CN114989467A - Ultrahigh molecular weight polyethylene/graphite composite material and preparation method thereof - Google Patents
Ultrahigh molecular weight polyethylene/graphite composite material and preparation method thereof Download PDFInfo
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- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 title claims abstract description 178
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 title claims abstract description 178
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 168
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 159
- 239000010439 graphite Substances 0.000 title claims abstract description 159
- 239000002131 composite material Substances 0.000 title claims abstract description 109
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 68
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000003607 modifier Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 239000008247 solid mixture Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 19
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 15
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000007731 hot pressing Methods 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- RELMFMZEBKVZJC-UHFFFAOYSA-N 1,2,3-trichlorobenzene Chemical compound ClC1=CC=CC(Cl)=C1Cl RELMFMZEBKVZJC-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 13
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000008096 xylene Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 1
- 238000013329 compounding Methods 0.000 abstract description 16
- 239000002861 polymer material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- -1 polyethylene Polymers 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 238000000113 differential scanning calorimetry Methods 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
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- 230000008569 process Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
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- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
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- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920010741 Ultra High Molecular Weight Polyethylene (UHMWPE) Polymers 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J3/00—Processes of treating or compounding macromolecular substances
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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- C—CHEMISTRY; METALLURGY
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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Abstract
The invention relates to the technical field of high polymer materials, and discloses an ultrahigh molecular weight polyethylene/graphite composite material and a preparation method thereof, wherein the preparation method comprises the following steps: s1: heating and melting the modifier, mixing the modifier with the ultra-high molecular weight polyethylene and graphite, and cooling to obtain a solid mixture; s2: removing the modifier in the solid mixture to obtain ultra-high molecular weight polyethylene/graphite composite powder; s3: mixing the ultra-high molecular weight polyethylene/graphite composite powder with tetrahydrofuran or dimethylbenzene to obtain ultra-high molecular weight polyethylene/graphite composite slurry; s4: smearing the ultra-high molecular weight polyethylene/graphite composite slurry, and carrying out hot-pressing treatment to obtain an ultra-high molecular weight polyethylene/graphite composite material; the modifier is one or two of phenol or 1,2, 3-trichlorobenzene. The invention obtains the ultra-high molecular weight polyethylene/graphite composite material with excellent performance by uniformly compounding the ultra-high molecular weight polyethylene and graphite.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to an ultrahigh molecular weight polyethylene/graphite composite material and a preparation method thereof.
Background
Ultra-high molecular weight polyethylene (UHMWPE) refers to unbranched linear polyethylene with the molecular weight of more than 150 ten thousand, and has the advantages of low density, high chemical stability, impact resistance, excellent biocompatibility, low friction coefficient, high wear resistance, good self-lubricating property and the like; meanwhile, the ultra-high molecular weight polyethylene also has the defects of low surface hardness, low mechanical strength, low thermal deformation temperature, poor high temperature resistance, difficult processing and the like. Therefore, in order to overcome the disadvantages of the ultra-high molecular weight polyethylene and widen the application range thereof, it is necessary to improve the properties of the ultra-high molecular weight polyethylene.
At present, common performance improvement methods of ultrahigh molecular weight polyethylene include oxidation, crosslinking, blending, filler compounding and the like, wherein the most common filler compounding method is melt compounding and solution compounding. Because the viscosity of the ultra-high molecular weight polyethylene is higher, the problems of difficult processing, high cost and the like exist when the melt compounding mode is used for improving the performance of the ultra-high molecular weight polyethylene; however, the solution compounding method does not have the problems, and the solution compounding method can stretch the ultra-long molecular chain of the ultra-high molecular weight polyethylene, improve the compounding capability, and further effectively improve and improve the performance of the ultra-high molecular weight polyethylene.
However, the existing solution compounding method is difficult to mix the high-viscosity ultrahigh molecular weight polyethylene and graphite uniformly, and the problems of graphite agglomeration, difficult stretching of ultrahigh molecular weight polyethylene molecular chains, nonuniform compounding and the like often occur.
Disclosure of Invention
The invention aims to overcome the problem that the solution compounding mode is difficult to uniformly mix the high-viscosity ultrahigh molecular weight polyethylene and graphite, and provides an ultrahigh molecular weight polyethylene/graphite composite material.
The invention also aims to provide a preparation method of the ultrahigh molecular weight polyethylene/graphite composite material. According to the invention, the ultrahigh molecular weight polyethylene is dissolved by adopting a proper solvent, the molecular chain of the ultrahigh molecular weight polyethylene is fully stretched, and the graphite is uniformly dispersed in a combined ultrasonic stirring mode, so that the uniform compounding of the ultrahigh molecular weight polyethylene and the graphite is ensured, and the ultrahigh molecular weight polyethylene/graphite composite material with excellent performance is obtained.
In order to achieve the technical purpose, the invention is realized by the following technical scheme:
a preparation method of an ultra-high molecular weight polyethylene/graphite composite material comprises the following steps:
s1: heating and melting the modifier, mixing the modifier with the ultra-high molecular weight polyethylene and graphite, and cooling to obtain a solid mixture;
s2: removing the modifier in the solid mixture to obtain ultra-high molecular weight polyethylene/graphite composite powder;
s3: mixing the ultra-high molecular weight polyethylene/graphite composite powder with tetrahydrofuran or dimethylbenzene to obtain ultra-high molecular weight polyethylene/graphite composite slurry;
s4: smearing the ultra-high molecular weight polyethylene/graphite composite slurry, and carrying out hot-pressing treatment to obtain an ultra-high molecular weight polyethylene/graphite composite material;
wherein, in the step S1, the modifier is one or two of phenol or 1,2, 3-trichlorobenzene.
The modifier phenol selected by the invention has a melting point higher than room temperature, is easy to dissolve the ultrahigh molecular weight polyethylene, can fully extend molecular chains of the ultrahigh molecular weight polyethylene, and can fix the extended state of the molecular chains of the ultrahigh molecular weight polyethylene and the dispersed state of graphite in the ultrahigh molecular weight polyethylene to prevent graphite aggregation when the phenol is cooled to form a solid, so that the ultrahigh molecular weight polyethylene/graphite composite material with excellent performance is obtained.
Preferably, in step S1, a magnetic stirrer is used to stir, heat and melt the modifier, the ultra-high molecular weight polyethylene and the graphite are added and mixed uniformly under the condition of ultrasonic dispersion, the heating is stopped, and the mixture is cooled naturally to obtain a solid mixture.
The inventor finds that molecular chains of the ultra-high molecular weight polyethylene can be more stretched through ultrasonic dispersion and magnetic stirring treatment under the condition of using a modifier phenol, and simultaneously, graphite is more uniformly dispersed in the ultra-high molecular weight polyethylene, so that the uniform compounding of the ultra-high molecular weight polyethylene and the graphite is ensured, and the performance of the ultra-high molecular weight polyethylene/graphite composite material is improved.
In addition, in the process of naturally cooling the modifier phenol to form a solid, the magnetic stirring is carried out, the cooling process is accelerated, the same cooling rate of each part of the system is ensured, the separation of the ultrahigh molecular weight polyethylene and the graphite due to different precipitation capacities in the modifier phenol in the natural cooling process is avoided, and the graphite is dispersed in the ultrahigh molecular weight polyethylene more uniformly.
Further preferably, the power of the ultrasonic dispersion is 100-1000W.
Further preferably, the temperature of the heating and melting modifier is 70-160 ℃.
Preferably, the molecular weight of the ultra-high molecular weight polyethylene in step S1 is 250 to 400 ten thousand, and preferably 330 ten thousand.
Preferably, the graphite in step S1 is one or more of graphite powder, graphite flake (GNP) or Graphene Oxide (GO).
Preferably, the mass ratio of the graphite to the ultrahigh molecular weight polyethylene in step S1 is 1:1 to 1: 9.
Preferably, the mass ratio of the modifier to the ultrahigh molecular weight polyethylene in the step S1 is 2500 (15-27).
Preferably, the step S2 is to mix the solid mixture with tetrahydrofuran, pump-filter, take the solid, wash with tetrahydrofuran, and dry to obtain the ultra-high molecular weight polyethylene/graphite composite powder.
Preferably, in step S3, the ultrahigh molecular weight polyethylene/graphite composite powder and tetrahydrofuran or xylene are dispersed by ball milling to obtain ultrahigh molecular weight polyethylene/graphite composite slurry.
Preferably, the using amount ratio of the ultra-high molecular weight polyethylene/graphite composite powder to tetrahydrofuran or xylene in the step S3 is 0.03-0.1 g/mL, and preferably 0.06 g/mL.
Preferably, in the step S4, the ultrahigh molecular weight polyethylene/graphite composite slurry is poured onto a substrate, blade-coated to form a film, and hot-pressed to obtain the ultrahigh molecular weight polyethylene/graphite composite material.
Further preferably, the substrate is a polytetrafluoroethylene film.
Preferably, the temperature of the hot pressing treatment in the step S4 is 200 to 250 ℃, and preferably 220 ℃.
An ultrahigh molecular weight polyethylene/graphite composite material is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, through the selection of the modifier phenol, the ultrasonic dispersion and the magnetic stirring, molecular chains of the ultra-high molecular weight polyethylene are fully unfolded, meanwhile, graphite is uniformly dispersed in the ultra-high molecular weight polyethylene, and through the cooling solidification of the modifier phenol, the effects of fixing the unfolded state of the molecular chains of the ultra-high molecular weight polyethylene and the dispersed state of the graphite in the ultra-high molecular weight polyethylene are achieved, the graphite is prevented from being aggregated, the ultra-high molecular weight polyethylene and the graphite are uniformly compounded, and the ultra-high molecular weight polyethylene/graphite composite material with excellent performance is obtained. In addition, the increase of the graphite mass content in the ultra-high molecular weight polyethylene/graphite composite material can increase the crystallization temperature, the electrical conductivity, the tensile strength and the tensile modulus of the composite material.
Drawings
Fig. 1 is an appearance diagram of a sample of the ultra-high molecular weight polyethylene/graphite composite powder and the ultra-high molecular weight polyethylene/graphite composite, fig. a is an appearance diagram of a sample of the ultra-high molecular weight polyethylene/graphite composite powder prepared in step S2 of example 1, and fig. B is an appearance diagram of a sample of the ultra-high molecular weight polyethylene/graphite composite prepared in comparative example 2.
FIG. 2 is a Differential Scanning Calorimetry (DSC) temperature rise melting curve of the ultra-high molecular weight polyethylene/graphite composite materials of examples 1-5 and the ultra-high molecular weight polyethylene material of comparative example 1.
FIG. 3 is a Differential Scanning Calorimetry (DSC) temperature decreasing crystallization curve of the ultra-high molecular weight polyethylene/graphite composite materials of examples 1-5 and the ultra-high molecular weight polyethylene material of comparative example 1.
FIG. 4 is a line graph showing the electrical conductivity of the ultrahigh molecular weight polyethylene/graphite composite materials of examples 1 to 5 having different graphite contents by mass.
FIG. 5 is a graph showing the trend of mechanical properties of the ultrahigh molecular weight polyethylene/graphite composite materials of examples 1 to 5 and the ultrahigh molecular weight polyethylene material of comparative example 1.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specific conditions noted in the examples below, generally according to conditions conventional in the art or as suggested by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Example 1
The embodiment provides an ultrahigh molecular weight polyethylene/graphite composite material, and a preparation method thereof comprises the following steps:
s1: stirring by using a magnetic stirrer, heating to 160 ℃ in an oil bath to melt 250g of phenol, simultaneously adding 2.7g of ultra-high molecular weight polyethylene (with the molecular weight of 330 ten thousand) and 0.3g of graphite powder (with the diameter of about 2.6 mu m) under the condition of 300W ultrasonic dispersion, performing ultrasonic mixing for 30min, stopping heating, and naturally cooling to obtain a solid mixture;
s2: adding 1000mL of tetrahydrofuran into the solid mixture, stirring and mixing for 1h at room temperature, performing suction filtration, taking the solid, repeatedly washing the solid with the tetrahydrofuran until the washing liquid is colorless, and drying the solid in an oven at 80 ℃ for 30min to obtain the ultra-high molecular weight polyethylene/graphite composite powder;
s3: taking 3g of ultrahigh molecular weight polyethylene/graphite composite powder and 50mL of tetrahydrofuran, and carrying out ball milling and dispersion for 10min to obtain ultrahigh molecular weight polyethylene/graphite composite slurry;
s4: pouring the ultra-high molecular weight polyethylene/graphite composite slurry on a polytetrafluoroethylene film, carrying out blade coating to form a film, heating to 220 ℃ after tetrahydrofuran is completely volatilized, and carrying out hot pressing treatment to obtain the ultra-high molecular weight polyethylene/graphite composite material, wherein the mass content of graphite is 10%.
Example 2
The embodiment provides an ultrahigh molecular weight polyethylene/graphite composite material, and a preparation method thereof comprises the following steps:
s1: stirring by using a magnetic stirrer, heating to 160 ℃ in an oil bath to melt 250g of phenol, simultaneously adding 2.4g of ultra-high molecular weight polyethylene (molecular weight is 330 ten thousand) and 0.6g of graphite powder (diameter is about 2.6 mu m) under the condition of 300W ultrasonic dispersion, uniformly mixing by ultrasonic 30min, stopping heating, and naturally cooling to obtain a solid mixture;
s2: adding 1000mL of tetrahydrofuran into the solid mixture, stirring and mixing for 1h at room temperature, performing suction filtration, taking the solid, repeatedly washing the solid with the tetrahydrofuran until the washing liquid is colorless, and drying the solid in an oven at 80 ℃ for 30min to obtain the ultra-high molecular weight polyethylene/graphite composite powder;
s3: taking 3g of ultrahigh molecular weight polyethylene/graphite composite powder and 50mL of tetrahydrofuran, and carrying out ball milling and dispersion for 10min to obtain ultrahigh molecular weight polyethylene/graphite composite slurry;
s4: pouring the ultra-high molecular weight polyethylene/graphite composite slurry on a polytetrafluoroethylene film, carrying out blade coating to form a film, heating to 220 ℃ after tetrahydrofuran is completely volatilized, and carrying out hot pressing treatment to obtain the ultra-high molecular weight polyethylene/graphite composite material, wherein the mass content of graphite is 20%.
Example 3
The embodiment provides an ultrahigh molecular weight polyethylene/graphite composite material, and a preparation method thereof comprises the following steps:
s1: stirring by using a magnetic stirrer, heating to 160 ℃ in an oil bath to melt 250g of phenol, simultaneously adding 2.1g of ultra-high molecular weight polyethylene (molecular weight is 330 ten thousand) and 0.9g of graphite powder (diameter is about 2.6 mu m) under the condition of 300W ultrasonic dispersion, uniformly mixing by ultrasonic 30min, stopping heating, and naturally cooling to obtain a solid mixture;
s2: adding 1000mL of tetrahydrofuran into the solid mixture, stirring and mixing for 1h at room temperature, performing suction filtration, taking the solid, repeatedly washing the solid with the tetrahydrofuran until the washing liquid is colorless, and drying the solid in an oven at 80 ℃ for 30min to obtain the ultra-high molecular weight polyethylene/graphite composite powder;
s3: taking 3g of ultrahigh molecular weight polyethylene/graphite composite powder and 50mL of tetrahydrofuran, and carrying out ball milling and dispersion for 10min to obtain ultrahigh molecular weight polyethylene/graphite composite slurry;
s4: pouring the ultra-high molecular weight polyethylene/graphite composite slurry on a polytetrafluoroethylene film, carrying out blade coating to form a film, heating to 220 ℃ after tetrahydrofuran is completely volatilized, and carrying out hot pressing treatment to obtain the ultra-high molecular weight polyethylene/graphite composite material, wherein the mass content of graphite is 30%.
Example 4
The embodiment provides an ultrahigh molecular weight polyethylene/graphite composite material, and a preparation method thereof comprises the following steps:
s1: stirring by using a magnetic stirrer, heating to 160 ℃ in an oil bath to melt 250g of phenol, simultaneously adding 1.8g of ultra-high molecular weight polyethylene (molecular weight is 330 ten thousand) and 1.2g of graphite powder (diameter is about 2.6 mu m) under the condition of 300W ultrasonic dispersion, uniformly mixing by ultrasonic 30min, stopping heating, and naturally cooling to obtain a solid mixture;
s2: adding 1000mL of tetrahydrofuran into the solid mixture, stirring and mixing for 1h at room temperature, performing suction filtration, taking the solid, repeatedly washing the solid with the tetrahydrofuran until the washing liquid is colorless, and drying the solid in an oven at 80 ℃ for 30min to obtain the ultra-high molecular weight polyethylene/graphite composite powder;
s3: taking 3g of ultrahigh molecular weight polyethylene/graphite composite powder and 50mL of tetrahydrofuran, and carrying out ball milling and dispersion for 10min to obtain ultrahigh molecular weight polyethylene/graphite composite slurry;
s4: pouring the ultra-high molecular weight polyethylene/graphite composite slurry on a polytetrafluoroethylene film, carrying out blade coating to form a film, heating to 220 ℃ after tetrahydrofuran is completely volatilized, and carrying out hot pressing treatment to obtain the ultra-high molecular weight polyethylene/graphite composite material, wherein the mass content of graphite is 40%.
Example 5
The embodiment provides an ultrahigh molecular weight polyethylene/graphite composite material, and a preparation method thereof comprises the following steps:
s1: stirring by using a magnetic stirrer, heating to 160 ℃ in an oil bath to melt 250g of phenol, simultaneously adding 1.5g of ultra-high molecular weight polyethylene (with the molecular weight of 330 ten thousand) and 1.5g of graphite powder (with the diameter of about 2.6 mu m) under the condition of 300W ultrasonic dispersion, performing ultrasonic mixing for 30min, stopping heating, and naturally cooling to obtain a solid mixture;
s2: adding 1000mL of tetrahydrofuran into the solid mixture, stirring and mixing for 1h at room temperature, performing suction filtration, taking the solid, repeatedly washing the solid with the tetrahydrofuran until the washing liquid is colorless, and drying the solid in an oven at 80 ℃ for 30min to obtain the ultra-high molecular weight polyethylene/graphite composite powder;
s3: taking 3g of ultrahigh molecular weight polyethylene/graphite composite powder and 50mL of tetrahydrofuran, and carrying out ball milling and dispersion for 10min to obtain ultrahigh molecular weight polyethylene/graphite composite slurry;
s4: pouring the ultra-high molecular weight polyethylene/graphite composite slurry on a polytetrafluoroethylene film, carrying out blade coating to form a film, heating to 220 ℃ after tetrahydrofuran is completely volatilized, and carrying out hot pressing treatment to obtain the ultra-high molecular weight polyethylene/graphite composite material, wherein the mass content of graphite is 50%.
Comparative example 1
The comparative example provides an ultra-high molecular weight polyethylene material, and the preparation method comprises the following steps:
s1: stirring by using a magnetic stirrer, heating to 160 ℃ in an oil bath to melt 250g of phenol, adding 3g of ultra-high molecular weight polyethylene (with the molecular weight of 330 ten thousand) under the condition of 300W ultrasonic dispersion, performing ultrasonic mixing for 30min, stopping heating, and naturally cooling to obtain a solid mixture;
s2: adding 1000mL of tetrahydrofuran into the solid mixture, stirring and mixing for 1h at room temperature, carrying out suction filtration, taking the solid, repeatedly washing the solid with the tetrahydrofuran until the washing liquid is colorless, and drying the solid in an oven at 80 ℃ for 30min to obtain ultrahigh molecular weight polyethylene powder;
s3: taking 3g of ultra-high molecular weight polyethylene powder and 50mL of tetrahydrofuran, and carrying out ball milling and dispersion for 10min to obtain ultra-high molecular weight polyethylene slurry;
s4: pouring the ultra-high molecular weight polyethylene slurry on a polytetrafluoroethylene film, blade-coating to form a film, heating to 220 ℃ after tetrahydrofuran is completely volatilized, and carrying out hot pressing treatment to obtain the ultra-high molecular weight polyethylene material, wherein the mass content of graphite is 0%.
Comparative example 2
The comparative example provides an ultra-high molecular weight polyethylene/graphite composite, xylene is used as a modifier, ultra-high molecular weight polyethylene and graphite are mixed in a solution compounding manner, and the preparation method of the ultra-high molecular weight polyethylene/graphite composite comprises the following steps:
290.7mL (250g) of xylene is heated to 160 ℃, then 2.7g of ultra-high molecular weight polyethylene (molecular weight is 330 ten thousand) and 0.3g of graphite powder (diameter is about 2.6 mu m) are added simultaneously, ultrasonic treatment is carried out for 30min, heating is stopped, natural cooling is carried out, and drying is carried out, thus obtaining paste, namely the ultra-high molecular weight polyethylene/graphite composite.
Sample characterization
Sample appearance analysis was performed on the ultra-high molecular weight polyethylene/graphite composite powder prepared in step S2 of example 1 and the ultra-high molecular weight polyethylene/graphite composite prepared in comparative example 2.
Fig. 1 is an appearance diagram of a sample of the ultra-high molecular weight polyethylene/graphite composite powder and the ultra-high molecular weight polyethylene/graphite composite, fig. a is an appearance diagram of a sample of the ultra-high molecular weight polyethylene/graphite composite powder prepared in step S2 of example 1, and fig. B is an appearance diagram of a sample of the ultra-high molecular weight polyethylene/graphite composite prepared in comparative example 2. As shown in fig. 1, when xylene is used as a modifier to compound ultra-high molecular weight polyethylene and graphite, ultra-high molecular weight polyethylene and graphite are not uniformly compounded due to difficulty in stretching molecular chains of the ultra-high molecular weight polyethylene and agglomeration of the graphite, so that a black paste-like ultra-high molecular weight polyethylene/graphite compound is generated; when the phenol is used as the modifier to compound the ultrahigh molecular weight polyethylene and the graphite, the molecular chain of the ultrahigh molecular weight polyethylene is fully stretched, the graphite is uniformly dispersed in the ultrahigh molecular weight polyethylene, and the ultrahigh molecular weight polyethylene and the graphite are uniformly compounded to obtain uniform and stable gray powder-shaped ultrahigh molecular weight polyethylene/graphite composite powder.
Performance testing
Differential Scanning Calorimetry (DSC) temperature-rising melting, DSC temperature-lowering crystallization, electrical conductivity and mechanical property analysis are carried out on the samples prepared in examples 1-5 and comparative example 1.
TABLE 1 DSC elevated temperature melting test and DSC reduced temperature crystallization test results for samples prepared in examples 1-5 and comparative example 1
FIG. 2 is a Differential Scanning Calorimetry (DSC) temperature rise melting curve of the ultra-high molecular weight polyethylene/graphite composite materials of examples 1-5 and the ultra-high molecular weight polyethylene material of comparative example 1. FIG. 3 is a Differential Scanning Calorimetry (DSC) temperature decreasing crystallization curve of the ultra-high molecular weight polyethylene/graphite composite materials of examples 1-5 and the ultra-high molecular weight polyethylene material of comparative example 1. As can be seen from table 1 and fig. 2 to 3, in the process of compounding the ultra-high molecular weight polyethylene and graphite, the addition of the graphite plays a role of heterogeneous nucleation, so that the melting temperature of the ultra-high molecular weight polyethylene/graphite composite material is reduced, and the crystallinity and crystallization temperature of the ultra-high molecular weight polyethylene/graphite composite material are increased, thereby obtaining the ultra-high molecular weight polyethylene/graphite composite material with excellent performance.
FIG. 4 is a line graph showing the electrical conductivity of the ultrahigh molecular weight polyethylene/graphite composite materials of examples 1 to 5 having different graphite contents by mass. As shown in fig. 4, as the mass content of graphite increases, the conductivity of the ultra-high molecular weight polyethylene/graphite composite material increases, which indicates that the mass content of graphite is in positive correlation with the conductivity of the ultra-high molecular weight polyethylene/graphite composite material, and when the mass content of graphite is 10% -50%, the conductivity of the ultra-high molecular weight polyethylene/graphite composite material is 0.122-5.8 s-cm -1 。
TABLE 2 mechanical Property test results of samples prepared in examples 1 to 5 and comparative example 1
FIG. 5 is a graph showing the trend of mechanical properties of the ultrahigh molecular weight polyethylene/graphite composite materials of examples 1 to 5 and the ultrahigh molecular weight polyethylene material of comparative example 1. It can be seen from table 2 and fig. 5 that, as the mass content of graphite increases, the tensile strength and the tensile modulus of the ultra-high molecular weight polyethylene/graphite composite material both increase, and the increase rate of the tensile modulus is much greater than that of the tensile strength, that is, the mechanical properties of the ultra-high molecular weight polyethylene material are enhanced by adding graphite.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The preparation method of the ultra-high molecular weight polyethylene/graphite composite material is characterized by comprising the following steps:
s1: heating and melting the modifier, mixing the modifier with the ultra-high molecular weight polyethylene and graphite, and cooling to obtain a solid mixture;
s2: removing the modifier in the solid mixture to obtain ultra-high molecular weight polyethylene/graphite composite powder;
s3: mixing the ultra-high molecular weight polyethylene/graphite composite powder with tetrahydrofuran or dimethylbenzene to obtain ultra-high molecular weight polyethylene/graphite composite slurry;
s4: smearing the ultra-high molecular weight polyethylene/graphite composite slurry, and carrying out hot pressing treatment to obtain an ultra-high molecular weight polyethylene/graphite composite material;
wherein, in the step S1, the modifier is one or two of phenol or 1,2, 3-trichlorobenzene.
2. The method of claim 1, wherein the step S1 is to heat the modifier by stirring with a magnetic stirrer, add the ultra-high molecular weight polyethylene and graphite under ultrasonic dispersion, mix them uniformly, stop heating, and cool them naturally to obtain a solid mixture.
3. The method for preparing the ultra-high molecular weight polyethylene/graphite composite material according to any one of claims 1 to 2, wherein the ultra-high molecular weight polyethylene has a molecular weight of 250 to 400 ten thousand in step S1.
4. The method for preparing the ultra-high molecular weight polyethylene/graphite composite material according to any one of claims 1 to 2, wherein the graphite in the step S1 is one or more of graphite powder, graphite flakes or graphene oxide.
5. The method for preparing the ultrahigh molecular weight polyethylene/graphite composite material according to any one of claims 1 to 2, wherein the mass ratio of the graphite to the ultrahigh molecular weight polyethylene in step S1 is 1:1 to 1: 9.
6. The method for preparing the ultrahigh molecular weight polyethylene/graphite composite material according to any one of claims 1 to 2, wherein the mass ratio of the modifier to the ultrahigh molecular weight polyethylene in the step S1 is 2500 (15-27).
7. The method for preparing the ultra-high molecular weight polyethylene/graphite composite material according to claim 1, wherein the step S2 is specifically to mix the solid mixture with tetrahydrofuran by stirring, pump-filtering, taking the solid, washing with tetrahydrofuran, and drying to obtain the ultra-high molecular weight polyethylene/graphite composite powder.
8. The method for preparing the ultra-high molecular weight polyethylene/graphite composite material according to claim 1, wherein the step S3 is specifically to obtain the ultra-high molecular weight polyethylene/graphite composite slurry by dispersing the ultra-high molecular weight polyethylene/graphite composite powder and tetrahydrofuran or xylene through ball milling.
9. The method for preparing the ultra-high molecular weight polyethylene/graphite composite material according to claim 1, wherein the step S4 is to pour the ultra-high molecular weight polyethylene/graphite composite slurry on a substrate, blade-coat the slurry into a film, and perform hot-pressing treatment to obtain the ultra-high molecular weight polyethylene/graphite composite material.
10. An ultra-high molecular weight polyethylene/graphite composite material, characterized by being prepared by the preparation method of any one of claims 1 to 9.
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