ultrasonically treated 30min；Afterwards
Will activated fiber immerse graphene oxide dispersion in, add ammoniacal liquor regulation pH be 11, add hydrazine hydrate (graphene oxide with
The mass ratio of hydrazine hydrate is 10: 10), 5h is stirred with the rotating speed of 200r/min at 95 DEG C, completes Graphene coating, washs drying
Afterwards, repeat this dipping reduction process 4 times, finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.998g/cm to fiber prepared by the method3, surface resistivity is 106Ω/cm, it is fine
Tieing up fastness is：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature8Ω/cm, that is, 100 times before cleaning.
Embodiment 5：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,5.00g graphene oxides are added in 500mL deionized waters, mechanical agitation 30min, ultrasonically treated 40min；Afterwards
Will activated fiber immerse graphene oxide dispersion in, add ammoniacal liquor regulation pH be 10, add hydrazine hydrate (graphene oxide with
The mass ratio of hydrazine hydrate is 10: 10), 3h is stirred with the rotating speed of 500r/min at 95 DEG C, completes Graphene coating, washs drying
Afterwards, repeat this dipping reduction process 8 times, finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 1.023g/cm to fiber prepared by the method3, surface resistivity is 104Ω/cm, it is fine
Tieing up fastness is：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature6Ω/cm, that is, 100 times before cleaning.
Embodiment 6：
The Tris-HCl cushioning liquid that 500mL pH are 9.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,0.25g graphene oxides are added in 500mL ethylene glycol, mechanical agitation 20min, ultrasonically treated 20min；Afterwards will
In activated fiber immersion graphene oxide dispersion, addition sodium borohydride (graphene oxide is 1 with the mass ratio of sodium borohydride:
4) 2h, is stirred with the rotating speed of 200r/min at 65 DEG C, Graphene coating is completed, after washing is dried, this dipping is repeated and was reduced
Journey 8 times, finally gives Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.979g/cm to fiber prepared by the method3, resistivity is 107Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 1 times before cleaning.
Embodiment 7：
The Tris-HCl cushioning liquid that 500mL pH are 9.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,1.25g graphene oxides are added in 500mL ethylene glycol, mechanical agitation 30min, ultrasonically treated 30min；Afterwards will
In activated fiber immersion graphene oxide dispersion, addition sodium borohydride (graphene oxide is 1 with the mass ratio of sodium borohydride:
6) 4h, is stirred with the rotating speed of 100r/min at 75 DEG C, Graphene coating is completed, after washing is dried, this dipping is repeated and was reduced
Journey 5 times, finally gives Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.989g/cm to fiber prepared by the method3, resistivity is 106Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 10 times before cleaning.
Embodiment 8：
The Tris-HCl cushioning liquid that 500mL pH are 9 is measured, 1g dopamines (as shown in table 2) is added, stirred, plus
Enter UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1, stand reaction 24h, obtain activated fiber；Then such as table 3
It is shown, 2.50g graphene oxides are added in 500mL deionized waters, mechanical agitation 30min, ultrasonically treated 40min；Afterwards
Activated fiber is immersed in graphene oxide dispersion, (graphene oxide is 1 with the mass ratio of sodium borohydride to add sodium borohydride
: 8), 5h is stirred with the rotating speed of 200r/min at 90 DEG C, after washing is dried, repeat this dipping reduction process 5 times；Again by fiber
In immersion graphene oxide dispersion, add glucose (mass ratio of graphene oxide and glucose is 1: 8), at 90 DEG C with
The rotating speed stirring 5h of 200r/min, completes Graphene coating, after washing is dried, repeats this dipping reduction process 5 times, finally gives
Graphene coats UHMWPE fibers.
As shown in table 4, its Midst density is 1.023g/cm to fiber prepared by the method3, resistivity is 104Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature5Ω/cm, that is, 10 times before cleaning.
Embodiment 9：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,0.25g graphene oxides are added in 500mL nmp solutions, mechanical agitation 20min, ultrasonically treated 20min；Afterwards
Activated fiber is immersed in graphene oxide dispersion, (graphene oxide is 1 with the mass ratio of ascorbic acid to add ascorbic acid
: 10), 1h is stirred with the rotating speed of 100r/min at 50 DEG C, complete Graphene coating, after washing is dried, repeat this dipping reduction
Process 2 times, finally gives Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.975g/cm to fiber prepared by the method3, resistivity is 1010Ω/cm, fiber
Fastness is：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature10Ω/cm, that is, 1 times before cleaning.
Embodiment 10：
The Tris-HCl cushioning liquid that 500mL pH are 9 is measured, 1g dopamines (as shown in table 2) is added, stirred, plus
Enter UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1, stand reaction 24h, obtain activated fiber；Then such as table 3
It is shown, 1.25g graphene oxides are added in 500mL nmp solutions, mechanical agitation 30min, ultrasonically treated 30min；Afterwards
Activated fiber is immersed in graphene oxide dispersion, (graphene oxide is 1 with the mass ratio of ascorbic acid to add ascorbic acid
: 12), 2h is stirred with the rotating speed of 100r/min at 55 DEG C, complete Graphene coating, after washing is dried, repeat this dipping reduction
Process 8 times, finally gives Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.994g/cm to fiber prepared by the method3, resistivity is 105Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature5Ω/cm, that is, resistivity is constant before and after cleaning.
Embodiment 11：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,2.50g graphene oxides are added in 500mL nmp solutions, mechanical agitation 30min, ultrasonically treated 40min；Afterwards
Activated fiber is immersed in graphene oxide dispersion, (graphene oxide is 1 with the mass ratio of ascorbic acid to add ascorbic acid
: 15), 5h is stirred with the rotating speed of 200r/min at 60 DEG C, complete Graphene coating, after washing is dried, repeat this dipping reduction
Process 4 times, finally gives Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 1.013g/cm to fiber prepared by the method3, resistivity is 106Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature8Ω/cm, that is, 100 times before cleaning.
Embodiment 12：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,0.25g graphene oxides are added in 500mL DMF, mechanical agitation 20min, ultrasonically treated 20min；Afterwards will be living
In chemical fibre dimension immersion graphene oxide dispersion, hydroiodic acid (graphene oxide is 1: 20 with the mass ratio of hydroiodic acid) is added,
3h is stirred with the rotating speed of 100r/min at 65 DEG C, Graphene coating is completed, after washing is dried, this dipping reduction process is repeated 7 times,
Finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.978g/cm to fiber prepared by the method3, resistivity is 107Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature8Ω/cm, that is, 10 times before cleaning.
Embodiment 13：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,1.25g graphene oxides are added in 500mL DMF, mechanical agitation 30min, ultrasonically treated 40min；Afterwards will be living
In chemical fibre dimension immersion graphene oxide dispersion, hydroiodic acid (graphene oxide is 1: 30 with the mass ratio of hydroiodic acid) is added,
4h is stirred with the rotating speed of 200r/min at 75 DEG C, Graphene coating is completed, after washing is dried, this dipping reduction process is repeated 9 times,
Finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.997g/cm to fiber prepared by the method3, resistivity is 105Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature6Ω/cm, that is, 10 times before cleaning.
Embodiment 14：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,2.50g graphene oxides are added in 500mL DMF, mechanical agitation 30min, ultrasonically treated 40min；Afterwards will be living
In chemical fibre dimension immersion graphene oxide dispersion, hydroiodic acid (graphene oxide is 1: 40 with the mass ratio of hydroiodic acid) is added,
5h is stirred with the rotating speed of 200r/min at 80 DEG C, Graphene coating is completed, after washing is dried, this dipping reduction process is repeated 7 times,
Finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 1.016g/cm to fiber prepared by the method3, resistivity is 105Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 100 times before cleaning.
Embodiment 15：
The Tris-HCl cushioning liquid that 500mL pH are 9 is measured, 1g dopamines (as shown in table 2) is added, stirred, plus
Enter UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1, stand reaction 24h, obtain activated fiber；Then such as table 3
It is shown, 2.50g graphene oxides are added in 500mL deionized waters, mechanical agitation 30min, ultrasonically treated 40min；Afterwards
Activated fiber is immersed in graphene oxide dispersion, (graphene oxide is 1 with the mass ratio of sodium peroxydisulfate to add sodium peroxydisulfate
: 10), 3h is stirred with the rotating speed of 200r/min at 90 DEG C, complete Graphene coating, after washing is dried, repeat this dipping reduction
Process 5 times, finally gives Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.991g/cm to fiber prepared by the method3, resistivity is 107Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature9Ω/cm, that is, 100 times before cleaning.
Embodiment 16：
The Tris-HCl cushioning liquid that 500mL pH are 9 is measured, 1g dopamines (as shown in table 2) is added, stirred, plus
Enter UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1, stand reaction 24h, obtain activated fiber；Then such as table 3
It is shown, 1.25g graphene oxides are added in 500mL deionized waters, mechanical agitation 30min, ultrasonically treated 30min；Afterwards
Activated fiber is immersed in graphene oxide dispersion, glucose (graphene oxide is 1: 8 with the mass ratio of glucose) is added,
4h is stirred with the rotating speed of 200r/min at 75 DEG C, Graphene coating is completed, after washing is dried, this dipping reduction process 10 is repeated
It is secondary, finally give Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 0.998g/cm to fiber prepared by the method3, resistivity is 103Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature5Ω/cm, that is, 100 times before cleaning.
Embodiment 17：
The Tris-HCl cushioning liquid that 500mL pH are 8.5 is measured, 1g dopamines (as shown in table 2) is added, stirred,
UHMWPE fibers (through the ultrasonically treated 1h of acetone) as shown in table 1 are added, reaction 24h is stood, activated fiber is obtained；Then such as table
Shown in 3,2.50g graphene oxides are added in 500mL deionized waters, mechanical agitation 30min, ultrasonically treated 40min；Afterwards
Activated fiber is immersed in graphene oxide dispersion, addition glucose (graphene oxide is 1 with the mass ratio of glucose:
12) 1h, is stirred with the rotating speed of 200r/min at 90 DEG C, Graphene coating is completed, after washing is dried, this dipping is repeated and was reduced
Journey 7 times, finally gives Graphene coating UHMWPE fibers.
As shown in table 4, its Midst density is 1.009g/cm to fiber prepared by the method3, resistivity is 106Ω/cm, fiber jail
Spend and be：Resistivity is changed into 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 10 times before cleaning.
Claims (10)
1. a kind of antistatic superhigh molecular weight polyethylene fibers of lightweight, density is 0.97~1.03g/cm3, a diameter of 15~25 μm,
Intensity is 30~40cN/dtex, and modulus is 800~1600cN/dtex, and elongation at break is 2.5%~4.5%, sheet resistance
Rate is 103~1010Ω/cm, surface carbon oxygen atom ratio is 4:1~10:1, it is characterised in that fine including ultra-high molecular weight polyethylene
Wiki layer, dopamine active layer and partial reduction graphene layer；Wherein dopamine active layer is attached at substrate surface, partial reduction
Graphene layer is attached at dopamine activation layer surface in lamella deployed condition；
The mass content of described partial reduction graphene layer is 0.1~5%, and carbon oxygen atom ratio is 5:1~10:1, sheet surfaces
Size is 0.1~2 μm, and the lamella number of plies is 1~10 layer.
2. a kind of antistatic superhigh molecular weight polyethylene fibers of lightweight as claimed in claim 1, it is characterised in that described is more
Bar amine active layer mass content is 0.01~1.0%, and carbon oxygen atom ratio is 4:1~6:1；
Described partial reduction graphene layer is 500 with the mass ratio of dopamine active layer:1~0.1:1.
3. a kind of preparation method of the antistatic superhigh molecular weight polyethylene fibers of lightweight as claimed in claim 1, its feature exists
In comprising the concrete steps that for the method：
Step (1), the preparation of graphene oxide dispersion：
Graphene oxide powder is added in decentralized medium under normal temperature, first 20~30min of mechanical agitation, mixing speed is 500
~800r/min, then ultrasonically treated 20~40min in ice-water bath, obtain uniform and stable graphene oxide dispersion；
Step (2), the cleaning of UHMWPE fibers：UHMWPE fibers are cleaned by ultrasonic 0.5~1.5h in a solvent at normal temperatures, are taken
Go out stand-by after drying；
Step (3), the preparation of activated fiber：In three (methylol) aminomethane-hydrochloric acid (Tris-HCl) bufferings that pH is 8~11
Dopamine is added in solution, dopamine solution is obtained；The fiber after step (2) treatment is added in above-mentioned dopamine solution again,
8~24h of reaction is stood, washing obtains dopamine activation UHMWPE fibers after drying；
The preparation of step (4), the antistatic UHMWPE of lightweight：The activated fiber that step 3 is obtained is immersed in the oxygen that step (1) is obtained
In graphite alkene dispersion, reducing agent is added, 1~5h is stirred with the rotating speed of 100~500r/min at 50~95 DEG C, so
Fiber wash is dried afterwards, repeats this dipping reduction process 2~10 times, obtained partial reduction Graphene coating super high molecular weight and gather
Vinyl fiber.
4. method as claimed in claim 3, it is characterised in that step (1) graphene oxide powder is decentralized medium weight
0.01~1%；UHMWPE fibers and the mass ratio of dopamine solution described in step (3) are 2~10%；Step (4) described oxygen
Graphite alkene is 1 with the mass ratio of reducing agent:0.5~1:40.
5. method as claimed in claim 3, it is characterised in that the carbon oxygen atom ratio of the graphene oxide described in step (1) is 2:
1~4:1, sheet surfaces size is 0.1~2 μm, and the lamella number of plies is 1~10 layer.
6. method as claimed in claim 3, it is characterised in that the molecular weight of the UHMWPE fibers described in step (2) is 100~
3000000, density is 0.973g/cm3, a diameter of 15~25 μm, intensity is 30~40cN/dtex, and modulus is 800~1600cN/
Dtex, elongation at break is 2.5%~4.5%, and surface resistivity is 1012~1016Ω/cm；Surface carbon oxygen atom ratio is 10:1
~1000:1.
7. method as claimed in claim 6, it is characterised in that a diameter of 20~23 μm of step (2) UHMWPE fibers, surface
Carbon oxygen atom ratio is 100:1~1000:1.
8. method as claimed in claim 3, it is characterised in that the dopamine described in step (3) is catecholamines or diphenylquinone
One or two mixture in class compound, structural formula is as follows：
Wherein R be with amino group-(CHy)x-NH2Or-(CHy)x-NH-(CHq)p-CH3Or-(CH2)x-NH-(CO)x-
(CH2)P-CH3Or-(CH2)x-NH-(CO)x-(CH2)P-C6H5Or-(CH2)x-NH2Or-(CHy)x-N(CHj)h-(CHq)p-(CH3)e
Or-CHOH-NH- (CH2)p-CH3Or-CHOH- (CH2)x-NH2, wherein x is 1~99 natural number, and p, h are 0~99 nature
Number, y, q, e are 1 or 2, j are 1,2 or 3.
9. method as claimed in claim 8, it is characterised in that the dopamine described in step (3) is catecholamines or diphenylquinone
One or two mixture in class compound, structural formula is as follows：
Wherein R is
N is 1~10 natural number.
10. method as claimed in claim 3, it is characterised in that step (4) described reducing agent be ammoniacal liquor, hydrazine hydrate, hydroiodic acid,
One or two mixture in sodium borohydride, ascorbic acid, sodium peroxydisulfate, glucose.
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