CN106854833B - A kind of antistatic ultra high molecular weight polyethylene fiber of lightweight and preparation method thereof - Google Patents
A kind of antistatic ultra high molecular weight polyethylene fiber of lightweight and preparation method thereof Download PDFInfo
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- CN106854833B CN106854833B CN201611260080.XA CN201611260080A CN106854833B CN 106854833 B CN106854833 B CN 106854833B CN 201611260080 A CN201611260080 A CN 201611260080A CN 106854833 B CN106854833 B CN 106854833B
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- 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
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Abstract
The present invention discloses a kind of antistatic ultra high molecular weight polyethylene fiber of lightweight and preparation method thereof.Fiber of the present invention includes high molecular weight polyethylene fiber base, the partial reduction graphene layer for investing the dopamine active layer of substrate surface and being attached at dopamine activation layer surface in lamella unfolded state.The present invention obtains the antistatic ultra high molecular weight polyethylene fiber of lightweight by the decentralized medium and dispersion liquid concentration of preferred graphene oxide, reducing agent type and dipping time.Utilize the characteristic of partial reduction graphene: 1) carbon oxygen atom ratio, suitable oxygen-containing group can guarantee section reduced graphene and the modified fiber of dopamine sufficiently strong interaction occurs, while providing enough electric conductivity；2) the lamella number of plies influences it and stablizes absorption on fiber；3) slice plane size influences coating and conductive path of the lamella in fiber surface.
Description
Technical field
The invention belongs to technical field of polymer materials, be related to a kind of antistatic ultra high molecular weight polyethylene fiber of lightweight and
Preparation method.
Background technique
Ultra-high molecular weight polyethylene (UHMWPE) fiber and carbon fiber, aramid fiber and referred to as the big high-performance in the world three is fine
Dimension is most important in national defense industry and protective gear field.UHMWPE fiber is in addition to high intensity, modulus, density
Lower (about 0.97g/cm3), be the high-performance fiber that uniquely may float on the water surface, at the same have shock resistance, it is corrosion-resistant,
Wear-resistant equal excellent properties.However, due to the dielectric constant of UHMWPE fiber low (2.4), resistance height (> 1014Ω), it is applying
When antistatic property it is poor.UHMWPE fiber is in elevated chemical inertia, and surface is extremely smooth, and being modified to it is also this field
One of great difficult problem.
Antistatic coating fiber type refers to using fiber as matrix, is solidificated in one layer of conduction of fiber surface absorption by coating and fills 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, the disadvantages such as thus bring unit resource benefit low.The Chinese invention patent of Publication No. CN102277728 is (close using silver
Degree is 10.49g/cm3) be conducting particles, using silver ammino solution as silver plating liquid, it is silver-plated it is preceding by fiber carry out slurry and surface active
Processing, finally obtains a kind of conductive UHMWPE fiber, wherein fibre density is from when line resistance is about 0.15 Ω/cm
0.97g/cm before reason3The about 1.92g/cm that becomes that treated3(density increase about 95%).The China of Publication No. CN1693576
Patent of invention deoils to fabric, is roughened, striping, sensitization, after the pre-treatments such as activation, once being changed using 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 surface resistance are 0.03 Ω/, and conductive fabric surface density is from 55g/cm2Increase to
111g/cm2(density increase about 102%).
In order to obtain same even higher benefit from less resource, exploitation lightweight antistatic fibre just seems very
It is significant.And graphene has lower density (based on graphite: 2.25g/cm as a kind of New Type of Carbon nanometer super light material3)、
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.Graphene is used as conductive coating in use, can be in irreducible minimum
Under 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 using dip dyeing technique preparation and its preparation method and application, fabric is subjected to base extraction, pretreatment, assisting-dyeing
Agent immersion and graphene aqueous dispersions dipping, are adsorbed onto fabric surface for conducting particles under ultrasonication, graphite in the fabric
The mass percent of alkene be 3.5%, fabric from insulate become conductivity be 3.6 × 102S/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 silane coupling agent surface activation process, be immersed in the graphene aqueous solution containing dispersing agent (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 of order of magnitude.
Metal coating and graphite ene coatings are compared for the improvement degree of fiber or fabric electric conductivity, it is not difficult to find that stone
Black alkene can be more favorable for the promotion of materials conductive performance under the conditions of identical weight gain, 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 removing of piece interlayer difficulty and coating is easy
Obscission seriously hinders the performance of its electrical-conductive nanometer material advantage.Graphene is especially applied to UHMWPE fiber
When surface treatment, since UHMWPE fiber is in elevated chemical inertia, surface is extremely smooth, and graphene sheet layer is caused to be difficult
UHMWPE fiber surface is evenly distributed and combines closely.Therefore, it is above-mentioned to solve to be badly in need of research new material system and method
Problem, and the antistatic UHMWPE fiber of lightweight is produced in a manner of economically viable.
Summary of the invention
The first purpose of the invention is to provide a kind of antistatic ultra high molecular weight polyethylene fibers of lightweight.
The antistatic ultra high molecular weight polyethylene fiber of lightweight includes high molecular weight polyethylene fiber base, dopamine work
Change layer and partial reduction graphene layer (being referred to as graphene antistatic layer)；Wherein dopamine active layer is attached at base's table
Face, partial reduction graphene layer are attached at dopamine activation layer surface in lamella unfolded state.
The density of the antistatic ultra high molecular weight polyethylene fiber of the lightweight is 0.97~1.03g/cm3, diameter 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 are 4: 1~10: 1；(surface carbon oxygen atom herein is than referring to
UHMWPE+ dopamine+graphene carbon oxygen atom ratio)；
The dopamine active layer mass content is 0.01%~1.0%, and carbon oxygen atom ratio is 4: 1~6: 1；
The mass content of the partial reduction graphene layer is 0.1%~5%, and carbon oxygen atom is than 5: 1~10: 1, lamella
Surface size is 0.1~2 μm, and the lamella number of plies is 1~10 layer；The matter of the partial reduction graphene layer and dopamine active layer
Amount is than being 500: 1~0.1: 1；
After being cleaned by ultrasonic 2h in the water of the antistatic ultra high molecular weight polyethylene fiber of the lightweight at room temperature, surface
Resistivity is 1~100 times before cleaning.
A second object of the present invention is to provide a kind of preparation method of the antistatic ultra high molecular weight polyethylene fiber of lightweight,
This method comprises the concrete steps that:
The preparation of step (1), graphene oxide dispersion:
Graphene oxide powder is added in decentralized medium under room temperature, first 20~30min of mechanical stirring, stirring rate is
500~800r/min, then 20~40min is ultrasonically treated 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 the graphene oxide is 2: 1~4: 1, and sheet surfaces are having a size of 0.1~2 μm, and piece is layer by layer
Number is 1~10 layer；
The decentralized medium is in water, ethylene glycol, N-Methyl pyrrolidone (NMP) and dimethylformamide (DMF)
One or two kinds of mixtures；
Preferably, the graphene oxide is the 0.05%~0.5% of decentralized medium weight；
Preferably, the pH value of the graphene oxide decentralized medium is 8~12；
The cleaning of step (2), UHMWPE fiber: UHMWPE fiber is cleaned by ultrasonic 0.5 in a solvent at room temperature~
1.5h, it is stand-by after taking-up is dry；The solvent is the mixture of one or both of ethyl alcohol, acetone and tetrahydrofuran；
The molecular weight of the UHMWPE fiber is 100~3,000,000, density 0.97g/cm3, diameter is 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, the diameter of UHMWPE fiber is 20~23 μm, carbon oxygen atom ratio in surface is 100: 1~1000: 1；
The preparation of step (3), activated fiber: three (methylol) aminomethane-hydrochloric acid (Tris-HCl) for being 8~11 in pH
Dopamine is added in buffer solution, obtains dopamine solution；It is added step 2 in above-mentioned dopamine solution again treated and is fine
Dimension, standing reaction 8~for 24 hours, dopamine activation UHMWPE fiber is obtained after washing is dry；
The dopamine is the mixture of one or both of 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, the natural number that wherein x is 1~99, the nature that p, h are 0~99
Number, y, q, e are 1 or 2, j 1,2 or 3；
Preferably, R is The natural number that n is 1~10；
Preferably, the pH of the Tris-HCl buffer solution is 8~10；
Preferably, the mass concentration of the dopamine solution is 0.1%~0.3%；
The mass ratio of the UHMWPE fiber and dopamine solution is 2%~10%；
The surface carbon oxygen atom ratio of the dopamine activation UHMWPE fiber is 4: 1~8: 1；(surface carbon oxygen is former herein
Carbon oxygen atom ratio of the son than referring to UHMWPE+ dopamine)；
The preparation of step (4), the antistatic UHMWPE of lightweight: the activated fiber that step (3) obtains is immersed in step (1) and is obtained
To graphene oxide dispersion in, add reducing agent, at 50~95 DEG C with the revolving speed of 100~500r/min stirring 1~
5h, it is then that fiber wash is dry, it repeats this dipping reduction process 2~10 times, obtains partial reduction graphene coating superelevation point
Sub- weight polyethylene fiber；
The reducing agent is ammonium hydroxide, in hydrazine hydrate, hydroiodic acid, sodium borohydride, ascorbic acid, sodium peroxydisulfate, glucose
One or two kinds of mixtures.
The mass ratio of the graphene oxide and reducing agent is 1: 0.5~1: 40；
In the graphene coating ultra high molecular weight polyethylene fiber, graphene content is 0.1%~5%, fiber surface
Carbon oxygen atom ratio is 4: 1~10: 1, and for graphene sheet layer having a size of 0.1~2 μm, 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 type and dipping time,
Obtain the antistatic ultra high molecular weight polyethylene fiber of lightweight.Utilize the characteristic of partial reduction graphene: 1) carbon oxygen atom ratio, in right amount
Oxygen-containing group can guarantee section reduced graphene and the modified fiber of dopamine sufficiently strong interaction occurs, simultaneously
Enough electric conductivity is provided；2) when the number of plies of the lamella number of plies, partial reduction graphene is excessively high, unit volume graphene number can be reduced
Amount, and then be unfavorable for its and stablize absorption on fiber, the and when number of plies of partial reduction graphene is too low then easily occurs from rolling up
It contracts and is unfavorable for being fully extended in UHMWPE fiber surface, and then drop low-fiber electric conductivity；3) slice plane size is fitted
Suitable slice plane size not only contributes to lamella in the coating of fiber surface, and is conducive to the formation of conductive path；4) divide
The oxygen-containing group of powder, graphene oxide is uniformly dispersed it in polar solvent, reduces the reunion between lamella, is conducive to
It is fully contacted with fiber；In addition, reducing agent type is by influencing reducing degree (the i.e. graphene surface of graphene oxide
Carbon oxygen atom ratio), and then change the binding force size of graphene and activated fiber surface, the final density and conduction for influencing fiber
Performance.Meanwhile dipping time determine fiber surface absorption graphene quantity number, so also direct fibre property.In short,
The present invention obtains the light of good antistatic property by the dispersion liquid of preferred graphene oxide, reducing agent type and dipping time
Matter ultra-high molecular weight fibers.
Detailed description of the invention
Fig. 1 is the electron microscope of ultra high molecular weight polyethylene fiber；
Fig. 2 is the electron microscope of activated fiber；
Fig. 3 is the electron microscope that graphene coats ultra high molecular weight polyethylene fiber.
Specific embodiment
Technical solution of the present invention and effect are further described below 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 cannot be interpreted as to the scope of the present invention
It limits.
The calculation method of fibre density described in the present embodiment are as follows: UHMWPE fibre density is 0.973g/cm3, diameter is
15~25 μm, surface resistivity 1012~1016The diameter (as shown in Figure 1) of Ω/cm, UHMWPE fiber is in activation (such as Fig. 2 institute
Show) and graphene coating it is (as shown in Figure 3) front and back be held essentially constant, pass through weigh a fixed length coating after fiber weight calculating
And it obtains.
Comparative example 1:
The Tris-HCl buffer solution that 500mL pH is 10 is measured, 1g dopamine is added, is stirring evenly and then adding into UHMWPE
Fiber (is ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtains activated fiber；Then into 1.0% silver nitrate solution, side is dripped
Waterside stirring is ammoniated, is by volume later that 1: 1 mixing is equal by itself and 5.0% potassium sodium tartrate solution until solution becomes clarification
It is even, form silver plating liquid；Finally activated fiber is immersed in silver plating liquid, 0.5h is reacted in shading at room temperature, obtains silver plated fiber.
The fibre density of the method preparation is 1.053g/cm3, resistivity 1010Ω/cm, fiber fastness are as follows: surpass at room temperature
Resistivity becomes 10 after sound cleaning 2h13Ω/cm, that is, 1000 times before cleaning.As it can be seen that right using dopamine processing UHMWPE fiber
Silver-plated afterwards, the resistivity of fiber reaches 10 after the usage amount of preferred silver makes processing10Ω/cm, density increase to 1.053g/
cm3, it is further reduced the usage amount of silver, the density of fiber reduces after processing, but resistivity is greater than 1010Ω/cm。
Comparative example 2:
The Tris-HCl buffer solution that 500mL pH is 9 is measured, 1g dopamine is added, is stirring evenly and then adding into UHMWPE fibre
It ties up (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then into 3.8% silver nitrate solution, side is added dropwise
Ammonium hydroxide side stirring, until solution become clarification, later by itself and 17% potassium sodium tartrate solution be by volume 1: 1 be uniformly mixed,
Form silver plating liquid；Finally activated fiber is immersed in silver plating liquid, 0.5h is reacted in shading at room temperature, obtains silver plated fiber.
The fibre density of the method preparation is 1.102g/cm3, resistivity 104Ω/cm, fiber fastness are as follows: surpass at room temperature
Resistivity becomes 10 after sound cleaning 2h7Ω/cm, that is, 1000 times before cleaning.As it can be seen that right using dopamine processing UHMWPE fiber
Silver-plated afterwards, although declining the resistivity of fiber, fibre density is higher, and the fastness of silver coating is insufficient.
Comparative example 3:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, 1g dopamine is added, is stirring evenly and then adding into UHMWPE
Fiber (is ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtains activated fiber；Then into 3.8% silver nitrate solution, side is dripped
Waterside stirring is ammoniated, is by volume later that 1: 1 mixing is equal by itself and 17% potassium sodium tartrate solution until solution becomes clarification
It is even, form silver plating liquid；Finally activated fiber is immersed in silver plating liquid, 8h is reacted in shading at room temperature, obtains silver plated fiber.
The fibre density of the method preparation is 1.943g/cm3, resistivity is≤1.0 Ω/cm, fiber fastness are as follows: at room temperature
Resistivity becomes 10 after ultrasonic cleaning 2h7Ω/cm, that is, 10 before cleaning7Times.As it can be seen that right using dopamine processing UHMWPE fiber
Silver-plated afterwards, when the usage amount of silver is higher, although declining the resistivity of fiber effectively, fibre density is sharply increased, and is plated
The fastness of silver layer is insufficient.
Comparative example 4:
Graphene oxide 1.25g is taken to be added in 500mL deionized water, mechanical stirring 30min is ultrasonically treated 30min；It will
UHMWPE fiber (being ultrasonically treated 1h through acetone) immerses in graphene oxide dispersion, and it is 9 that ammonium hydroxide, which is added, and adjusts pH, adds water
Hydrazine (mass ratio of graphene oxide and hydrazine hydrate is 10: 7) is closed, 3h is stirred with the revolving speed of 200r/min at 95 DEG C, completes stone
Black alkene coating, repeats this dipping reduction process 8 times, obtains graphene coating UHMWPE fiber.
The fibre density of the method preparation is 0.976g/cm3, resistivity 1011Ω/cm, fiber fastness are as follows: surpass at room temperature
Resistivity becomes 10 after sound cleaning 2h14Ω, that is, 1000 times before cleaning.As it can be seen that UHMWPE fiber is coated using graphene, although
Decline the resistivity of fiber, and density keeps lower, but the fastness of graphene coat is insufficient.
Embodiment 1:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,0.05g graphene oxide is added in 500mL deionized water, mechanical stirring 20min, is ultrasonically treated 20min；Later
By activated fiber immerse graphene oxide dispersion in, be added ammonium hydroxide adjust pH be 9, add hydrazine hydrate (graphene oxide with
The mass ratio of hydrazine hydrate is 10: 5), stirring 2h at 50 DEG C with the revolving speed of 100r/min, complete graphene coating, wash drying
Afterwards, it repeats this dipping reduction process 6 times, finally obtains graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.976g/cm3, surface resistivity 108Ω/cm, it is fine
Tie up fastness are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature9Ω/cm, that is, 10 times before cleaning.
Embodiment 2:
The Tris-HCl buffer solution that 500mL pH is 10 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,0.25g graphene oxide is added in 500mL deionized water, mechanical stirring 20min, is ultrasonically treated 20min；Later
By activated fiber immerse graphene oxide dispersion in, be added ammonium hydroxide adjust pH be 9, add hydrazine hydrate (graphene oxide with
The mass ratio of hydrazine hydrate is 10: 5), stirring 3h at 70 DEG C with the revolving speed of 100r/min, complete graphene coating, wash drying
Afterwards, it repeats this dipping reduction process 5 times, finally obtains graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.977g/cm3, surface resistivity 108Ω/cm,
Fiber fastness are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature10Ω/cm, that is, 100 times before cleaning.
Embodiment 3:
The Tris-HCl buffer solution that 500mL pH is 9 is measured, is added 1g dopamine (as shown in table 2), is stirred evenly, add
Enter UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table 3
It is shown, 1.25g graphene oxide is added in 500mL ml deionized water, mechanical stirring 30min, is ultrasonically treated 30min；
Activated fiber is immersed in graphene oxide dispersion later, it is 10 that ammonium hydroxide, which is added, and adjusts pH, adds hydrazine hydrate (graphite oxide
The mass ratio of alkene and hydrazine hydrate is 10: 7), stirring 2h at 85 DEG C with the revolving speed of 300r/min, complete graphene coating, washing
After drying, this dipping is repeated reduction process 7 times, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.991g/cm3, surface resistivity 106Ω/cm, it is fine
Tie up fastness are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 10 times before cleaning.
Embodiment 4:
The Tris-HCl buffer solution that 500mL pH is 10 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,2.50g graphene oxide is added in 500mL deionized water, mechanical stirring 30min, is ultrasonically treated 30min；Later
By activated fiber immerse graphene oxide dispersion in, be added ammonium hydroxide adjust pH be 11, add hydrazine hydrate (graphene oxide with
The mass ratio of hydrazine hydrate is 10: 10), stirring 5h at 95 DEG C with the revolving speed of 200r/min, complete graphene coating, wash drying
Afterwards, it repeats this dipping reduction process 4 times, finally obtains graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.998g/cm3, surface resistivity 106Ω/cm, it is fine
Tie up fastness are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature8Ω/cm, that is, 100 times before cleaning.
Embodiment 5:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,5.00g graphene oxide is added in 500mL deionized water, mechanical stirring 30min, is ultrasonically treated 40min；Later
By activated fiber immerse graphene oxide dispersion in, be added ammonium hydroxide adjust pH be 10, add hydrazine hydrate (graphene oxide with
The mass ratio of hydrazine hydrate is 10: 10), stirring 3h at 95 DEG C with the revolving speed of 500r/min, complete graphene coating, wash drying
Afterwards, it repeats this dipping reduction process 8 times, finally obtains graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 1.023g/cm3, surface resistivity 104Ω/cm, it is fine
Tie up fastness are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature6Ω/cm, that is, 100 times before cleaning.
Embodiment 6:
The Tris-HCl buffer solution that 500mL pH is 9.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,0.25g graphene oxide is added in 500mL ethylene glycol, mechanical stirring 20min, is ultrasonically treated 20min；Later will
Activated fiber immerses in graphene oxide dispersion, addition sodium borohydride (mass ratio of graphene oxide and sodium borohydride is 1:
4) 2h, is stirred with the revolving speed of 200r/min at 65 DEG C, completes graphene coating, after washing is dry, this dipping is repeated and restored
Journey 8 times, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.979g/cm3, resistivity 107Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 1 times before cleaning.
Embodiment 7:
The Tris-HCl buffer solution that 500mL pH is 9.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,1.25g graphene oxide is added in 500mL ethylene glycol, mechanical stirring 30min, is ultrasonically treated 30min；Later will
Activated fiber immerses in graphene oxide dispersion, addition sodium borohydride (mass ratio of graphene oxide and sodium borohydride is 1:
6) 4h, is stirred with the revolving speed of 100r/min at 75 DEG C, completes graphene coating, after washing is dry, this dipping is repeated and restored
Journey 5 times, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.989g/cm3, resistivity 106Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 10 times before cleaning.
Embodiment 8:
The Tris-HCl buffer solution that 500mL pH is 9 is measured, is added 1g dopamine (as shown in table 2), is stirred evenly, add
Enter UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table 3
It is shown, 2.50g graphene oxide is added in 500mL deionized water, mechanical stirring 30min, is ultrasonically treated 40min；Later
Activated fiber is immersed in graphene oxide dispersion, sodium borohydride is added, and (mass ratio of graphene oxide and sodium borohydride is 1
: 8), 5h is stirred with the revolving speed of 200r/min at 90 DEG C, after washing is dry, repeats this dipping reduction process 5 times；Again by fiber
Immerse in graphene oxide dispersion, glucose (mass ratio of graphene oxide and glucose be 1: 8) be added, at 90 DEG C with
The revolving speed of 200r/min stirs 5h, completes graphene coating, after washing is dry, repeats this dipping reduction process 5 times, finally obtains
Graphene coats UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 1.023g/cm3, resistivity 104Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature5Ω/cm, that is, 10 times before cleaning.
Embodiment 9:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,0.25g graphene oxide is added in 500mL nmp solution, mechanical stirring 20min, is ultrasonically treated 20min；Later
Activated fiber is immersed in graphene oxide dispersion, ascorbic acid is added, and (mass ratio of graphene oxide and ascorbic acid is 1
: 10), 1h is stirred with the revolving speed of 100r/min at 50 DEG C, complete graphene coating, after washing is dry, repeats this dipping reduction
Process 2 times, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.975g/cm3, resistivity 1010Ω/cm, fiber
Fastness are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature10Ω/cm, that is, 1 times before cleaning.
Embodiment 10:
The Tris-HCl buffer solution that 500mL pH is 9 is measured, is added 1g dopamine (as shown in table 2), is stirred evenly, add
Enter UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table 3
It is shown, 1.25g graphene oxide is added in 500mL nmp solution, mechanical stirring 30min, is ultrasonically treated 30min；Later
Activated fiber is immersed in graphene oxide dispersion, ascorbic acid is added, and (mass ratio of graphene oxide and ascorbic acid is 1
: 12), 2h is stirred with the revolving speed of 100r/min at 55 DEG C, complete graphene coating, after washing is dry, repeats this dipping reduction
Process 8 times, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.994g/cm3, resistivity 105Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature5Ω/cm, i.e. cleaning front and back resistivity are constant.
Embodiment 11:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,2.50g graphene oxide is added in 500mL nmp solution, mechanical stirring 30min, is ultrasonically treated 40min；Later
Activated fiber is immersed in graphene oxide dispersion, ascorbic acid is added, and (mass ratio of graphene oxide and ascorbic acid is 1
: 15), 5h is stirred with the revolving speed of 200r/min at 60 DEG C, complete graphene coating, after washing is dry, repeats this dipping reduction
Process 4 times, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 1.013g/cm3, resistivity 106Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature8Ω/cm, that is, 100 times before cleaning.
Embodiment 12:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,0.25g graphene oxide is added in 500mL DMF, mechanical stirring 20min, is ultrasonically treated 20min；It will live later
Chemical fibre dimension immerses in graphene oxide dispersion, and hydroiodic acid (mass ratio of graphene oxide and hydroiodic acid is 1: 20) is added,
3h is stirred with the revolving speed of 100r/min at 65 DEG C, completes graphene coating, after washing is dry, repeats this dipping reduction process 7 times,
Finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.978g/cm3, resistivity 107Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature8Ω/cm, that is, 10 times before cleaning.
Embodiment 13:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,1.25g graphene oxide is added in 500mL DMF, mechanical stirring 30min, is ultrasonically treated 40min；It will live later
Chemical fibre dimension immerses in graphene oxide dispersion, and hydroiodic acid (mass ratio of graphene oxide and hydroiodic acid is 1: 30) is added,
4h is stirred with the revolving speed of 200r/min at 75 DEG C, completes graphene coating, after washing is dry, repeats this dipping reduction process 9 times,
Finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.997g/cm3, resistivity 105Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature6Ω/cm, that is, 10 times before cleaning.
Embodiment 14:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,2.50g graphene oxide is added in 500mL DMF, mechanical stirring 30min, is ultrasonically treated 40min；It will live later
Chemical fibre dimension immerses in graphene oxide dispersion, and hydroiodic acid (mass ratio of graphene oxide and hydroiodic acid is 1: 40) is added,
5h is stirred with the revolving speed of 200r/min at 80 DEG C, completes graphene coating, after washing is dry, repeats this dipping reduction process 7 times,
Finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 1.016g/cm3, resistivity 105Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 100 times before cleaning.
Embodiment 15:
The Tris-HCl buffer solution that 500mL pH is 9 is measured, is added 1g dopamine (as shown in table 2), is stirred evenly, add
Enter UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table 3
It is shown, 2.50g graphene oxide is added in 500mL deionized water, mechanical stirring 30min, is ultrasonically treated 40min；Later
Activated fiber is immersed in graphene oxide dispersion, sodium peroxydisulfate is added, and (mass ratio of graphene oxide and sodium peroxydisulfate is 1
: 10), 3h is stirred with the revolving speed of 200r/min at 90 DEG C, complete graphene coating, after washing is dry, repeats this dipping reduction
Process 5 times, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.991g/cm3, resistivity 107Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature9Ω/cm, that is, 100 times before cleaning.
Embodiment 16:
The Tris-HCl buffer solution that 500mL pH is 9 is measured, is added 1g dopamine (as shown in table 2), is stirred evenly, add
Enter UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table 3
It is shown, 1.25g graphene oxide is added in 500mL deionized water, mechanical stirring 30min, is ultrasonically treated 30min；Later
Activated fiber is immersed in graphene oxide dispersion, glucose (mass ratio of graphene oxide and glucose is 1: 8) is added,
4h is stirred with the revolving speed of 200r/min at 75 DEG C, completes graphene coating, after washing is dry, repeats this dipping reduction process 10
It is secondary, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 0.998g/cm3, resistivity 103Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature5Ω/cm, that is, 100 times before cleaning.
Embodiment 17:
The Tris-HCl buffer solution that 500mL pH is 8.5 is measured, is added 1g dopamine (as shown in table 2), stirs evenly,
It is added UHMWPE fiber as shown in Table 1 (being ultrasonically treated 1h through acetone), stands reaction for 24 hours, obtain activated fiber；Then such as table
Shown in 3,2.50g graphene oxide is added in 500mL deionized water, mechanical stirring 30min, is ultrasonically treated 40min；Later
Activated fiber is immersed in graphene oxide dispersion, addition glucose (mass ratio of graphene oxide and glucose is 1:
12) 1h, is stirred with the revolving speed of 200r/min at 90 DEG C, completes graphene coating, after washing is dry, this dipping is repeated and restored
Journey 7 times, finally obtain graphene coating UHMWPE fiber.
The fiber of the method preparation is as shown in table 4, and wherein density is 1.009g/cm3, resistivity 106Ω/cm, fiber jail
Degree are as follows: resistivity becomes 10 after being cleaned by ultrasonic 2h at room temperature7Ω/cm, that is, 10 times before cleaning.
Claims (10)
1. a kind of antistatic ultra high molecular weight polyethylene fiber of lightweight, density is 0.97~1.03g/cm3, diameter is 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 are 4:1~10:1, it is characterised in that including ultra-high molecular weight polyethylene fibre
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 unfolded state；
The mass content of the partial reduction graphene layer is 0.1~5%, and carbon oxygen atom ratio is 5:1~10:1, sheet surfaces
Having a size of 0.1~2 μm, the lamella number of plies is 1~10 layer.
2. a kind of antistatic ultra high molecular weight polyethylene fiber of lightweight as described 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；
The mass ratio of the partial reduction graphene layer and dopamine active layer is 500:1~0.1:1.
3. a kind of preparation method of the antistatic ultra high molecular weight polyethylene fiber of lightweight as described in claim 1, feature exist
In comprising the concrete steps that for this method:
The preparation of step (1), graphene oxide dispersion:
Graphene oxide powder is added in decentralized medium under room temperature, first 20~30min of mechanical stirring, mixing speed 500
~800r/min, then 20~40min is ultrasonically treated in ice-water bath, obtain uniform and stable graphene oxide dispersion；
The cleaning of step (2), UHMWPE fiber: at normal temperature UHMWPE fiber is cleaned by ultrasonic 0.5~1.5h in a solvent, taken
It is stand-by after drying out；
The preparation of step (3), activated fiber: it is buffered in three (methylol) aminomethane-hydrochloric acid (Tris-HCl) that pH is 8~11
Dopamine is added in solution, obtains dopamine solution；The fiber that is added that step (2) treated in above-mentioned dopamine solution again,
Standing reaction 8~for 24 hours, dopamine activation UHMWPE fiber is obtained after washing is dry；
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) obtains
In graphite alkene dispersion, reducing agent is added, 1~5h is stirred with the revolving speed of 100~500r/min at 50~95 DEG C, so
It is afterwards that fiber wash is dry, it repeats this dipping reduction process 2~10 times, it is poly- to obtain partial reduction graphene coating super high molecular weight
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 fiber described in step (3) and the mass ratio of dopamine solution are 2~10%；Step (4) described oxygen
The mass ratio of graphite alkene and reducing agent is 1:0.5~1:40.
5. method as claimed in claim 3, it is characterised in that the carbon oxygen atom ratio of graphene oxide described in step (1) is 2:
1~4:1, for sheet surfaces having a size of 0.1~2 μm, 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 UHMWPE fiber described in step (2) be 100~
3000000, density 0.973g/cm3, diameter is 15~25 μm, and intensity is 30~40cN/dtex, and modulus is 800~1600cN/
Dtex, elongation at break are 2.5%~4.5%, surface resistivity 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 the diameter of step (2) UHMWPE fiber is 20~23 μm, surface
Carbon oxygen atom ratio is 100:1~1000:1.
8. method as claimed in claim 3, it is characterised in that dopamine described in step (3) is catecholamines or diphenylquinone
The mixture of one or both of class compound, structural formula are 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, the natural number that wherein x is 1~99, the nature that p, h are 0~99
Number, y, q, e are 1 or 2, j 1,2 or 3.
9. method according to claim 8, it is characterised in that dopamine described in step (3) is catecholamines or diphenylquinone
The mixture of one or both of class compound, structural formula are as follows:
Wherein R is The natural number that n is 1~10.
10. method as claimed in claim 3, it is characterised in that step (4) reducing agent be ammonium hydroxide, hydrazine hydrate, hydroiodic acid,
The mixture of one or both of sodium borohydride, ascorbic acid, sodium peroxydisulfate, glucose.
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| CN109972387B (en) * | 2017-12-28 | 2022-06-14 | 青岛大学 | Graphene grafted modified conductive fiber and preparation method and application thereof |
| CN108126678B (en) * | 2017-12-29 | 2020-11-24 | 中国科学院宁波材料技术与工程研究所 | Renewable carbon nanomaterial coated fiber adsorbent and preparation method thereof |
| CN110552193B (en) * | 2018-05-31 | 2021-05-18 | 中国科学院化学研究所 | Modified ultrahigh molecular weight polyethylene fiber, fabric and preparation method and application thereof |
| CN108854162A (en) * | 2018-07-13 | 2018-11-23 | 北京欧美中科学技术研究院 | A kind of preparation method of the graphene composite material for water process |
| CN109281156B (en) * | 2018-07-19 | 2020-11-24 | 中国科学院宁波材料技术与工程研究所 | High-stability electrolyte corrosion-resistant conductive fiber and preparation method thereof |
| CN114381821B (en) * | 2022-03-01 | 2023-03-17 | 江苏清大际光新材料有限公司 | Graphene-containing conductive antibacterial nylon composite fiber and preparation method and application thereof |
| CN115232384B (en) * | 2022-08-25 | 2023-02-10 | 青岛优派普环保科技股份有限公司 | Antistatic PE gas pipe and preparation method thereof |
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