CN108423664A - A kind of preparation method of phosphorus alkene-graphene composite material - Google Patents
A kind of preparation method of phosphorus alkene-graphene composite material Download PDFInfo
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- CN108423664A CN108423664A CN201810384310.6A CN201810384310A CN108423664A CN 108423664 A CN108423664 A CN 108423664A CN 201810384310 A CN201810384310 A CN 201810384310A CN 108423664 A CN108423664 A CN 108423664A
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- phosphorus alkene
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- phosphorus
- alkene
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- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 101
- 239000011574 phosphorus Substances 0.000 title claims abstract description 101
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002131 composite material Substances 0.000 title claims abstract description 87
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 31
- 239000010439 graphite Substances 0.000 claims abstract description 31
- 238000002604 ultrasonography Methods 0.000 claims abstract description 24
- 241000446313 Lamella Species 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000006228 supernatant Substances 0.000 claims abstract description 22
- 239000000725 suspension Substances 0.000 claims abstract description 22
- 150000001336 alkenes Chemical class 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002608 ionic liquid Substances 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 5
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 150000002357 guanidines Chemical class 0.000 claims description 2
- 150000002460 imidazoles Chemical group 0.000 claims description 2
- 150000002916 oxazoles Chemical class 0.000 claims description 2
- 150000004714 phosphonium salts Chemical class 0.000 claims description 2
- 150000003053 piperidines Chemical class 0.000 claims description 2
- 150000003217 pyrazoles Chemical class 0.000 claims description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 2
- CZNJIWCDRJWKLG-UHFFFAOYSA-N 1-hydroperoxy-2-propan-2-ylbenzene Chemical compound CC(C)C1=CC=CC=C1OO CZNJIWCDRJWKLG-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract 1
- -1 Phosphorus alkene Chemical class 0.000 description 39
- 238000005119 centrifugation Methods 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 11
- 239000002023 wood Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 125000004437 phosphorous atom Chemical group 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 210000003739 neck Anatomy 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 150000004040 pyrrolidinones Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 206010068052 Mosaicism Diseases 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- YQHLDYVWEZKEOX-UHFFFAOYSA-N cumene hydroperoxide Chemical compound OOC(C)(C)C1=CC=CC=C1 YQHLDYVWEZKEOX-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960001760 dimethyl sulfoxide Drugs 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 210000003765 sex chromosome Anatomy 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/003—Phosphorus
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention relates to a kind of preparation methods of phosphorus alkene graphene composite material, belong to technical field of composite materials.The present invention respectively by lamella black phosphorus and Sheet Graphite grind into powder, be added in solvent be uniformly mixed obtain mixed liquor A；Wherein solvent is deionized water, organic solvent or ionic liquid；Mixed liquor A is subjected to 0.5 ~ 2h of ultrasound pretreatment；Using the air in inert gas emptying high pressure homogenizer, the pretreated mixed liquor A of ultrasound is placed in high pressure homogenizer, carrying out 5 ~ 60min of high-pressure homogeneous processing under the conditions of pressure is 500 ~ 4000bar obtains suspension；Suspension is centrifugally separating to obtain precipitation and supernatant；Supernatant is freeze-dried or is filtered by vacuum and is drying to obtain phosphorus alkene graphene composite material.There is phosphorus alkene graphene composite material prepared by the present invention good electric conductivity, thermal conductivity and flexibility, large specific surface area, high stability, the method for the present invention to have the characteristics that easy to operate, efficient, continuous operation, equipment requirement are low.
Description
Technical field
The present invention relates to a kind of preparation methods of phosphorus alkene-graphene composite material, belong to technical field of composite materials.
Background technology
Phosphorus alkene refers to the black phosphorus of few layer, is a kind of two-dimensional material, and it is excellent that a large amount of theoretical and experimental study shows that phosphorus alkene has
Different performance, such as higher carrier mobility and the adjustable direct band gap of on-off ratio, the number of plies, the anisotropy of height, pole
Good biocompatibility etc., in necks such as solar cell, energy-storage battery, biological medicine, field-effect transistor, sensor, catalysis
Domain has shown huge potential using value.Graphene is also a kind of two-dimensional material haveing excellent performance, especially by machinery
The graphene of stripping, the properties such as good optics, mechanics, calorifics make it have good application prospect in each field.The two is answered
The advantages of obtained phosphorus alkene-graphene composite material can have both the two simultaneously is closed, has shown in numerous areas and has answered well
With foreground, great Development volue.
The preparation method of current phosphorus alkene-graphene composite material is mainly by first preparing single phosphorus alkene, graphite
Alkene dispersion liquid, then again by the two physical mixed.And the method for phosphorus alkene, graphene is prepared mostly using liquid phase ultrasound, this side
Time-consuming for method, and low yield, while being difficult prepared by serialization, is not suitable for extensive prepare.It is reported in phosphorus alkene according to pertinent literature
Each phosphorus atoms and 3 phosphorus atoms of surrounding connected in a manner of covalent bond, therefore each phosphorus atoms are outer that there are two lonely electricity
Son, it is easy to and the oxygen reaction in air, cause phosphorus alkene easily to be aoxidized, and the mode of physical mixed is difficult to solve the stabilization of phosphorus alkene
Sex chromosome mosaicism.
Invention content
The problem of existing for the above-mentioned prior art and deficiency, the present invention provide a kind of phosphorus alkene-graphene composite material
Preparation method, the present invention use high pressure homogenizer, when material being made to pass through homogeneous chamber, at the same by high speed shear, high frequency oscillation and
The effects that convection current is hit, a step realize phosphorus alkene, graphene stripping with it is compound, while phosphorus alkene graphene can also be made to form bonding work
With improving the stability of composite material.Phosphorus alkene-graphene composite material prepared by the present invention has good electric conductivity, heat conduction
Property and flexibility, large specific surface area, high stability, the method for the present invention have easy to operate, efficient, continuous operation, equipment
It is required that the features such as low.
A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by lamella black phosphorus and Sheet Graphite grind into powder, be added in solvent be uniformly mixed obtain mixed liquor A；Its
Middle solvent is deionized water, organic solvent or ionic liquid；
（2）By step（1）Gained mixed liquor A carries out 0.5 ~ 2h of ultrasound pretreatment；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out 5 ~ 60min of high-pressure homogeneous processing under the conditions of pressure is 500 ~ 4000bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；
（5）By step（4）Gained supernatant is freeze-dried or is dried in vacuo up to phosphorus alkene-graphene composite material；
The lamella black phosphorus is phosphorus alkene；
The step（1）The mass ratio of lamella black phosphorus and Sheet Graphite is (4 ~ 0.5):1；
The step（1）Organic solvent is N-Methyl pyrrolidone, n-vinyl pyrrolidone, N,N-dimethylformamide, two
Methyl sulfoxide, o-dichlorohenzene, cumyl hydroperoxide, alcohols or ethers；
The step（1）Ionic liquid be imidazoles, quaternary ammonium salt, pyroles, piperidines, pyrazoles, morpholine Lei, oxazoles class,
Guanidine salt class, sulfonium salt class or quaternary phosphonium salt class；
The step（2）Middle ultrasonic power is 100 ~ 300W；
There is P-C keys in phosphorus alkene-graphene composite material of the present invention；It is detected through EDS, in phosphorus alkene-graphene composite material
The mass percent of phosphorus alkene is 10 ~ 90%.
The beneficial effects of the invention are as follows：
（1）The present invention uses high pressure homogenizer, when material being made to pass through homogeneous chamber, while by high speed shear, high frequency oscillation and right
The effects that stream is hit, a step realize stripping and compound, the lone electron and carbon while stripping outside phosphorus atoms of phosphorus alkene, graphene
Atom combines and forms covalent bond P-C keys, improves the stability of composite material；
（2）Phosphorus alkene-graphene composite material prepared by the present invention has good electric conductivity, thermal conductivity and flexibility, specific surface area
Greatly, high stability can be used for the necks such as solar cell, energy-storage battery, biological medicine, field-effect transistor, sensor, catalysis
Domain；
（3）The method of the present invention has the characteristics that easy to operate, efficient, continuous operation, equipment requirement are low.
Description of the drawings
Fig. 1 is the XRD spectrum of phosphorus alkene-graphene composite material of the preparation of embodiment 1, phosphorus alkene, graphene；
Fig. 2 is the transmission electron microscope picture of phosphorus alkene-graphene composite material prepared by embodiment 1, and wherein a is that phosphorus alkene-graphene is compound
The transmission electron microscope picture of material；B is the transmission electron microscope enlarged drawing of phosphorus alkene-graphene composite material；C is phosphorus alkene-graphene composite wood
The high power electron microscope of material, d are the electron diffraction diagram of phosphorus alkene-graphene composite material；
Fig. 3 is the Raman figure of phosphorus alkene-graphene composite material prepared by embodiment 1；
Fig. 4 is the XPS figures of phosphorus alkene-graphene composite material prepared by embodiment 1.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1：A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by 100mg lamellas black phosphorus and 100mg Sheet Graphite grind into powder, it is added to 200mL solvents（Solvent is to go
Ionized water）In be uniformly mixed obtain mixed liquor A；Wherein the mass ratio of lamella black phosphorus and Sheet Graphite is 1:1；
（2）By step（1）Gained mixed liquor A carries out ultrasound pretreatment 0.5h；Wherein ultrasonic power is 300W；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out high-pressure homogeneous processing 5min under the conditions of pressure is 1000bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；Wherein centrifugation rate is 1000rpm, centrifugation
Time 10min；
（5）By step（4）Gained supernatant is freeze-dried up to phosphorus alkene-graphene composite material；
The XRD spectrum of phosphorus alkene-graphene composite material phosphorus alkene, graphene obtained by the present embodiment is as shown in Figure 1, from fig. 1, it can be seen that single
One phosphorus alkene is in 300 ~ 500cm-1Between there are three absorption peak, single graphene is in 1200 ~ 2800cm-1Between also there are three absorb
Also there is the absorption peak of phosphorus alkene and graphene in phosphorus alkene/graphene composite material in peak, illustrates that high pressure homogenizer well will
Phosphorus alkene and graphene have carried out compound；
The transmission electron microscope picture of phosphorus alkene-graphene composite material obtained by the present embodiment is as shown in Figure 2（A is phosphorus alkene-graphene composite wood
The transmission electron microscope picture of material；B is the transmission electron microscope enlarged drawing of phosphorus alkene-graphene composite material；C is phosphorus alkene-graphene composite material
High power electron microscope, d be phosphorus alkene-graphene composite material electron diffraction diagram）, as can be seen from Figure 2, a, b show the composite material
Lamella it is relatively thin, illustrate high pressure homogenization method prepare phosphorus alkene/graphene composite material quality it is preferable；From c figure this it appears that
Lattice fringe illustrates that composite material is sheared in high pressure homogenizer, hit repeatedly, but is not damaged to its structure, d
Electronic diffraction collection of illustrative plates illustrate that composite material still maintains intact crystallinity；
The Raman figure of phosphorus alkene-graphene composite material obtained by the present embodiment is as shown in figure 3, as can be seen from Figure 3, and three relative to phosphorus alkene
A Raman signatures go out peak position, have it is different degrees of to low frequency range deviate, illustrate that high pressure homogenization method is preparing phosphorus alkene/graphite
P-C keys are formd when alkene composite material；
The XPS figures of phosphorus alkene-graphene composite material obtained by the present embodiment are as shown in figure 4, as can be seen from Figure 4, be located at 132.27eV
There is the peak that faint peak is P-C keys；
Therefore there is P-C keys in the present embodiment phosphorus alkene-graphene composite material；It is detected through EDS, phosphorus alkene-graphene composite material
The mass percent of middle phosphorus alkene is 50%.
Embodiment 2：A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by 100mg lamellas black phosphorus and 200mg Sheet Graphite grind into powder, it is added to 200mL solvents（Solvent is to go
Ionized water）In be uniformly mixed obtain mixed liquor A；Wherein the mass ratio of lamella black phosphorus and Sheet Graphite is 0.5:1；
（2）By step（1）Gained mixed liquor A carries out ultrasound pretreatment 1h；Wherein ultrasonic power is 200W；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out high-pressure homogeneous processing 30min under the conditions of pressure is 1000bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；Wherein centrifugation rate is 3000rpm, centrifugation
Time 20min；
（5）By step（4）Gained supernatant is freeze-dried up to phosphorus alkene-graphene composite material；
Phosphorus alkene-graphene the composite wood learnt that black phosphorus alkene realizes compound with graphene in the present embodiment after testing, and obtained
Expect that its structure is not destroyed, maintain perfect crystallinity, there are P-C keys in composite material；It is detected through EDS, phosphorus alkene-graphite
The mass percent of phosphorus alkene is 35% in alkene composite material.
Embodiment 3：A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by 200mg lamellas black phosphorus and 400mg Sheet Graphite grind into powder, it is added to 300mL solvents（Solvent is to go
Ionized water）In be uniformly mixed obtain mixed liquor A；Wherein the mass ratio of lamella black phosphorus and Sheet Graphite is 0.5:1；
（2）By step（1）Gained mixed liquor A carries out ultrasound pretreatment 2h；Wherein ultrasonic power is 100W；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out high-pressure homogeneous processing 60min under the conditions of pressure is 4000bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；Wherein centrifugation rate is 10000rpm, from
Heart time 30min；
（5）By step（4）Gained supernatant is dried in vacuo up to phosphorus alkene-graphene composite material；
Black phosphorus alkene realizes phosphorus alkene-graphene composite wood that is compound, and obtaining with graphene in the present embodiment known to after testing
Expect that its structure is not destroyed, maintain perfect crystallinity, there are P-C keys in composite material；It is detected through EDS, phosphorus alkene-graphite
The mass percent of phosphorus alkene is 37% in alkene composite material.
Embodiment 4：A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by 10mg lamellas black phosphorus and 100mg Sheet Graphite grind into powder, it is added to 300mL solvents（Solvent is N- first
Base pyrrolidones）In be uniformly mixed obtain mixed liquor A；Wherein the mass ratio of lamella black phosphorus and Sheet Graphite is 0.1:1；
（2）By step（1）Gained mixed liquor A carries out ultrasound pretreatment 2h；Wherein ultrasonic power is 150W；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out high-pressure homogeneous processing 30min under the conditions of pressure is 500bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；Wherein centrifugation rate is 10000rpm, from
Heart time 30min；
（5）By step（4）Gained supernatant is dried in vacuo up to phosphorus alkene-graphene composite material；
Black phosphorus alkene realizes phosphorus alkene-graphene composite wood that is compound, and obtaining with graphene in the present embodiment known to after testing
Expect that its structure is not destroyed, maintain perfect crystallinity, there are P-C keys in composite material；It is detected through EDS, phosphorus alkene-graphite
The mass percent of phosphorus alkene is 15% in alkene composite material.
Embodiment 5：A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by 90mg lamellas black phosphorus and 10mg Sheet Graphite grind into powder, it is added to 50mL solvents（Solvent is N- methyl
Pyrrolidones）In be uniformly mixed obtain mixed liquor A；Wherein the mass ratio of lamella black phosphorus and Sheet Graphite is 9:1；
（2）By step（1）Gained mixed liquor A carries out ultrasound pretreatment 2h；Wherein ultrasonic power is 150W；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out high-pressure homogeneous processing 30min under the conditions of pressure is 500bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；Wherein centrifugation rate is 9000rpm, centrifugation
Time 30min；
（5）By step（4）Gained supernatant is dried in vacuo up to phosphorus alkene-graphene composite material；
Black phosphorus alkene realizes phosphorus alkene-graphene composite wood that is compound, and obtaining with graphene in the present embodiment known to after testing
Expect that its structure is not destroyed, maintain perfect crystallinity, there are P-C keys in composite material；It is detected through EDS, phosphorus alkene-graphite
The mass percent of phosphorus alkene is 90% in alkene composite material.
Embodiment 6：A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by 10mg lamellas black phosphorus and 100mg Sheet Graphite grind into powder, it is added to 300mL solvents（Solvent is N- first
Base pyrrolidones）In be uniformly mixed obtain mixed liquor A；Wherein the mass ratio of lamella black phosphorus and Sheet Graphite is 0.1:1；
（2）By step（1）Gained mixed liquor A carries out ultrasound pretreatment 2h；Wherein ultrasonic power is 150W；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out high-pressure homogeneous processing 30min under the conditions of pressure is 500bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；Wherein centrifugation rate is 10000rpm, from
Heart time 30min；
（5）By step（4）Gained supernatant is dried in vacuo up to phosphorus alkene-graphene composite material；
Black phosphorus alkene realizes phosphorus alkene-graphene composite wood that is compound, and obtaining with graphene in the present embodiment known to after testing
Expect that its structure is not destroyed, maintain perfect crystallinity, there are P-C keys in composite material；It is detected through EDS, phosphorus alkene-graphite
The mass percent of phosphorus alkene is 12% in alkene composite material.
Embodiment 7：A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by 200mg lamellas black phosphorus and 100mg Sheet Graphite grind into powder, it is added to 300mL solvents（Solvent is 1-
- 3 methylimidazole of alkyl）In be uniformly mixed obtain mixed liquor A；Wherein the mass ratio of lamella black phosphorus and Sheet Graphite is 2:1；
（2）By step（1）Gained mixed liquor A carries out ultrasound pretreatment 2h；Wherein ultrasonic power is 200W；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out high-pressure homogeneous processing 30min under the conditions of pressure is 3000bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；Wherein centrifugation rate is 10000rpm, from
Heart time 30min；
（5）By step（4）Gained supernatant is dried in vacuo up to phosphorus alkene-graphene composite material；
Black phosphorus alkene realizes phosphorus alkene-graphene composite wood that is compound, and obtaining with graphene in the present embodiment known to after testing
Expect that its structure is not destroyed, maintain perfect crystallinity, there are P-C keys in composite material；It is detected through EDS, phosphorus alkene-graphite
The mass percent of phosphorus alkene is 65% in alkene composite material.
Embodiment 8：A kind of preparation method of phosphorus alkene-graphene composite material, is as follows：
（1）Respectively by 500mg lamellas black phosphorus and 100mg Sheet Graphite grind into powder, it is added to 500mL solvents（Solvent is 1-
Butyl -3- methyl imidazolium tetrafluoroborates）In be uniformly mixed obtain mixed liquor A；The wherein quality of lamella black phosphorus and Sheet Graphite
Than being 5:1；
（2）By step（1）Gained mixed liquor A carries out ultrasound pretreatment 2h；Wherein ultrasonic power is 250W；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out high-pressure homogeneous processing 30min under the conditions of pressure is 2500bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；Wherein centrifugation rate is 10000rpm, from
Heart time 30min；
（5）By step（4）Gained supernatant is dried in vacuo up to phosphorus alkene-graphene composite material；
Black phosphorus alkene realizes phosphorus alkene-graphene composite wood that is compound, and obtaining with graphene in the present embodiment known to after testing
Expect that its structure is not destroyed, maintain perfect crystallinity, there are P-C keys in composite material；It is detected through EDS, phosphorus alkene-graphite
The mass percent of phosphorus alkene is 85% in alkene composite material.
The specific implementation mode of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art
Go out various change.
Claims (6)
1. a kind of preparation method of phosphorus alkene-graphene composite material, which is characterized in that be as follows：
（1）Respectively by lamella black phosphorus and Sheet Graphite grind into powder, be added in solvent be uniformly mixed obtain mixed liquor A；Its
Middle solvent is deionized water, organic solvent or ionic liquid；
（2）By step（1）Gained mixed liquor A carries out 0.5 ~ 2h of ultrasound pretreatment；
（3）Using the air in inert gas emptying high pressure homogenizer, by step（2）The pretreated mixed liquor A of ultrasound is placed in height
It presses in homogenizer, carrying out 5 ~ 60min of high-pressure homogeneous processing under the conditions of pressure is 500 ~ 4000bar obtains suspension；
（4）By step（3）Gained suspension is centrifugally separating to obtain precipitation and supernatant；
（5）By step（4）Gained supernatant is freeze-dried or is dried in vacuo up to phosphorus alkene-graphene composite material.
2. the preparation method of phosphorus alkene-graphene composite material according to claim 1, it is characterised in that：Step（1）Lamella is black
The mass ratio of phosphorus and Sheet Graphite is (9 ~ 0.1):1.
3. the preparation method of phosphorus alkene-graphene composite material according to claim 1, it is characterised in that：Step（1）It is organic molten
Agent is N-Methyl pyrrolidone, n-vinyl pyrrolidone, N,N-dimethylformamide, dimethyl sulfoxide (DMSO), o-dichlorohenzene, isopropyl
Phenyl hydrogen peroxide, alcohols or ethers.
4. the preparation method of phosphorus alkene-graphene composite material according to claim 1, it is characterised in that：Step（1）Ionic liquid
Body is imidazoles, quaternary ammonium salt, pyroles, piperidines, pyrazoles, morpholine Lei, oxazoles class, guanidine salt class, sulfonium salt class or quaternary phosphonium salt
Class.
5. the preparation method of phosphorus alkene-graphene composite material according to claim 1, it is characterised in that：Step（2）Middle ultrasound
Wave power is 100 ~ 300W.
6. phosphorus alkene-graphite prepared by the preparation method of the claim 1 ~ 5 any one phosphorus alkene-graphene composite material
Alkene composite material.
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