CN113683861A - High-wear-resistance and high-thermal-conductivity composite material and preparation method and application thereof - Google Patents
High-wear-resistance and high-thermal-conductivity composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 111
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000004696 Poly ether ether ketone Substances 0.000 claims abstract description 87
- 229920002530 polyetherether ketone Polymers 0.000 claims abstract description 87
- 230000002829 reductive effect Effects 0.000 claims abstract description 73
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 70
- 239000000463 material Substances 0.000 claims abstract description 60
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000011165 3D composite Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 27
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 claims abstract 11
- 238000002156 mixing Methods 0.000 claims description 36
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 23
- 229910052750 molybdenum Inorganic materials 0.000 claims description 23
- 239000011733 molybdenum Substances 0.000 claims description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 21
- 239000011593 sulfur Substances 0.000 claims description 20
- 229910052717 sulfur Inorganic materials 0.000 claims description 20
- 239000006185 dispersion Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 18
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 16
- 238000003825 pressing Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 235000015393 sodium molybdate Nutrition 0.000 claims description 11
- 239000011684 sodium molybdate Substances 0.000 claims description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052961 molybdenite Inorganic materials 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 6
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 6
- 239000011609 ammonium molybdate Substances 0.000 claims description 6
- 229940010552 ammonium molybdate Drugs 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- 229960003151 mercaptamine Drugs 0.000 claims description 4
- 238000011534 incubation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 7
- 239000000945 filler Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000007792 addition Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical class N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a composite material with high wear resistance and high thermal conductivity, a preparation method and application thereof, wherein the composite material comprises a molybdenum disulfide/reductive graphene oxide three-dimensional composite material and PEEK; the composite material takes the molybdenum disulfide/reductive graphene oxide three-dimensional composite material as a high-thermal-conductivity filler, so that a thermal-conductivity network can be formed in a PEEK matrix, the purpose of improving the heat-conductivity of the PEEK is achieved, and the wear resistance of the PEEK can be improved; the preparation method has simple process flow and good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of plastic production, particularly relates to a composite material and a preparation method and application thereof, and particularly relates to a composite material with high wear resistance and high thermal conductivity and a preparation method and application thereof.
Background
Polyether ether ketone (PEEK) as a special engineering plastic has a series of advantages of high modulus, high strength, corrosion resistance, good dimensional stability and the like, is widely applied to the high-tech fields of aerospace, electronics, electricity, energy, medical treatment and the like, and can effectively prevent the surface of a heat exchange material from being scratched, so that a heat conduction interface material which is used stably and has good heat conductivity is obtained. PEEK has a thermal conductivity of only 0.25W/(m · K) at ambient temperature, limiting its application in the field of thermal conduction. In order to improve the heat conductivity of PEEK, a high thermal conductive filler is usually added to form a thermal conductive network in the PEEK matrix, so as to improve the heat conductivity of PEEK.
CN107286571A discloses an injection-moldable high-temperature-resistant wear-resistant composite material, which is prepared from the following components in parts by weight: 30-85 parts of PEEK, 10-40 parts of carbon fiber and 5-30 parts of modified nano boron nitride hollow microspheres. CN108219359A discloses a polyetheretherketone composite ultrasonic motor alloy friction material, which comprises 60-80 parts of polyetheretherketone, 3-8 parts of polyphenyl ester, 10-15 parts of polytetrafluoroethylene, 8-12 parts of nano silicon dioxide and 5-15 parts of molybdenum disulfide. The materials are prepared by adding a large amount of carbon fibers as reinforcing agents and adding PTFE as wear-resistant modifiers or other large amounts of wear-resistant materials, the prepared materials have certain strength and wear resistance, but the strength and the wear resistance are still required to be further improved, the existing materials do not fully consider that a large amount of heat is generated in the wear process, and if the heat of the materials cannot be timely removed, the high-temperature wear resistance and the service life of the materials are influenced.
CN104250423A discloses a high thermal conductive composite material. The composite material is formed by binary compounding of PEEK polymer and electrolytic copper powder in a tree structure. Wherein, the PEEK polymer has the grain diameter less than or equal to 5 μm and the volume ratio of 20-80 percent; the electrolytic copper powder is in a tree structure, the particle size is less than or equal to 15 mu m, and the volume ratio is 20-80%. The composite material adopts copper powder as the heat-conducting filler, although the copper powder can endow excellent heat-conducting property, the copper powder can be oxidized to generate copper oxide in the processing or using process, so that a large number of black spots appear on the surfaces of materials such as modified PEEK and the like, the appearance of the materials is influenced, and the application field of the materials is greatly limited.
In view of the above, how to provide a method for improving the heat conductivity and wear resistance of PEEK is a problem to be solved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a composite material with high wear resistance and high thermal conductivity, and a preparation method and application thereof, wherein the composite material adopts a molybdenum disulfide/reductive graphene oxide three-dimensional composite material as a high thermal conductive filler, so that a thermal conductive network can be formed in a PEEK matrix, the purpose of improving the thermal conductive property of the PEEK is achieved, and the wear resistance of the PEEK can be improved; the preparation method has simple process flow and good industrial application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a high wear resistance and high thermal conductivity composite comprising a molybdenum disulfide/reduced graphene oxide three-dimensional composite and PEEK.
In the invention, the molybdenum disulfide/reductive graphene oxide composite material is in a three-dimensional structure, a heat conduction path can be formed in a PEEK matrix, the interface thermal resistance is greatly reduced, the heat conduction performance of the matrix is effectively improved, and in addition, the molybdenum disulfide can not only improve the tensile strength of a plastic film, but also improve the friction resistance of the plastic film; and the PEEK is added to effectively prevent the surface of the heat exchange material from being scratched, so that the heat-conducting interface material which is used stably and has good heat conductivity is obtained.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferred technical solution of the present invention, the content of the molybdenum disulfide/reduced graphene oxide three-dimensional composite material is 20 to 40 wt%, for example, 20 wt%, 25 wt%, 30 wt%, 35 wt%, or 40 wt%; the PEEK content is 60 to 80 wt.%, for example 60 wt.%, 65 wt.%, 70 wt.%, 75 wt.% or 80 wt.%, and the selection of the above-mentioned values is not limited to the recited values, and other values not recited within the respective ranges of values are equally applicable.
In the invention, the content of the molybdenum disulfide/reduced graphene oxide three-dimensional composite material has an important influence on the performance of the finally obtained composite material. If the content of the organic silicon compound is too large, the heat conducting property of the composite material can be better improved, but the wear resistance of the composite material is deteriorated; if the content is too small, the improvement performance of the thermal conductivity is poor, and the later use of the composite material is influenced.
In a preferred embodiment of the present invention, the ratio of the molybdenum disulfide to the reduced graphene oxide in the molybdenum disulfide/reduced graphene oxide three-dimensional composite material is (0.02-0.1):1mol/g, for example, 0.02:1mol/g, 0.03:1mol/g, 0.04:1mol/g, 0.05:1mol/g, 0.06:1mol/g, 0.07:1mol/g, 0.08:1mol/g, 0.09:1mol/g, or 0.1:1mol/g, but not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
In the invention, the adding proportion of the molybdenum source and the graphene oxide needs to be controlled. If the addition amount of the molybdenum source is too much, too much sulfur source is consumed, and graphene oxide cannot be fully reduced; if the addition amount of the molybdenum source is too small, the sulfur source is wasted, and the molybdenum disulfide pieces on the surface of the graphene oxide are too few, which affects the formation of a three-dimensional structure.
In a second aspect, the present invention provides a method for preparing the above composite material, the method comprising the following steps:
(1) dispersing graphene oxide to obtain a graphene oxide dispersion liquid; mixing a molybdenum source, a sulfur source and graphene oxide dispersion liquid, and then carrying out hydrothermal reaction to obtain a molybdenum disulfide/reductive graphene oxide three-dimensional composite material;
(2) mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1), and after mixing, sequentially granulating, cold-pressing and sintering to obtain PEEK/MoS2A reduced graphene oxide composite material.
In the invention, molybdenum disulfide is generated from a molybdenum source and a sulfur source through a hydrothermal reaction and is dispersed on layered graphene oxide to form a three-dimensional structure; then compounding the molybdenum disulfide/reductive graphene oxide three-dimensional composite material with PEEK to obtain PEEK/MoS2The reductive graphene oxide composite material effectively improves the heat conductivity and the wear resistance of the composite material.
As a preferable technical scheme of the invention, the dispersing mode in the step (1) comprises ultrasonic treatment.
Preferably, the time period of the ultrasonic treatment in the step (1) is 1 to 3 hours, such as 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours, but not limited to the enumerated values, and other non-enumerated values in the numerical range are also applicable.
As a preferred embodiment of the present invention, the molybdenum source in step (1) comprises any one of sodium molybdate, potassium molybdate or ammonium molybdate, or a combination of at least two of them, and the combination is exemplified by, but not limited to: combinations of sodium molybdate and potassium molybdate, combinations of potassium molybdate and ammonium molybdate, combinations of sodium molybdate, potassium molybdate and ammonium molybdate, and the like.
Preferably, the sulphur source of step (1) comprises any one or a combination of at least two of thiourea, thioacetamide or L-cysteamine, typical but non-limiting examples of which are: combinations of thiourea and thioacetamide, thiourea and L-cysteamine, thiourea, thioacetamide and L-cysteamine, and the like.
Preferably, the molar ratio of the sulfur source to the molybdenum source in step (1) is (3-8):1, e.g., 3:1, 4:1, 5:1, 6:1, 7:1 or 8:1, but not limited to the recited values, and other values not recited within this range are equally applicable.
In the present invention, the sulfur source is added in an excessive amount because it is used for the purpose other than the production of MoS2In addition, the surplus sulfur source is used for reducing the graphene oxide to obtain the reducing graphene oxide with high conductivity, large specific surface area, good flexibility and good chemical stability, and the conductivity of the material can be further improved.
Preferably, the molybdenum source and the sulfur source in step (1) are mixed with the graphene oxide dispersion liquid and then stirred.
Preferably, the stirring time is 1-2 hours, such as 1 hour, 1.2 hours, 1.4 hours, 1.6 hours, 1.8 hours, 2 hours, etc., but not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, the equipment used in the hydrothermal reaction in step (1) comprises a p-polytetrafluoroethylene reaction kettle.
Preferably, the hydrothermal reaction temperature in step (1) is 170-.
Preferably, the hydrothermal reaction time in step (1) is 10-30h, such as 10h, 15h, 20h, 25h or 30h, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the hydrothermal reaction in step (1) is followed by washing and drying in sequence.
Preferably, the washing is performed with water and/or ethanol.
Preferably, the drying temperature is 60-80 ℃, such as 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
As a preferable technical scheme of the invention, the pretreatment mode in the step (2) comprises heat preservation treatment.
Preferably, the temperature of the heat-preservation treatment is 100-150 ℃, such as 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ or 150 ℃, but not limited to the recited values, and other unrecited values within the range of the values are also applicable.
Preferably, the incubation time is 5-10 hours, such as 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, or 10 hours, but not limited to the recited values, and other values not recited within the range are equally applicable, preferably 6-8 hours.
In the invention, the PEEK is subjected to heat preservation treatment to remove moisture in the PEEK, and if the PEEK is not dried sufficiently, silver streaks are easy to generate, so that the quality of a subsequent composite material is influenced.
In a preferred embodiment of the present invention, the mass ratio of PEEK to the molybdenum disulfide/reduced graphene oxide three-dimensional composite material in step (2) is (1.5-4):1, for example, 1.5:1, 2:1, 2.5:1, 3:1, 3.5:1, or 4:1, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the mixing time in step (2) is 5-20min, such as 5min, 10min, 15min or 20min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the granulation in step (2) is carried out by using any one of a twin-screw extruder, a single-screw extruder or a main and auxiliary granulator.
Preferably, the temperature for the granulation in step (2) is 350-.
Preferably, the rotation speed in the granulation process in step (2) is 30-80r/min, such as 30r/min, 40r/min, 50r/min, 60r/min, 70r/min or 80r/min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the pressure of the cold pressing in step (2) is 8-15MPa, such as 8MPa, 9MPa, 10MPa, 11MPa, 12MPa, 13MPa, 14MPa or 15MPa, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the cold pressing time in step (2) is 5-20min, such as 5min, 10min, 15min or 20min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the sintering temperature in step (2) is 350-400 ℃, such as 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃ or 400 ℃, but not limited to the recited values, and other unrecited values within the range of values are equally applicable.
Preferably, the sintering time in step (2) is 1-2h, such as 1h, 1.2h, 1.4h, 1.6h, 1.8h or 2h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the sintering of step (2) is followed by cold pressing again.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) dispersing graphene oxide in water, and performing ultrasonic treatment for 1-3h to obtain a graphene oxide dispersion liquid; mixing a sulfur source and a molybdenum source with the graphene oxide dispersion liquid according to the molar ratio of (3-8):1, wherein the ratio of the molybdenum source to the graphene oxide is (0.02-0.1):1mol/g in the mixing process, stirring for 1-2h after mixing, then carrying out hydrothermal reaction at the temperature of 170-250 ℃, reacting for 10-30h, washing with water and/or ethanol, and drying at the temperature of 60-80 ℃ to obtain the molybdenum disulfide/reductive graphene oxide three-dimensional composite material;
(2) firstly, the PEEK is insulated for 5-10h at the temperature of 100-150 ℃; and (2) mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to the mass ratio of (1.5-4) to 1, granulating at 385 ℃ of 350-.
In a third aspect, the invention provides the use of the composite material for preparing a total heat exchanger in a fresh air purifier or an air purifier.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the composite material, the molybdenum disulfide/reductive graphene oxide composite material with a three-dimensional structure is compounded with the PEEK, so that the heat-conducting property of a PEEK matrix is effectively improved, and the PEEK/MoS is ensured2The friction resistance of the reductive graphene oxide composite material; the content of the molybdenum disulfide/reductive graphene oxide composite material and the content of PEEK are further controlled, so that the thermal conductivity coefficient reaches more than 1.9W/(m.K), and the average friction coefficient is below 0.31;
(2) the preparation method provided by the invention is simple in process flow and has a good industrial application prospect.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a high-wear-resistance and high-thermal-conductivity composite material and a preparation method thereof, wherein the composite material comprises 20 wt% of molybdenum disulfide/reduced graphene oxide three-dimensional composite material and 80 wt% of PEEK.
The preparation method comprises the following steps:
(1) dispersing 100mg of graphene oxide in water, and performing ultrasonic treatment for 1h to obtain a graphene oxide dispersion liquid; mixing 0.4g of sodium molybdate and 0.72g of thiourea (namely the molar ratio of the sulfur source to the molybdenum source is 5:1) with the graphene oxide dispersion liquid, wherein the ratio of the sodium molybdate to the graphene oxide is 0.09:1mol/g in the mixing process, and stirring for 1h after mixing; then transferring the mixture to a para-polytetrafluoroethylene reaction kettle, carrying out hydrothermal reaction at 210 ℃ for 24 hours, washing with water, and drying at 80 ℃ to obtain a molybdenum disulfide/reductive graphene oxide three-dimensional composite material;
(2) firstly, keeping the temperature of PEEK at 120 ℃ for 6 h; then mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to a mass ratio of 4:1, adopting a double-screw extruder after mixing, setting the rotating speed to be 30r/min, granulating at 350 ℃, cold-pressing the obtained granules for 10min under the condition of 10MPa, sintering for 1.5h under the condition of 380 ℃, cold-pressing for 10min under the condition of 10MPa again after sintering, and obtaining PEEK/MoS2A reduced graphene oxide composite material.
Example 2:
the embodiment provides a high-wear-resistance and high-thermal-conductivity composite material and a preparation method thereof, wherein the composite material comprises 30 wt% of molybdenum disulfide/reduced graphene oxide three-dimensional composite material and 70 wt% of PEEK.
The preparation process is as in example 1, except that: and (3) mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to a mass ratio of 7: 3.
Example 3:
the embodiment provides a high-wear-resistance and high-thermal-conductivity composite material and a preparation method thereof, wherein the composite material comprises 40 wt% of molybdenum disulfide/reduced graphene oxide three-dimensional composite material and 60 wt% of PEEK.
The preparation process is as in example 1, except that: and (3) mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to a mass ratio of 3: 2.
Example 4:
the embodiment provides a high-wear-resistance and high-thermal-conductivity composite material and a preparation method thereof, wherein the composite material comprises 30 wt% of molybdenum disulfide/reduced graphene oxide three-dimensional composite material and 70 wt% of PEEK.
The preparation method comprises the following steps:
(1) dispersing 100mg of graphene oxide in water, and performing ultrasonic treatment for 2 hours to obtain a graphene oxide dispersion liquid; mixing 0.14g of sodium molybdate and 0.15g of thiourea (namely the molar ratio of the sulfur source to the molybdenum source is 3:1) with the graphene oxide dispersion liquid, wherein the ratio of the sodium molybdate to the graphene oxide is 0.02:1mol/g in the mixing process, and stirring for 2 hours after mixing; then transferring the mixture to a para-polytetrafluoroethylene reaction kettle, carrying out hydrothermal reaction at 170 ℃, reacting for 30h, washing with ethanol, and drying at 60 ℃ to obtain a molybdenum disulfide/reductive graphene oxide three-dimensional composite material;
(2) firstly, keeping the temperature of PEEK at 100 ℃ for 10 h; and (2) mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to a mass ratio of 7:3, mixing, granulating at 385 ℃ by using a double-screw extruder at a set rotating speed of 80r/min, cold-pressing the obtained granules for 20min under the condition of 8MPa, sintering for 2h at 350 ℃, cold-pressing for 5min under the condition of 12MPa again after sintering, and obtaining PEEK/MoS2A reduced graphene oxide composite material.
Example 5:
the embodiment provides a high-wear-resistance and high-thermal-conductivity composite material and a preparation method thereof, wherein the composite material comprises 40 wt% of molybdenum disulfide/reduced graphene oxide three-dimensional composite material and 60 wt% of PEEK.
The preparation method comprises the following steps:
(1) dispersing 100mg of graphene oxide in water, and performing ultrasonic treatment for 1.5h to obtain a graphene oxide dispersion liquid; mixing 0.123g of ammonium molybdate and 0.376g of thioacetamide (namely the molar ratio of the sulfur source to the molybdenum source is 8:1) with the graphene oxide dispersion liquid, wherein the ratio of the ammonium molybdate to the graphene oxide is 0.05:1mol/g in the mixing process, and stirring for 1.5 hours after mixing; then transferring the mixture to a para-polytetrafluoroethylene reaction kettle, carrying out hydrothermal reaction at 250 ℃ for 10h, washing with water, and drying at 75 ℃ to obtain a molybdenum disulfide/reductive graphene oxide three-dimensional composite material;
(2) firstly, keeping the temperature of PEEK at 150 ℃ for 5 h; then mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to a mass ratio of 3:2, granulating at 365 ℃ by adopting a double-screw extruder after mixing, cold-pressing the obtained granules for 5min under the condition of 15MPa, sintering for 1.5h under the condition of 370 ℃, cold-pressing for 8min under the condition of 12MPa again after sintering, and obtaining PEEK/MoS2A reduced graphene oxide composite material.
Example 6:
the embodiment provides a high-wear-resistance and high-thermal-conductivity composite material and a preparation method thereof, wherein the composite material comprises 50 wt% of molybdenum disulfide/reduced graphene oxide three-dimensional composite material and 50 wt% of PEEK.
The preparation process is referred to the preparation process in example 3, with the only difference that: and (3) mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to the mass ratio of 1:1 in the step (2).
Example 7:
the embodiment provides a high-wear-resistance and high-thermal-conductivity composite material and a preparation method thereof, wherein the composite material comprises a molybdenum disulfide/reduced graphene oxide three-dimensional composite material in an amount of 10 wt% and PEEK in an amount of 90 wt%.
The preparation process is as in example 1, except that: and (3) mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to a mass ratio of 9:1 in the step (2).
Example 8:
the embodiment provides a high-wear-resistance and high-thermal-conductivity composite material and a preparation method thereof, wherein the composite material comprises 20 wt% of molybdenum disulfide/reduced graphene oxide three-dimensional composite material and 80 wt% of PEEK.
The preparation process is as in example 1, except that: in the step (1), 0.63g of sodium molybdate and 1.14g of thiourea (namely, the molar ratio of the sulfur source to the molybdenum source is 5:1) are mixed with the graphene oxide dispersion liquid, and the ratio of the sodium molybdate to the graphene oxide in the mixing process is 0.15:1 mol/g.
Comparative example 1:
this comparative example provides a PEEK material that is the same as the PEEK material used in example 1.
Comparative example 2:
this comparative example provides a composite material comprising 20 wt% graphene oxide and 80 wt% PEEK and a method of making the same.
The preparation is as in example 1, with the difference that: in the step (1), 0.4g of sodium molybdate and 0.72g of thiourea (the molar ratio of the sulfur source to the molybdenum source is 2:1) are mixed with the graphene oxide dispersion liquid, namely the sulfur source is not excessive, the graphene oxide cannot be reduced to obtain the reduced graphene oxide, and therefore the obtained composite material is PEEK/MoS2Graphene oxide composite material.
Comparative example 3:
the present comparative example provides a composite material including 20 wt% reduced graphene oxide and 80 wt% PEEK, and a method of preparing the same.
The preparation is as in example 1, with the difference that: and (3) adding no molybdenum source to obtain the PEEK/reducing graphene oxide composite material.
Comparative example 4:
this comparative example provides a composite material comprising 20 wt% molybdenum disulfide and 80 wt% PEEK and a method of making the same.
The preparation is as in example 1, with the difference that: and adding no graphene oxide to obtain the PEEK/molybdenum disulfide composite material. Comparative example 5:
this comparative example provides a composite material comprising 20 wt% molybdenum disulfide/C and a method of making the same3N4Composite material and 80 wt% PEEK.
The preparation is as in example 1, with the difference that: changing graphene oxide to C3N4Thus obtaining PEEK/molybdenum disulfide/C3N4A composite material.
PEEK/MoS obtained in examples 1 to 8 were measured2The thermal conductivity and average friction coefficient of the/reduced graphene oxide composite and the PEEK material in comparative example 1 and the composite in comparative examples 2-5 are shown in table 1.
TABLE 1
Embodiments 1-5 compound the molybdenum disulfide/reductive graphene oxide three-dimensional composite material with PEEK, and control the content of the two, effectively improve the thermal conductivity of the composite material and ensure the friction resistance, so that PEEK/MoS2The thermal conductivity coefficient of the/reductive graphene oxide composite material is more than 1.91W/(m.K), and the average friction coefficient is less than 0.31; fruit of Chinese wolfberryIn example 6, the content of the molybdenum disulfide/reductive graphene oxide three-dimensional composite material is increased, and although the heat conductivity is obviously improved, the friction resistance is reduced; in example 7, the content of the molybdenum disulfide/reduced graphene oxide three-dimensional composite material is reduced, so that the improvement of the thermal conductivity is very limited; in example 8, the ratio of the molybdenum source to the graphene oxide in the process of preparing the molybdenum disulfide/reductive graphene oxide three-dimensional composite material is increased, so that the friction performance is relatively improved, but the improvement of the heat conductivity is limited.
In the comparative example 1, the PEEK material is not improved at all, the heat conductivity is only 0.25W/(m.K), and the heat conductivity is poor; in comparative example 2, the graphene oxide was not reduced, resulting in a decrease in electrical properties; in the comparative example 3, only the reduced graphene oxide and the PEEK are compounded, so that a molybdenum disulfide/reduced graphene oxide three-dimensional composite material cannot be formed, a complete heat conduction path cannot be formed, and the heat conduction performance is reduced; in the embodiment 4, only molybdenum disulfide and PEEK are compounded, and a complete heat conduction path cannot be formed, so that the heat conduction performance is reduced; example 5 with C3N4The graphene oxide is replaced, and the improvement of the heat conductivity is limited.
It can be seen from the above examples and comparative examples that the composite material of the present invention combines the molybdenum disulfide/reduced graphene oxide composite material having a three-dimensional structure with PEEK, thereby effectively improving the thermal conductivity of the PEEK matrix and simultaneously ensuring PEEK/MoS2The friction resistance of the reductive graphene oxide composite material; the content of the molybdenum disulfide/reductive graphene oxide composite material and the content of PEEK are further controlled, so that the thermal conductivity coefficient reaches more than 1.9W/(m.K), and the average friction coefficient is below 0.31; the preparation method has simple process flow and better industrial application prospect.
The applicant states that the present invention is illustrated by the above examples to show the products and detailed methods of the present invention, but the present invention is not limited to the above products and detailed methods, i.e. it is not meant that the present invention must rely on the above products and detailed methods to be carried out. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents thereof, additions of additional operations, selection of specific ways, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A high wear resistance and high thermal conductivity composite comprising a molybdenum disulfide/reduced graphene oxide three dimensional composite and PEEK.
2. The composite material of claim 1, wherein the molybdenum disulfide/reduced graphene oxide three-dimensional composite material is in an amount of 20-40 wt%, and the PEEK is in an amount of 60-80 wt%.
3. The composite material according to claim 1 or 2, wherein the ratio of molybdenum disulfide to reduced graphene oxide in the molybdenum disulfide/reduced graphene oxide three-dimensional composite material is (0.02-0.1):1 mol/g.
4. A method for preparing a composite material according to any one of claims 1 to 3, characterized in that it comprises the following steps:
(1) dispersing graphene oxide to obtain a graphene oxide dispersion liquid; mixing a molybdenum source, a sulfur source and graphene oxide dispersion liquid, and then carrying out hydrothermal reaction to obtain a molybdenum disulfide/reductive graphene oxide three-dimensional composite material;
(2) mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1), and after mixing, sequentially granulating, cold-pressing and sintering to obtain PEEK/MoS2A reduced graphene oxide composite material.
5. The method according to claim 4, wherein the dispersing means of step (1) comprises ultrasonic treatment;
preferably, the time of the ultrasonic treatment in the step (1) is 1-3 h.
6. The method according to claim 4 or 5, wherein the molybdenum source of step (1) comprises any one of sodium molybdate, potassium molybdate or ammonium molybdate, or a combination of at least two thereof;
preferably, the sulfur source of step (1) comprises any one or a combination of at least two of thiourea, thioacetamide or L-cysteamine;
preferably, the molar ratio of the sulfur source to the molybdenum source in step (1) is (3-8): 1;
preferably, the molybdenum source and the sulfur source in the step (1) are mixed with the graphene oxide dispersion liquid and then stirred;
preferably, the stirring time is 1-2 h;
preferably, the hydrothermal reaction in step (1) uses equipment comprising a p-polytetrafluoroethylene reaction kettle;
preferably, the temperature of the hydrothermal reaction in the step (1) is 170-250 ℃;
preferably, the hydrothermal reaction time of the step (1) is 10-30 h;
preferably, the hydrothermal reaction in step (1) is followed by washing and drying in sequence;
preferably, the washing is carried out with water and/or ethanol;
preferably, the temperature of the drying is 60-80 ℃.
7. The method according to any one of claims 4 to 6, wherein the pretreatment in step (2) comprises an incubation treatment;
preferably, the temperature of the heat preservation treatment is 100-150 ℃;
preferably, the time of the heat preservation treatment is 5-10h, preferably 6-8 h.
8. The preparation method according to any one of claims 4 to 7, wherein the mass ratio of the PEEK to the molybdenum disulfide/reduced graphene oxide three-dimensional composite material in the step (2) is (1.5-4): 1;
preferably, the mixing time of the step (2) is 5-20 min;
preferably, the granulation in the step (2) adopts any one of a double-screw extruder, a single-screw extruder or a main and auxiliary granulator;
preferably, the temperature for the granulation in the step (2) is 350-385 ℃;
preferably, the rotating speed in the granulating process in the step (2) is 30-80 r/min;
preferably, the pressure of the cold pressing in the step (2) is 8-15 MPa;
preferably, the cold pressing time in the step (2) is 5-20 min;
preferably, the sintering temperature in the step (2) is 350-400 ℃;
preferably, the sintering time of the step (2) is 1-2 h;
preferably, the sintering of step (2) is followed by cold pressing again.
9. The method according to any one of claims 4 to 8, characterized in that it comprises the following steps:
(1) dispersing graphene oxide in water, and performing ultrasonic treatment for 1-3h to obtain a graphene oxide dispersion liquid; mixing a sulfur source and a molybdenum source with the graphene oxide dispersion liquid according to the molar ratio of (3-8):1, wherein the ratio of the molybdenum source to the graphene oxide is (0.02-0.1):1mol/g in the mixing process, stirring for 1-2h after mixing, then carrying out hydrothermal reaction at the temperature of 170-250 ℃, reacting for 10-30h, washing with water and/or ethanol, and drying at the temperature of 60-80 ℃ to obtain the molybdenum disulfide/reductive graphene oxide three-dimensional composite material;
(2) firstly, the PEEK is insulated for 5-10h at the temperature of 100-150 ℃; then mixing the pretreated PEEK with the molybdenum disulfide/reductive graphene oxide three-dimensional composite material obtained in the step (1) according to the mass ratio of (1.5-4) to 1, granulating at 385 ℃ of 350-2A reduced graphene oxide composite material.
10. Use of the composite material according to any one of claims 1 to 3 for the preparation of a total heat exchanger in a fresh air or air purifier.
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