CN105862426B - A kind of enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide and preparation method thereof - Google Patents
A kind of enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide and preparation method thereof Download PDFInfo
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- CN105862426B CN105862426B CN201610265634.9A CN201610265634A CN105862426B CN 105862426 B CN105862426 B CN 105862426B CN 201610265634 A CN201610265634 A CN 201610265634A CN 105862426 B CN105862426 B CN 105862426B
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
- D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/53—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 sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/285—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acid amides or imides
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/35—Abrasion, pilling or fibrillation resistance
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
Abstract
The present invention relates to a kind of enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide and preparation method thereof, the mixed system being made up of organic resin, emulsifying agent, dispersant, compatible modified Nano lamella molybdenum disulfide, organic solvent and deionized water, wherein by percentage to the quality, emulsifying agent is the 0.5 5% of organic resin, dispersant is organic resin 0.1 0.5%, 0.05 1% that compatible modified Nano lamella molybdenum disulfide is organic resin, 20 200% that organic solvent is organic resin, gained mixed system solid content is 25 35%.The lubricity for the addition carbon fibre composite that sizing agent of the present invention passes through nanoscale twins molybdenum disulfide increases substantially, interface performance optimization, significant to carbon fibre composite industrial upgrading.
Description
Technical field
The invention belongs to technical field of composite materials, in more particularly to a kind of compatible modified Nano lamella molybdenum disulfide enhancing
Starch agent and preparation method thereof.
Background technology
Carbon fiber has high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, endurance, creep resistant, conduction, heat transfer and heat
A series of excellent properties such as the coefficient of expansion is small, are widely used in fiber-reinforced resin matrix compound material.But because carbon fiber is crisp
Property material, in production and process, phenomena such as lousiness and single wire fracture are easily produced through mechanical friction, make the strong of carbon fiber
Degree reduces.Due to the presence of lousiness, prevent matrix resin from fully soaking carbon fiber, thus can be in the composite of preparation
Hole is produced, influences the mechanical property of composite.On the other hand, the presence of fiber surface groove will be helpful to improve fiber with
The interfacial adhesion situation of resin, that is, contribute to the raising of composite material interface performance but the performance of carbon fiber in itself may be made
Decline, so that the combination property of composite declines.And problem above can preferably be solved by carrying out starching to carbon fiber.
In the production process of fiber, starching is one of them particularly important link.In recent years, nano material is due to its dimensional effect,
Big specific surface area and the interaction compared with strong interface are concerned by people as the modifying agent of sizing agent.
At present, sizing agent mainly has two kinds of solvent-borne type and emulsion-type.Solvent-borne type sizing agent is substantial amounts of organic molten due to needing
Agent, and workshop environmental pollution is serious, does not use already abroad.Emulsion-type sizing agent is then that a kind of resin is main body,
It is equipped with the emulsion that a certain amount of emulsifying agent and other auxiliary agents are formulated.With carbon fibre composite industry continuous development,
The performance requirement of sizing agent is also improved constantly, is gradually evolved into from simple protection carbon fiber and is answered in order to which carbon fiber can be strengthened
Condensation material interface binding intensity, composite materials property is improved, i.e., developed from universal sizing agent to functional form sizing agent.
Starching is an important procedure in the production process of carbon fiber.The main function of carbon fiber starching is isolation
Dust in air and moisture, so as to avoid damage to the fiber surface activity after surface treated.Use inorganic nano SiO in addition2
It is material modified as size resin, carbon fiber functional form emulsion pasting agent is prepared into, but due to inorganic particulate, its size is small, uniformly
It is scattered certain difficulty, therefore Nano-meter SiO_2 to be present2How many pairs of sizing agent performance impacts of dosage also need further to be studied.Also have
It is related to graphene modified carbon fiber emulsion pasting agent and preparation method, but contains for the oxygen of compatible modified Nano lamella molybdenum disulfide
Amount ratio, which is not done, clearly to be identified.
The content of the invention
In view of above-mentioned analysis, the present invention is intended to provide a kind of enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide and
Its preparation method, the sizing agent have good stability, can effectively improve the processing characteristics of carbon fiber, preparation side of the invention
Method is simple to operate, and cost is low, in actual applications can be by changing the proportioning of component in sizing agent, applied to different types of
Resin matrix.
The purpose of the present invention is mainly achieved through the following technical solutions：A kind of enhanced carbon of nanoscale twins molybdenum disulfide
Fiber sizing agent, it is by organic resin, emulsifying agent, dispersant, compatible modified Nano lamella molybdenum disulfide dispersion liquid, organic solvent
The mixed system formed with deionized water, wherein, by percentage to the quality, the emulsifying agent is the 0.5-5% of organic resin, divided
Powder is the 0.1-0.5% of organic resin, compatible modified Nano lamella molybdenum disulfide dispersion liquid is organic resin 0.05-1%,
Organic solvent is the 20-200% of organic resin, and gained mixed system solid content is 25-35%.
Described mixed system solid content, it is organic resin, emulsifying agent, dispersant and compatible modified Nano lamella curing
Molybdenum dispersion liquid accounts for the percentage composition of gross mass in mixed system.
The organic resin is modified epoxy.
Described emulsifying agent is a kind of nonionic surfactant, or the mixture of a variety of nonionic surfactants.
Described dispersant is γ-(methacryloxypropyl) base propyldimethoxy-silane, or polyethylene glycol.
Described organic solvent is 1-METHYLPYRROLIDONE, acetone or butanone.
Described compatible modified Nano lamella molybdenum disulfide, it is that ammonium persulfate initiator is passed through by polyacrylamide with one kind
The polyacrylamide modified Nano lamella molybdenum disulfide that situ-formed graft is formed on the nanoscale twins molybdenum disulfide surface of stripping.
A kind of method for preparing the described enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide, comprises the following steps：
Step (1)：At 30-100 DEG C, organic resin is disperseed to form organic resin solution in organic solvent, it is organic
Solvent quality is the 20-200% of organic resin；
Step (2)：After organic resin solution is down to room temperature, by the well mixed addition of emulsifying agent, dispersant and deionized water
In organic resin solution, the emulsifying agent quality of addition is the 0.5-5% of organic resin, and the dispersant quality of addition is organic resin
0.1-0.5%, addition deionized water to mixed system solid content be 30-50%, obtained organic resin emulsion；
Step (3)：Compatible modified Nano lamella molybdenum disulfide dispersion liquid is slowly added into organic resin emulsion, ultrasound
It is scattered, then proceed to add deionized water, be 25-35% to system solid content, compatible modified Nano lamella molybdenum disulfide is made
Strengthen sizing agent.
In the steps (2), emulsifying agent, dispersant and deionized water are well mixed and are added in organic resin solution,
First sheared with dispersion emulsifying machine to mixed system and phase transfer occurs, the rotating speed of dispersion emulsifying machine is 10000-28000rpm, then
It is further continued for after shearing 30-60 minutes, then adds deionized water.
The preparation method of the compatible modified Nano lamella molybdenum disulfide dispersion liquid is：
1) mixed liquor with preparing isopropanol and water, wherein volume ratio of the isopropanol in the mixed liquor is 30%-
70%, the molybdenum disulfide that size is less than 100 microns is added, forms the dispersion liquid that molybdenum disulfide concentration is 10mg/mL；
2) after dispersion liquid obtained by step 1) being carried out ultrasound, stood, centrifugation obtains upper strata dispersion liquid；
3) dispersion liquid obtained by step 2) is subjected to polyacrylamide modification：Acrylamide and ammonium persulfate are added, instead
Polyacrylamide modified Nano lamella molybdenum disulfide dispersion liquid should be obtained；The addition of wherein described acrylamide and ammonium persulfate
It is by weight：10:1-200:1, the addition of the acrylamide and molybdenum disulfide is by weight：5:1-25:1, reaction
Temperature is 40-80 DEG C, reaction time 4-96h.
The molybdenum disulfide lamella that the present invention is modified by adding polyacrylamide, the addition of the material can effectively with it is upper
It is compatible to starch agent matrix, so as to improve the wearability of starching agent material and other mechanical properties.
Brief description of the drawings
Accompanying drawing is only used for the supplementary explanation to description, is not intended as limiting.
Fig. 1 is the stereoscan photograph of molybdenum disulfide sheet layer material in example 1；
Fig. 2 is the stereoscan photograph of molybdenum disulfide sheet layer material in example 3.
Embodiment
Specifically describe the preferred embodiments of the present invention below in conjunction with the accompanying drawings.
Sizing agent of the present invention is disperseed by organic resin, emulsifying agent, dispersant, compatible modified Nano lamella molybdenum disulfide
The mixed system of liquid, organic solvent and deionized water composition, wherein emulsifying agent quality are 0.5-5%, the dispersant of organic resin
Quality is the 0.1-0.5% of organic resin, compatible modified Nano lamella molybdenum disulfide dispersion liquid is organic resin 0.05-1%,
Organic solvent quality is the 20-200% of organic resin, and gained mixed system solid content is 25-35%.
Described mixed system solid content is organic resin, emulsifying agent, dispersant and compatible modified Nano lamella curing
Molybdenum dispersion liquid accounts for the percentage composition of gross mass in mixed system.
Heretofore described organic resin is modified epoxy.
Heretofore described emulsifying agent is the mixture of one or more nonionic surfactants.
Heretofore described dispersant is γ-(methacryloxypropyl) base propyldimethoxy-silane (KH570) or gathered
Ethylene glycol.
Heretofore described organic solvent is acetone, butanone or 1-METHYLPYRROLIDONE.
Heretofore described compatible modified Nano lamella molybdenum disulfide, being will be poly- by ammonium persulfate initiator with one kind
The polyacrylamide modified Nano piece that acrylamide situ-formed graft is formed on the nanoscale twins molybdenum disulfide surface being effectively peeled off
Layer molybdenum disulfide, added in the form of molybdenum disulfide dispersion liquid, it is as described below on preparing for dispersion liquid：
1) mixed liquor of isopropyl alcohol and water is configured, wherein volume ratio of the isopropanol in the mixed liquor is 30%-
70%, the molybdenum disulfide that crystallite dimension is less than 100 microns is added, forms the dispersion liquid that molybdenum disulfide concentration is 10mg/mL；
2) after dispersion liquid obtained by step 1) being carried out ultrasound, stood, centrifugation obtains upper strata dispersion liquid；
3) dispersion liquid obtained by step 2) is subjected to polyacrylamide modification：Acrylamide and ammonium persulfate are added, instead
Polyacrylamide modified Nano lamella molybdenum disulfide dispersion liquid should be obtained.
Ultrasonic power described in step 2) is 100W, sonication treatment time 1-8h, time of repose 4-12h, and centrifugation turns
Speed is 2000-6000rpm.
The addition of acrylamide described in step 3) and ammonium persulfate, it is by weight：10:1-200:1, preferably
100：1；The addition of acrylamide and molybdenum disulfide, it is by weight：5:1-25:1, preferably 10:1；Reaction temperature is 40-
80 DEG C, preferably 60 DEG C；Reaction time is 4-96h, preferably 48h.
In the present invention by add polyacrylamide be modified molybdenum disulfide lamella, the material can effectively with sizing agent
Matrix is compatible, so as to improve the wearability of starching agent material and other mechanical properties.
So preparation of the enhanced carbon fiber sizing agent based on above-mentioned compatible modified Nano lamella molybdenum disulfide dispersion liquid
Method is as follows：
Step (1)：At 30-100 DEG C, organic resin is disperseed to form organic resin solution in organic solvent, it is organic
Solvent quality is the 20-200% of organic resin；
Step (2)：After organic resin solution is down to room temperature, by the well mixed addition of emulsifying agent, dispersant and deionized water
In organic resin solution, and sheared with dispersion emulsifying machine to mixed system and phase transfer occurs, the rotating speed of dispersion emulsifying machine is
10000-28000rpm, the emulsifying agent quality of addition are the 0.5-5% of organic resin, and the dispersant quality of addition is organic resin
0.1-0.5%；Continue after shearing 30-60 minutes, addition deionized water to mixed system solid content is 30-50%, and being made has
Machine resin emulsion；
Step (3)：Compatible modified Nano lamella molybdenum disulfide dispersion liquid is slowly added into organic resin emulsion, power
300-600W ultrasonic disperse 0.5-3 hours, then proceed to add deionized water, it is 25- that mixed system is diluted into solid content
35%, compatible modified Nano lamella molybdenum disulfide enhancing sizing agent is made.
The inventive method technique is simple, reliable, and obtained compatible modified Nano lamella molybdenum disulfide can rise to carbon fiber
Increased to good protective effect, while to the mechanical property of composite.The carbon fiber sizing agent of this functional form can
To optimize carbon fiber and its composite material interface performance and macro property, there is important meaning to carbon fibre composite industrial upgrading
Justice.
Embodiment 1
Step (1)：At 70 DEG C, by epoxy resin (trade mark 618), 1000 grams are dispersed in 1500 grams of 1-METHYLPYRROLIDONEs
Middle formation organic resin solution；
Step (2)：After resin solution is down to room temperature, by 10 grams of Solulan, 98,6 grams of cetomacrogol 1000s and 500 grams
Deionized water is well mixed to be added in organic resin solution, and is sheared with dispersion emulsifying machine to mixed system and phase transfer occurs, point
The rotating speed for dissipating mulser is 18000rpm；After continuing shearing 60 minutes, addition deionized water to mixed system solid content is 35%,
Organic resin emulsion is made；
Compatible 6 grams of modified Nano lamella molybdenum disulfide dispersion liquid is slowly added into organic resin emulsion by step (3), work(
Rate 600W ultrasonic disperses 1 hour, then proceed to add deionized water, it is 25% that mixed system is diluted into solid content, and phase is made
Hold modified Nano lamella molybdenum disulfide enhancing sizing agent.
The stereoscan photograph of modified molybdenum disulfide sheet layer material is as shown in Figure 1 in this example.
Embodiment 2
Step (1)：At 70 DEG C, 1000 grams of epoxy resin (trade mark 634) is dispersed in 1200 grams of acetone formed it is organic
Resin solution；
Step (2)：After resin solution is down to room temperature, by 10 grams of Solulan, 98,5 grams of KH570 and 500 gram of deionized waters
It is well mixed to add in organic resin solution, and sheared with dispersion emulsifying machine to mixed system and phase transfer, dispersion emulsifying machine occurs
Rotating speed be 16000rpm；After continuing shearing 60 minutes, addition deionized water to mixed system solid content is 35%, is made organic
Resin emulsion；
Step (3)：Compatible 8 grams of modified Nano lamella molybdenum disulfide dispersion liquid is slowly added into organic resin emulsion,
Power 500W ultrasonic disperses 1 hour, then proceed to add deionized water, it is 28% that mixed system is diluted into solid content, is made
Compatible modified Nano lamella molybdenum disulfide strengthens sizing agent.
Embodiment 3
Step (1)：At 60 DEG C, 1000 grams of epoxy resin (trade mark 618) is dispersed in 1500 grams of butanone formed it is organic
Resin solution；
Step (2)：After resin solution is down to room temperature, by 10 grams of Solulan, 97,5 grams of KH570,6 grams of polyethylene glycol
1000 and 500 grams of deionized waters are well mixed to be added in organic resin solution, and is sheared to mixed system and sent out with dispersion emulsifying machine
Raw phase transfer, the rotating speed of dispersion emulsifying machine is 14000rpm；After continuing shearing 45 minutes, addition deionized water to mixed system is consolidated
Content is 35%, and organic resin emulsion is made；
Step (3)：Compatible 5 grams of modified Nano lamella molybdenum disulfide dispersion liquid is slowly added into organic resin emulsion,
Power 400W ultrasonic disperses 1 hour, then proceed to add deionized water, it is 30% that mixed system is diluted into solid content, is made
Compatible modified Nano lamella molybdenum disulfide strengthens sizing agent.The stereoscan photograph of modified molybdenum disulfide sheet layer material in this example
As shown in Figure 2.
The mechanical property pair of the modified epoxy based composites obtained in embodiment 1-3 and unmodified composite
Than such as following table：
Pass through this contrast table, it can be seen that show by modified composite (embodiment 1,2,3) interlaminar shear strength
Work is more than unmodified composite.Amplitude of variation refers to compared with the sizing agent of unused modified molybdenum disulfide material, uses
The increase ratio of its interlaminar shear strength afterwards.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in,
It should all be included within the scope of the present invention.
Claims (8)
- A kind of 1. enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide, it is characterised in that：Be by organic resin, emulsifying agent, dispersant, compatible modified Nano lamella molybdenum disulfide dispersion liquid, organic solvent and go from The mixed system of sub- water composition, wherein, by percentage to the quality,The emulsifying agent is the 0.5-5% of organic resin, dispersant is organic resin 0.1-0.5%, compatible modified Nano piece Layer molybdenum disulfide dispersion liquid is the 0.05-1% of organic resin, the 20-200% that organic solvent is organic resin, gained mixture It is that solid content is 25-35%；Described mixed system solid content, it is organic resin, emulsifying agent, dispersant and compatible modified Nano Lamella molybdenum disulfide dispersion liquid accounts for the percentage composition of gross mass in mixed system；Described compatible modified Nano lamella molybdenum disulfide dispersion liquid is a kind of ammonium persulfate initiator of passing through by polyacrylamide Situ-formed graft disperses in the polyacrylamide modified Nano lamella molybdenum disulfide that the nanoscale twins molybdenum disulfide surface of stripping is formed Liquid.
- 2. the enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide according to claim 1, it is characterised in that：It is described to have Machine resin is modified epoxy.
- 3. the enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide according to claim 1, it is characterised in that：Described Emulsifying agent is a kind of nonionic surfactant, or the mixture of a variety of nonionic surfactants.
- 4. the enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide according to claim 1, it is characterised in that：Described Dispersant is γ-(methacryloxypropyl) base propyldimethoxy-silane, or polyethylene glycol.
- 5. the enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide according to claim 1, it is characterised in that：Described Organic solvent is 1-METHYLPYRROLIDONE, acetone or butanone.
- A kind of 6. preparation side of enhanced carbon fiber sizing agent of nanoscale twins molybdenum disulfide as described in one of claim 1-5 Method, it is characterised in that：Comprise the following steps：Step (1)：At 30-100 DEG C, organic resin is disperseed to form organic resin solution, organic solvent in organic solvent Quality is the 20-200% of organic resin；Step (2)：It is after organic resin solution is down to room temperature, the well mixed addition of emulsifying agent, dispersant and deionized water is organic In resin solution, the emulsifying agent quality of addition is the 0.5-5% of organic resin, and the dispersant quality of addition is organic resin 0.1-0.5%, addition deionized water to mixed system solid content is 30-50%, and organic resin emulsion is made；Step (3)：Compatible modified Nano lamella molybdenum disulfide dispersion liquid is slowly added into organic resin emulsion, ultrasound point Dissipate, then proceed to add deionized water, be 25-35% to system solid content, compatible modified Nano lamella molybdenum disulfide is made and increases Strong sizing agent.
- 7. preparation method according to claim 6, it is characterised in that：In the step (2), by emulsifying agent, dispersant and Deionized water is well mixed to be added in organic resin solution, is first sheared with dispersion emulsifying machine to mixed system and phase transfer occurs, The rotating speed of dispersion emulsifying machine is 10000-28000rpm, is then further continued for after shearing 30-60 minutes, then add deionized water.
- 8. preparation method according to claim 7, it is characterised in that：The compatible modified Nano lamella molybdenum disulfide disperses The preparation method of liquid is：1) mixed liquor with preparing isopropanol and water, wherein volume ratio of the isopropanol in the mixed liquor is 30%-70%, then The molybdenum disulfide that size is less than 100 microns is added, forms the dispersion liquid that molybdenum disulfide concentration is 10mg/mL；2) after dispersion liquid obtained by step 1) being carried out ultrasound, stood, centrifugation obtains upper strata dispersion liquid；3) dispersion liquid obtained by step 2) is subjected to polyacrylamide modification：Add acrylamide and ammonium persulfate, reaction obtain Obtain polyacrylamide modified Nano lamella molybdenum disulfide dispersion liquid；The addition of wherein described acrylamide and ammonium persulfate is by weight Measuring ratio is：10:1-200:1, the addition of the acrylamide and molybdenum disulfide is by weight：5:1-25:1, reaction temperature For 40-80 DEG C, reaction time 4-96h.
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| JPH0441779A (en) * | 1990-06-04 | 1992-02-12 | Asahi Chem Ind Co Ltd | Sized carbon fiber |
| CN101463181B (en) * | 2009-01-08 | 2011-06-22 | 西安交通大学 | Self-lubricating composite material and manufacturing method of self-lubricating composite material mould |
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| CN103937329A (en) * | 2014-05-09 | 2014-07-23 | 浙江大学 | Method for preparing molybdenum disulfide nano-layered dispersion with high stability |
| CN104120001A (en) * | 2014-08-07 | 2014-10-29 | 福建省将乐三华轴瓦股份有限公司 | Lubricant and use thereof |
| CN104593131A (en) * | 2014-12-29 | 2015-05-06 | 北京航空航天大学 | Method for preparing tungsten disulfide nanosheet water-based lubricating agent in situ |
| CN105293580A (en) * | 2015-10-15 | 2016-02-03 | 南京大学 | Method for preparing dispersion liquid of two-dimensional nano-sheet layer of transition metal sulfide |
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2016
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