CN106564962A - Method for preparing graphene-like molybdenum disulfide-ferroferric oxide composite material through reduction for proteic substances - Google Patents
Method for preparing graphene-like molybdenum disulfide-ferroferric oxide composite material through reduction for proteic substances Download PDFInfo
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- CN106564962A CN106564962A CN201610962901.8A CN201610962901A CN106564962A CN 106564962 A CN106564962 A CN 106564962A CN 201610962901 A CN201610962901 A CN 201610962901A CN 106564962 A CN106564962 A CN 106564962A
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- powder
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- molybdenum disulfide
- intercalation
- molybdenum
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 128
- 239000011733 molybdenum Substances 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 76
- 239000002131 composite material Substances 0.000 title claims abstract description 68
- 230000009467 reduction Effects 0.000 title claims abstract description 24
- 239000000126 substance Substances 0.000 title abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 146
- 238000003756 stirring Methods 0.000 claims abstract description 98
- 238000009830 intercalation Methods 0.000 claims abstract description 77
- 230000002687 intercalation Effects 0.000 claims abstract description 77
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 71
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- 238000006722 reduction reaction Methods 0.000 claims abstract description 38
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002243 precursor Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 21
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 85
- 229910021389 graphene Inorganic materials 0.000 claims description 81
- 239000000243 solution Substances 0.000 claims description 79
- 102000004169 proteins and genes Human genes 0.000 claims description 38
- 108090000623 proteins and genes Proteins 0.000 claims description 38
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 38
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 34
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 19
- 235000010344 sodium nitrate Nutrition 0.000 claims description 19
- 239000004317 sodium nitrate Substances 0.000 claims description 19
- 235000011149 sulphuric acid Nutrition 0.000 claims description 19
- 239000001117 sulphuric acid Substances 0.000 claims description 19
- 229910052786 argon Inorganic materials 0.000 claims description 18
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims description 18
- 229910021529 ammonia Inorganic materials 0.000 claims description 17
- AYFVYJQAPQTCCC-UHFFFAOYSA-N Threonine Natural products CC(O)C(N)C(O)=O AYFVYJQAPQTCCC-UHFFFAOYSA-N 0.000 claims description 12
- 239000004473 Threonine Substances 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims description 11
- COLNVLDHVKWLRT-QMMMGPOBSA-N phenylalanine group Chemical group N[C@@H](CC1=CC=CC=C1)C(=O)O COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 9
- 239000011593 sulfur Substances 0.000 claims description 9
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 claims description 8
- 230000014759 maintenance of location Effects 0.000 claims description 8
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 claims description 6
- 125000000430 tryptophan group Chemical group [H]N([H])C(C(=O)O*)C([H])([H])C1=C([H])N([H])C2=C([H])C([H])=C([H])C([H])=C12 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical group OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 125000000341 threoninyl group Chemical group [H]OC([H])(C([H])([H])[H])C([H])(N([H])[H])C(*)=O 0.000 claims description 2
- VAJVDSVGBWFCLW-UHFFFAOYSA-N 3-Phenyl-1-propanol Chemical compound OCCCC1=CC=CC=C1 VAJVDSVGBWFCLW-UHFFFAOYSA-N 0.000 claims 1
- 241000040710 Chela Species 0.000 claims 1
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropyl alcohol Natural products CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract description 36
- 230000009920 chelation Effects 0.000 abstract 1
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 39
- 239000010410 layer Substances 0.000 description 32
- 239000003643 water by type Substances 0.000 description 30
- 229940056319 ferrosoferric oxide Drugs 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 19
- 239000002114 nanocomposite Substances 0.000 description 19
- 238000010792 warming Methods 0.000 description 19
- 235000015165 citric acid Nutrition 0.000 description 17
- 238000010438 heat treatment Methods 0.000 description 16
- 238000012512 characterization method Methods 0.000 description 15
- 150000002823 nitrates Chemical class 0.000 description 14
- 239000012065 filter cake Substances 0.000 description 13
- 238000005987 sulfurization reaction Methods 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 7
- 238000001069 Raman spectroscopy Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000002356 single layer Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 229910052961 molybdenite Inorganic materials 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000007306 functionalization reaction Methods 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 241000446313 Lamella Species 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000009418 renovation Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 230000008685 targeting Effects 0.000 description 2
- 230000010415 tropism Effects 0.000 description 2
- 102000014914 Carrier Proteins Human genes 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- AYFVYJQAPQTCCC-GBXIJSLDSA-N L-threonine Chemical compound C[C@@H](O)[C@H](N)C(O)=O AYFVYJQAPQTCCC-GBXIJSLDSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- -1 Molybdenum sulfide-titanium dioxide compound Chemical class 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 108091008324 binding proteins Proteins 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002153 concerted effect Effects 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Materials For Photolithography (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a method for preparing a graphene-like molybdenum disulfide-ferroferric oxide composite material through reduction for proteic substances. The method comprises the following steps: adding a molybdenum disulfide powder in an intercalation solution and carrying out an intercalation reaction, and filtering and drying after the reaction is finished to obtain an intercalation molybdenum disulfide powder; mixing the intercalation molybdenum disulfide powder prepared in the step 1 with the proteic substances and water, uniformly stirring, drying and grinding to obtain a precursor powder; mixing ferric nitrate with citric acid and then adding the mixture in water, and carrying out a chelation reaction to obtain a yellow sol solution; adding the precursor powder in the yellow sol solution, stirring and mixing to obtain a mixed gel, drying and grinding to obtain a dry gel powder; and carrying out a reduction reaction on the dry gel powder under a protective gas, cooling after the reaction is complete, and taking out a reaction product. The method provided by the invention realizes peeling for molybdenum disulfide and generation for ferroferric oxide simultaneously, and finishes a compounding process of graphene-like molybdenum disulfide and ferroferric oxide in one step.
Description
Technical field
The invention belongs to New Two Dimensional Material Field, is related to class Graphene molybdenum bisuphide composite, and in particular to a kind of
The method that protein matter reduction prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material.
Background technology
Class Graphene molybdenum bisuphide (the Graphene-like MoS being made up of few layer of molybdenum bisuphide2) it is that one kind has class
Like New Two Dimensional (2D) lamellar compound of graphene-structured and performance, formed with its unique physics, chemical property in recent years
For emerging study hotspot.Class Graphene molybdenum bisuphide by the multilamellar molybdenum bisuphide of hexagonal crystal system constitute with " sandwich
It is sandwich " the two dimensional crystal material of layer structure, monolayer molybdenum bisuphide is made up of three layers of atomic layer, and middle one layer is molybdenum atom layer,
Two-layer is sulphur atom layer up and down, and molybdenum atom layer forms class " sandwich " structure, molybdenum atom and sulfur folded by two-layer sulphur atom layer
Atom forms two-dimensional atomic crystal with Covalent bonding together；Multilamellar molybdenum bisuphide is made up of some monolayer molybdenum bisuphide, is not typically surpassed
Five layers are crossed, interlayer has weak Van der Waals force, interlamellar spacing is about 0.65nm.
Used as the important two-dimensional layer nano material of a class, few layer molybdenum bisuphide is with " sandwich " stratiform of its uniqueness
Structure is widely used in various fields such as lubricant, catalysis, energy stores, composites.Compared to zero band gap of Graphene,
There is regulatable band gap in class Graphene molybdenum bisuphide, possess brighter prospect in field of photoelectric devices；Compared to silicon material
The three-dimensional bulk structure of material, class Graphene molybdenum bisuphide have the two-dimensional layered structure of nanoscale, can be used to manufacture and partly lead
Body or the electronic chip that specification is less, efficiency is higher, will be used widely in fields such as follow-on nano-electric devices.
Although platelike molybdenumdisulfide has good greasy property and photoelectric properties, which has in all many performances
Treat further to be lifted, by molybdenum bisuphide with other organic or inorganic microgranule compound uses, using their cooperative effect, be to be lifted
One of method of molybdenum bisuphide performance.Patent CN201410369695 disclose a kind of molybdenum bisuphide-titanium dioxide compound and
, there is collaboration lubrication and concerted catalysis effect using titanium dioxide and molybdenum bisuphide, synthesize two by chemical method in its preparation method
Molybdenum sulfide-titanium dioxide compound is to improve one of effective way of lubrication and catalytic performance of molybdenum bisuphide and titanium dioxide；
Patent of invention CN201510149438 discloses a kind of preparation method of the graphene composite film of doping monolayer curing molybdenum sheet,
By Graphene and the compound electric conductivity that can improve composite of molybdenum disulfide nano sheet, strengthen electrochemical electrode reaction and urge
Change the transmission of electronics in course of reaction, so as to improve the chemical property and catalytic performance of composite；Patent of invention
CN201510349912 discloses a kind of molybdenum bisuphide-carbon composite and preparation method thereof, using cheap titanium dioxide
Silicon grain and glucose are prepared for being applied to molybdenum bisuphide lithium cell negative pole material curing molybdenum sheet as template and base material
Layer-carbon hollow ball nano composite material, this structural composite material are conducive to the stability of holding electrode, and can shorten lithium
The transmission range of ion, is conducive to the lifting of high rate performance.
Although molybdenum bisuphide composite disclosed above is in greasy property and photoelectric properties to molybdenum bisuphide stratiform
The performance of material has very big lifting, but for the performance boost of magnetic steering and adsorbing domain does not propose effectively to solve to do
Method.
By compound with magnetic medium, such as and Fe3O4Functionalization is combined, and obtains the molybdenum bisuphide stratiform material of functionalization,
Its saturation magnetization can effectively be increased, and make it have magnetic conductance tropism energy, biocompatibility and strong adsorptivity, can be used
In fields such as living things catalysis, drug targeting, environmental renovation and desalinizations, class Graphene molybdenum bisuphide is greatly expanded
Range of application.
Patent of invention CN201210524859 discloses a kind of synthesis MoS2-Fe3O4The preparation method of nano composite material,
With Fe3O4Nano-particle is raw material, in distributing it to deionized water and adds sodium molybdate, Sodium Chloride, sodium rhodanate and surface to live
Property agent CTAB, reacts 6-10h in stainless steel cauldron, MoS is obtained after cleaning-drying2The Fe of cladding3O4Nano-particle.The party
Although method has been obtained MoS using hydro-thermal method2-Fe3O4Nano composite material, but its preparation flow is complicated, and energy consumption is big, is not suitable for work
Industry metaplasia is produced, and its product structure is MoS2The Fe of cladding3O4Nano-particle, and it is usual in adsorbing domain and photocatalysis field
Need large-area stratiform MoS2Composite, with Fe3O4Fe is needed after nano-particles reinforcement3O4Nano-particle is uniformly attached to which
On lamella, and with its functionalization, obtain modified stratiform MoS2-Fe3O4Nano composite material.In addition, MoS2The layer of stratified material
Number is fewer, and its band gap is bigger, and electron transfer efficiency is higher, and photoelectric properties are better.Therefore, explore one kind and prepare class Graphene two
The simple and easy method of molybdenum sulfide-ferriferrous oxide nano composite is very necessary.
The content of the invention
Based on problems of the prior art, it is an object of the present invention to provide prepared by a kind of reduction of protein matter
The method of class Graphene molybdenum bisuphide-ferriferrous oxide composite material, it is possible to obtain the class stone with nanoscale, superior performance
Black alkene molybdenum bisuphide-ferriferrous oxide nano composite, solves existing class Graphene molybdenum bisuphide-ferroso-ferric oxide and is combined
Material preparation flow is complicated, and energy consumption is big, not environmentally and is not suitable for industrialized production, and granular composite material granule in absorption
With the technical problem of poor performance in terms of photocatalysis.
In order to solve above-mentioned technical problem, the application is adopted the following technical scheme that and is achieved：
A kind of method that protein matter reduction prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material, the party
Method is comprised the following steps：
Step one, molybdenum disulfide powder is added in intercalation solution carries out intercalation, filters, dries after the completion of reaction
It is dry, obtain intercalation molybdenum disulfide powder；
Described intercalation solution is the mixed solution of potassium chlorate, sodium nitrate, concentrated sulphuric acid and hydrogen peroxide composition；
Described molybdenum disulfide powder and potassium chlorate, sodium nitrate, the concentrated sulphuric acid of mass concentration 98% and mass concentration 30%
Hydrogen peroxide between proportion relation be 1g：(1～4) g：(0.5～2) g：(9～40) mL：(4～20) mL；
Step 2, intercalation molybdenum disulfide powder obtained in step one is mixed and stirred for uniformly with protein matter and water,
It is dried, grinds, obtains precursor powder；
Described intercalation molybdenum disulfide powder and the proportion relation between protein matter and water are 2g：(0.25～1.25)
g：(5～30) g；
Step 3, is added to the water after ferric nitrate is mixed with citric acid, carries out chelatropic reaction, obtains sol solution；
Described ferric nitrate, the proportion relation between citric acid and deionized water are 1g：(0.8～1.2) g:(1～3) g；
Step 4, adds precursor powder in sol solution, obtains mixed gel, be dried, grind after stirring mixing
To dry gel powder；
Proportion relation between described sol solution and precursor powder is：100g：(1.7～5.5) g；
Step 5, dry gel powder carry out reduction reaction under a shielding gas, cool down after reaction completely, take out reaction and produce
Thing, obtains class Graphene molybdenum bisuphide-ferriferrous oxide composite material after grinding.
The present invention also has following distinguishing feature：
Specifically, described protein matter is TYR, tryptophan, Phenylalanine or threonine.
Preferably, described molybdenum disulfide powder is dense with potassium chlorate, sodium nitrate, the concentrated sulphuric acid of mass concentration 98% and quality
Proportion relation between the hydrogen peroxide of degree 30% is 1g：2g：1g：23mL：7mL.
Preferably, described intercalation molybdenum disulfide powder and the proportion relation between protein matter and water are 2g：0.5g：
15g。
Specifically, in step one, the process of described intercalation is：Molybdenum disulfide powder is added in mixed solution,
10～30 DEG C of 1～3h of reaction are heated to, then at 30～70 DEG C and 20～50min is stirred, stirring reaction 10 at 75～100 DEG C～
30min, then sucking filtration, drying, obtains intercalation molybdenum disulfide powder.
Specifically, in step 2, after described intercalation molybdenum disulfide powder, protein matter and water mixing and stirring,
It is dried through 6～24h at a temperature of 50～100 DEG C in drying baker, grinding obtains precursor powder.
Specifically, in step 3, the detailed process of chelatropic reaction is：It is added to the water after ferric nitrate is mixed with citric acid,
Add ammonia the pH of reaction system to be adjusted 6.5～7.5, stir 4～6h of chelatropic reaction, obtain colloidal sol molten at 45～80 DEG C
Liquid.
Specifically, in step 4, precursor powder is added in sol solution, stir 2～3.5h and obtain at 45～80 DEG C
To mixed gel, obtain xerogel after 7～15h being dried at 90～130 DEG C, xerogel is ground to into 200 mesh sieves and done
Gel powder.
Specifically, in step 5, the process of described reduction reaction is：The dry gel powder of gained in step 4 is loaded
Boat is burnt, is put in tube furnace, being continually fed into protective atmosphere carries out reduction reaction, taken out after cooling to room temperature after the completion of reaction with the furnace
Reduzate, that is, obtain class Graphene molybdenum bisuphide-bismuth molybdate composite；
When described protein matter is TYR, the temperature of reduction reaction is 280～400 DEG C, temperature retention time is 40～
90min；When described protein matter is tryptophan, the temperature of reduction reaction is 240～320 DEG C, temperature retention time is 30～
80min；When described protein matter is Phenylalanine, the temperature of reduction reaction is 250～320 DEG C, temperature retention time is 50～
120min；When described protein matter is threonine, the temperature of reduction reaction is 200～300 DEG C, temperature retention time is 40～
120min。
Preferably, described protective atmosphere is nitrogen or argon.
Compared with prior art, beneficial has the technical effect that the present invention：
(I) present invention is mixed to form presoma using protide organic carbon source and molybdenum bisuphide so that organic carbon source is inserted
Molybdenum disulfide powder interlayer increases its interfloor distance, weakens molybdenum bisuphide interlayer van der Waals interaction, binding protein organic carbon
Source heating carbonization promotes to realize the reduction of molybdenum bisuphide and peel off.
(II) present invention is reduced with the heating of protide organic carbon by sol-gel process, while realizing molybdenum bisuphide
The generation with ferroso-ferric oxide is peeled off, and a step completes the recombination process of class Graphene molybdenum bisuphide and ferroso-ferric oxide.
(III) product prepared by the present invention is the class Graphene molybdenum bisuphide with high carrier mobility and four oxidations three
The compound nano material of iron nano-particle, and Fe3O4Nano-particle is uniformly attached on monolayer molybdenum bisuphide lamella, with preferable
Magnetic conductance tropism energy, drug targeting, the field such as environmental renovation and desalinization, greatly expand the application model of molybdenum bisuphide
Enclose.
(IV) class Graphene molybdenum bisuphide-ferriferrous oxide nano composite prepared by the present invention, simple to operate, is not required to
Will complicated and loaded down with trivial details preparation facilitiess, preparation efficiency is high, and yield is big, environmental protection and is adapted to industrialized production.
Description of the drawings
Fig. 1 is the Raman collection of illustrative plates of the class Graphene molybdenum bisuphide-ferriferrous oxide nano composite in embodiment 1.
Fig. 2 is the TEM figures of the class Graphene molybdenum bisuphide-ferriferrous oxide nano composite in embodiment 1.
Fig. 3 is the XRD figure of the class Graphene molybdenum bisuphide-ferriferrous oxide nano composite in embodiment 1.
Fig. 4 is the Raman collection of illustrative plates of the molybdenum bisuphide-ferriferrous oxide nano composite in comparative example 1.
Fig. 5 is the TEM figures of the molybdenum bisuphide-ferriferrous oxide nano composite in comparative example 1.
With reference to embodiments the particular content of the present invention is described in more detail.
Specific embodiment
It should be noted that heretofore described class Graphene molybdenum bisuphide is the molybdenum bisuphide of few Rotating fields, it is described
Few Rotating fields are 1～5 layer of structure.The molecular formula of ferric nitrate is Fe (NO3)3·9H2O。
Defer to above-mentioned technical proposal, the specific embodiment of the present invention given below, it should be noted that the present invention not office
It is limited to specific examples below, all equivalents done on the basis of technical scheme each fall within the protection model of the present invention
Enclose.The present invention is described in further details with reference to embodiment.
Embodiment 1：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 20g, sodium nitrate be 10g, mass concentration 98% concentrated sulphuric acid be 230mL
Hydrogen peroxide with mass concentration 30% is 70mL；
Then heating in water bath at 30 DEG C and stirs 30min, carries out intercalation, be subsequently heated to 75 to 15 DEG C of reaction 2h
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain two sulfur of intercalation by DEG C stirring reaction 30min
Change molybdenum powder.
Step 2, takes in 0.5g TYRs addition 15g deionized waters, treats that TYR is stirring evenly and then adding into 2.0g intercalations two
Sulfuration molybdenum powder, stirs, and is dried through 8h, is ground to 200 mesh and sieves, obtain forerunner at a temperature of 60 DEG C in drying baker
Body powder.
Step 3, takes in adding 120g deionized waters after 120g ferric nitrates are mixed with 96g citric acids, adds ammonia to adjust pH
It is worth for 6.8, at 65 DEG C, after stirring chelating 6h, is obtaining yellow sol solution.
Step 4, takes 100g sol solutions and adds 2.3g precursor powders wherein, continues the stirring 3h at 65 DEG C and obtains
To mixed gel, xerogel after mixed gel is dried 8h at 100 DEG C, is obtained, and be ground to 200 mesh and sieve and done
Gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 330 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 60min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
Raman collection of illustrative plates such as Fig. 1 of class Graphene molybdenum bisuphide-ferroso-ferric oxide nano composite material prepared by the present embodiment
Shown, XRD figure is as shown in Fig. 2 high-resolution TEM figure is as shown in Figure 3.
E in Raman collection of illustrative plates in Fig. 12g 1With Ag 1Value is respectively 384.3 and 408.4, and displacement difference is 24.1, with reference to Raman spectral difference
Related article (Li H, Zhang Q, Yap C C R, the et al.From Bulk to of relation between value and the molybdenum bisuphide number of plies
Monolayer MoS2:Evolution of Raman Scattering[J].Advanced Functional
Materials,2012,22(7):1385-1390.) understand, displacement difference is less than 25, and the number of plies of the product is 1～5 layer, belongs to few
Rotating fields molybdenum bisuphide, shows the class Graphene molybdenum bisuphide that molybdenum bisuphide in composite prepared by the present embodiment is few layer.
In Fig. 2, XRD data have ferroso-ferric oxide to generate in may indicate that product.Fig. 3 middle high-resolution TEM figures are shown as few layer of class stone
Black alkene molybdenum bisuphide-ferriferrous oxide nano composite.Comprehensive accompanying drawing can show that the sample prepared by the present embodiment is class
Graphene molybdenum bisuphide-ferriferrous oxide nano composite.
Embodiment 2：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 40g, sodium nitrate be 5g, mass concentration 98% concentrated sulphuric acid be 300mL and
The hydrogen peroxide of mass concentration 30% is 60mL.
Then heating in water bath at 10 DEG C and stirs 30min, carries out intercalation, be subsequently heated to 95 to 10 DEG C of reaction 2h
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain two sulfur of intercalation by DEG C stirring reaction 25min
Change molybdenum powder.
Step 2, takes in 1.1g TYRs addition 12.5g deionized waters, treats that TYR is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder, stirs, and is dried through 7.5h, is ground to 200 mesh and sieves, obtain at a temperature of 70 DEG C in drying baker
Precursor powder.
Step 3, takes in adding 120g deionized waters after 120g ferric nitrates are mixed with 108g citric acids, adds ammonia to adjust
PH value is 7.2, is obtaining yellow sol solution at 55 DEG C after stirring chelating 4h.
Step 4, takes 100g sol solutions and adds 2.8g precursor powders, continuation to stir 2.5h at 55 DEG C wherein
Mixed gel is obtained, xerogel after mixed gel is dried 15h at 90 DEG C, is obtained, and is ground to 200 mesh and is sieved and obtain
Dry gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 300 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 80min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 3：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 10g, sodium nitrate be 8g, mass concentration 98% concentrated sulphuric acid be 400mL and
The hydrogen peroxide of mass concentration 30% is 45mL.
Then heating in water bath at 45 DEG C and stirs 50min, carries out intercalation, be subsequently heated to 98 to 30 DEG C of reaction 1h
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain two sulfur of intercalation by DEG C stirring reaction 15min
Change molybdenum powder.
Step 2, takes in 1.1g TYRs addition 25g deionized waters, treats that TYR is stirring evenly and then adding into 2.0g intercalations two
Sulfuration molybdenum powder, stirs, and is dried through 8h, is ground to 200 mesh and sieves, obtain forerunner at a temperature of 50 DEG C in drying baker
Body powder.
Step 3, takes in adding 200g deionized waters after 120g ferric nitrates are mixed with 144g citric acids, adds ammonia to adjust
PH value is 6.7, is obtaining yellow sol solution at 45 DEG C after stirring chelating 6h.
Step 4, takes 100g sol solutions and adds 3.5g precursor powders wherein, continues the stirring 2h at 45 DEG C and obtains
To mixed gel, xerogel after mixed gel is dried 12h at 110 DEG C, is obtained, and be ground to 200 mesh and sieve and done
Gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 400 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 40min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 4：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 15g, sodium nitrate be 20g, mass concentration 98% concentrated sulphuric acid be 210mL
Hydrogen peroxide with mass concentration 30% is 100mL.
Then heating in water bath at 35 DEG C and stirs 20min, carries out intercalation to 12 DEG C of reaction 2.5h, be subsequently heated to
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain intercalation two by 80 DEG C of stirring reactions 30min
Sulfuration molybdenum powder.
Step 2, takes in 0.9g TYRs addition 5g deionized waters, treats that TYR is stirring evenly and then adding into 2.0g intercalations two
Sulfuration molybdenum powder, stirs, and is dried through 7h, is ground to 200 mesh and sieves, obtain forerunner at a temperature of 90 DEG C in drying baker
Body powder.
Step 3, takes in adding 150g deionized waters after 120g ferric nitrates are mixed with 100g citric acids, adds ammonia to adjust
PH value is 6.6, is obtaining yellow sol solution at 80 DEG C after stirring chelating 5.5h.
Step 4, takes 100g sol solutions and adds 5.5g precursor powders wherein, continues the stirring 2h at 80 DEG C and obtains
To mixed gel, xerogel after mixed gel is dried 7h at 90 DEG C, is obtained, and be ground to 200 mesh and sieve and obtain dry solidifying
Rubber powder end.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through nitrogen, is warming up to 280 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 90min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 5：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 35g, sodium nitrate be 18g, mass concentration 98% concentrated sulphuric acid be 90mL and
The hydrogen peroxide of mass concentration 30% is 150mL.
Then heating in water bath at 50 DEG C and stirs 20min, carries out intercalation, be subsequently heated to 100 to 25 DEG C of reaction 3h
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain two sulfur of intercalation by DEG C stirring reaction 10min
Change molybdenum powder.
Step 2, takes in 1g tryptophans addition 28g deionized waters, treats that tryptophan is stirring evenly and then adding into two sulfur of 2.0g intercalations
Change molybdenum powder, stir, be dried through 18h at a temperature of 100 DEG C in drying baker, be ground to 200 mesh and sieve, obtain forerunner
Body powder.
Step 3, takes in adding 250g deionized waters after 120g ferric nitrates are mixed with 132g citric acids, adds ammonia to adjust
PH value is 7.2, is obtaining yellow sol solution at 80 DEG C after stirring chelating 6h.
Step 4, takes 100g sol solutions and adds 3.7g precursor powders, continuation to stir 2.5h at 80 DEG C wherein
Mixed gel is obtained, xerogel after mixed gel is dried 15h at 130 DEG C, is obtained, and is ground to 200 mesh and is sieved and obtain
Dry gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 240 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 80min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 6：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 25g, sodium nitrate be 15g, mass concentration 98% concentrated sulphuric acid be 150mL
Hydrogen peroxide with mass concentration 30% is 120mL.
Then heating in water bath at 32 DEG C and stirs 25min, carries out intercalation to 18 DEG C of reaction 2.5h, be subsequently heated to
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain intercalation two by 78 DEG C of stirring reactions 20min
Sulfuration molybdenum powder.
Step 2, takes in 1.1g tryptophans addition 29g deionized waters, treats that tryptophan is stirring evenly and then adding into 2.0g intercalations two
Sulfuration molybdenum powder, stirs, and is dried through 24h, is ground to 200 mesh and sieves, before obtaining at a temperature of 80 DEG C in drying baker
Drive body powder.
Step 3, takes in adding 360g deionized waters after 120g ferric nitrates are mixed with 144g citric acids, adds ammonia to adjust
PH value is 6.8, is obtaining yellow sol solution at 80 DEG C after stirring chelating 6h.
Step 4, takes 100g sol solutions and adds 3.1g precursor powders wherein, continues the stirring 3h at 80 DEG C and obtains
To mixed gel, xerogel after mixed gel is dried 15h at 110 DEG C, is obtained, and be ground to 200 mesh and sieve and done
Gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 320 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 30min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 7：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 30g, sodium nitrate be 12g, mass concentration 98% concentrated sulphuric acid be 255mL
Hydrogen peroxide with mass concentration 30% is 65mL.
Then heating in water bath at 42 DEG C and stirs 45min, carries out intercalation to 20 DEG C of reaction 1.5h, be subsequently heated to
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain intercalation two by 88 DEG C of stirring reactions 12min
Sulfuration molybdenum powder.
Step 2, takes in 0.65g tryptophans addition 20g deionized waters, treats that tryptophan is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder, stirs, and is dried through 20h, is ground to 200 mesh and sieves, obtain at a temperature of 75 DEG C in drying baker
Precursor powder.
Step 3, takes in adding 150g deionized waters after 120g ferric nitrates are mixed with 115g citric acids, adds ammonia to adjust
PH value is 7.0, is obtaining yellow sol solution at 65 DEG C after stirring chelating 4h.
Step 4, takes 100g sol solutions and adds 5.5g precursor powders wherein, continues the stirring 2h at 65 DEG C and obtains
To mixed gel, xerogel after mixed gel is dried 8h at 120 DEG C, is obtained, and be ground to 200 mesh and sieve and done
Gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 280 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 60min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 8：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 20g, sodium nitrate be 10g, mass concentration 98% concentrated sulphuric acid be 225mL
Hydrogen peroxide with mass concentration 30% is 75mL.
Then heating in water bath at 35 DEG C and stirs 20min, carries out intercalation to 15 DEG C of reaction 2.5h, be subsequently heated to
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain intercalation two by 83 DEG C of stirring reactions 18min
Sulfuration molybdenum powder.
Step 2, takes in 0.45g tryptophans addition 16g deionized waters, treats that tryptophan is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder, stirs, and is dried through 16h, is ground to 200 mesh and sieves, obtain at a temperature of 80 DEG C in drying baker
Precursor powder.
Step 3, takes in adding 260g deionized waters after 120g ferric nitrates are mixed with 120g citric acids, adds ammonia to adjust
PH value is 7.2, is obtaining yellow sol solution at 55 DEG C after stirring chelating 4h.
Step 4, takes 100g sol solutions and adds 2.7g precursor powders, continuation to stir 3.5h at 55 DEG C wherein
Mixed gel is obtained, xerogel after mixed gel is dried 12h at 120 DEG C, is obtained, and is ground to 200 mesh and is sieved and obtain
Dry gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through nitrogen, is warming up to 300 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 80min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 9：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 40g, sodium nitrate be 5g, mass concentration 98% concentrated sulphuric acid be 300mL and
The hydrogen peroxide of mass concentration 30% is 60mL.
Then heating in water bath at 38 DEG C and stirs 25min, carries out intercalation, be subsequently heated to 86 to 12 DEG C of reaction 2h
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain two sulfur of intercalation by DEG C stirring reaction 11min
Change molybdenum powder.
Step 2, takes in 0.95g Phenylalanine addition 26g deionized waters, treats that Phenylalanine is stirring evenly and then adding into 2.0g
Intercalation molybdenum disulfide powder, stirs, and is dried through 13h, is ground to 200 mesh and sieves at a temperature of 85 DEG C in drying baker,
Obtain precursor powder.
Step 3, takes in adding 120g deionized waters after 120g ferric nitrates are mixed with 102g citric acids, adds ammonia to adjust
PH value is 6.5, is obtaining yellow sol solution at 55 DEG C after stirring chelating 4h.
Step 4, takes 100g sol solutions and adds 3.9g precursor powders wherein, continues the stirring 2h at 55 DEG C and obtains
To mixed gel, xerogel after mixed gel is dried 8h at 90 DEG C, is obtained, and be ground to 200 mesh and sieve and obtain dry solidifying
Rubber powder end.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 320 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 50min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 10：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 10g, sodium nitrate be 8g, mass concentration 98% concentrated sulphuric acid be 400mL and
The hydrogen peroxide of mass concentration 30% is 45mL.
Then heating in water bath at 70 DEG C and stirs 30min, carries out intercalation to 25 DEG C of reaction 1.5h, be subsequently heated to
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain intercalation two by 90 DEG C of stirring reactions 22min
Sulfuration molybdenum powder.
Step 2, takes in 0.9g Phenylalanine addition 5g deionized waters, treats that Phenylalanine is stirring evenly and then adding into 2.0g and inserts
Layer molybdenum disulfide powder, stirs, and is dried through 10h, is ground to 200 mesh and sieves, obtain at a temperature of 55 DEG C in drying baker
To precursor powder.
Step 3, takes in adding 120g deionized waters after 120g ferric nitrates are mixed with 98g citric acids, adds ammonia to adjust pH
It is worth for 7.0, at 75 DEG C, after stirring chelating 5h, is obtaining yellow sol solution.
Step 4, takes 100g sol solutions and adds 1.75g precursor powders, continuation to stir 2.5h at 75 DEG C wherein
Mixed gel is obtained, xerogel after mixed gel is dried 10h at 130 DEG C, is obtained, and is ground to 200 mesh and is sieved and obtain
Dry gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 250 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 120min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide multiple
Condensation material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 11：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 15g, sodium nitrate be 20g, mass concentration 98% concentrated sulphuric acid be 200mL
Hydrogen peroxide with mass concentration 30% is 100mL.
Then heating in water bath at 60 DEG C and stirs 36min, carries out intercalation, be subsequently heated to 96 to 20 DEG C of reaction 2h
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain two sulfur of intercalation by DEG C stirring reaction 10min
Change molybdenum powder.
Step 2, takes in 1g Phenylalanine addition 30g deionized waters, treats that Phenylalanine is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder, stirs, and is dried through 9h, is ground to 200 mesh and sieves, before obtaining at a temperature of 75 DEG C in drying baker
Drive body powder.
Step 3, takes in adding 230g deionized waters after 120g ferric nitrates are mixed with 130g citric acids, adds ammonia to adjust
PH value is 6.8, is obtaining yellow sol solution at 55 DEG C after stirring chelating 6h.
Step 4, takes 100g sol solutions and adds 3.3g precursor powders wherein, continues the stirring 2h at 55 DEG C and obtains
To mixed gel, xerogel after mixed gel is dried 12h at 120 DEG C, is obtained, and be ground to 200 mesh and sieve and done
Gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 280 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 80min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 12：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, take 10g siftage molybdenum disulfide powders be added to it is slotting
Layer solution in, intercalation solution consist of potassium chlorate for 35g, sodium nitrate be 18g, mass concentration 98% concentrated sulphuric acid be 90mL and
The hydrogen peroxide of mass concentration 30% is 150mL.
Then heating in water bath at 52 DEG C and stirs 42min, carries out intercalation to 10 DEG C of reaction 2.5h, be subsequently heated to
Resulting solution after reaction is filtered and dries filter cake, is ground to 200 mesh and sieves, obtain intercalation by 100 DEG C of stirring reactions 10min
Molybdenum disulfide powder.
Step 2, takes in 0.25g Phenylalanine addition 27g deionized waters, treats that Phenylalanine is stirring evenly and then adding into 2.0g
Intercalation molybdenum disulfide powder, stirs, and is dried through 8h, is ground to 200 mesh and sieves, obtain at a temperature of 60 DEG C in drying baker
To precursor powder.
Step 3, takes in adding 160g deionized waters after 120g ferric nitrates are mixed with 108g citric acids, adds ammonia to adjust
PH value is 7.2, is obtaining yellow sol solution at 55 DEG C after stirring chelating 4.5h.
Step 4, takes 100g sol solutions and adds 2.2g precursor powders wherein, continues the stirring 2h at 55 DEG C and obtains
To mixed gel, xerogel after mixed gel is dried 13h at 90 DEG C, is obtained, and be ground to 200 mesh and sieve and done
Gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through nitrogen, is warming up to 300 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 70min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 13：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Step one is identical with the step of embodiment 1 one.
Step 2, takes in 1.2g threonine addition 21g deionized waters, treats that threonine is stirring evenly and then adding into 2.0g intercalations two
Sulfuration molybdenum powder, stirs, and is dried through 18h, is ground to 200 mesh and sieves, before obtaining at a temperature of 75 DEG C in drying baker
Drive body powder.
Step 3, takes in adding 300g deionized waters after 120g ferric nitrates are mixed with 125g citric acids, adds ammonia to adjust
PH value is 7.0, is obtaining yellow sol solution at 60 DEG C after stirring chelating 5.5h.
Step 4, takes 100g sol solutions and adds 1.7g precursor powders, continuation to stir 2.5h at 60 DEG C wherein
Mixed gel is obtained, xerogel after mixed gel is dried 15h at 130 DEG C, is obtained, and is ground to 200 mesh and is sieved and obtain
Dry gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 300 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 40min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 14：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Step one is identical with the step of embodiment 1 one.
Step 2, takes in 0.27g threonine addition 6.5g deionized waters, treats that threonine is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder, stirs, and is dried through 24h, is ground to 200 mesh and sieves, obtain at a temperature of 60 DEG C in drying baker
Precursor powder.
Step 3, takes in adding 280g deionized waters after 120g ferric nitrates are mixed with 100g citric acids, adds ammonia to adjust
PH value is 7.5, is obtaining yellow sol solution at 55 DEG C after stirring chelating 6h.
Step 4, takes 100g sol solutions and adds 4.1g precursor powders, continuation to stir 3.5h at 55 DEG C wherein
Mixed gel is obtained, xerogel after mixed gel is dried 15h at 120 DEG C, is obtained, and is ground to 200 mesh and is sieved and obtain
Dry gel powder.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 200 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 120min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide multiple
Condensation material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 15：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Step one is identical with the step of embodiment 1 one.
Step 2, takes in 0.6g threonine addition 21g deionized waters, treats that threonine is stirring evenly and then adding into 2.0g intercalations two
Sulfuration molybdenum powder, stirs, and is dried through 9h, is ground to 200 mesh and sieves, obtain forerunner at a temperature of 80 DEG C in drying baker
Body powder.
The step of step 3, the present embodiment three, is identical with the step of embodiment 1 three.
The step of step 4, the present embodiment four, is identical with the step of embodiment 1 four.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 250 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 70min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 16：
The present embodiment provides a kind of protein matter reduction and prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material
Method, the method comprises the following steps：
Step one is identical with the step of embodiment 1 one.
Step 2, takes in 1.25g threonine addition 23g deionized waters, treats that threonine is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder, stirs, and is dried through 9h, is ground to 200 mesh and sieves, before obtaining at a temperature of 80 DEG C in drying baker
Drive body powder.
The step of step 3, the present embodiment three, is identical with the step of embodiment 1 three.
The step of step 4, the present embodiment four, is identical with the step of embodiment 1 four.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 280 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 50min with the furnace, that is, obtain class Graphene molybdenum bisuphide-ferroso-ferric oxide and be combined
Material.
The characterization result and embodiment of the present embodiment products therefrom class Graphene molybdenum bisuphide-ferriferrous oxide composite material
1 is essentially identical.
Comparative example 1：
This comparative example provides a kind of method for preparing molybdenum bisuphide-ferriferrous oxide composite material, and the method includes following
Step：
Molybdenum disulfide powder is ground to 200 mesh and is sieved by step one, is taken 10g siftage molybdenum disulfide powders, is added into
During mass concentration is the 10%, ethanol solution containing 100g polyphenylene sulfides, heating in water bath is to 30 DEG C and stirs 12h, is mixed
Liquid.5gKMnO is added in above-mentioned mixed liquor4Powder, heating in water bath is to 50 DEG C and stirs 18h, filters and dries filter cake, grinds
It is milled to 200 mesh to sieve, obtains intercalation molybdenum disulfide powder.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Step 5 is identical with the step of embodiment 1 five.
Raman spectrum analyses and TEM point are carried out to molybdenum bisuphide-ferriferrous oxide composite material obtained in this comparative example
Analysis.The Raman spectrum of composite are as shown in figure 4, its E2g 1With Ag 1Value is respectively 375.7 and 402.5, and displacement difference is 26.8, position
Difference is moved more than 25, shows that the molybdenum bisuphide in the composite belongs to block structure molybdenum bisuphide.The TEM image of composite is such as
Shown in Fig. 5, illustrate that this product molybdenum bisuphide block is piled up, multiple structure is presented, and ferroso-ferric oxide is combined the uneven group of presentation
Poly- phenomenon, so the composite is not belonging to class Graphene molybdenum bisuphide-ferriferrous oxide nano composite.
Comparative example 2：
This comparative example provides a kind of method for preparing molybdenum bisuphide-ferriferrous oxide composite material, and the method includes following
Step：
Step one, it is identical with other processes in the step of embodiment 1 one, differ only in：The composition of intercalation solution
For potassium permanganate 20g, sodium nitrate be 10g, mass concentration 98% concentrated sulphuric acid be 230mL.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Step 5 is identical with the step of embodiment 1 five.
Obtained in this comparative example, molybdenum bisuphide-ferriferrous oxide composite material occurs molybdenum bisuphide block as comparative example 1
Body is piled up, and does not find the appearance of graphene-structured, is not belonging to class Graphene molybdenum disulfide nano-composite material.
Comparative example 3：
This comparative example provides a kind of method for preparing molybdenum bisuphide-ferriferrous oxide composite material, and the method includes following
Step：
Step one is identical with the step of embodiment 1 one.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 500 DEG C, react 5min by step 5
After cool to room temperature with the furnace after take out product be ground, that is, obtain molybdenum bisuphide-ferriferrous oxide composite material.
Comparative example 4：
This comparative example provides a kind of method for preparing molybdenum bisuphide-ferriferrous oxide composite material, and the method includes following
Step：
Step one is identical with the step of embodiment 1 one.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 250 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 40min with the furnace, that is, obtain molybdenum bisuphide-ferriferrous oxide composite material.
Obtained in this comparative example, molybdenum bisuphide-ferriferrous oxide composite material occurs molybdenum bisuphide block as comparative example 1
Body is piled up, and does not find the appearance of graphene-structured, is not belonging to class Graphene molybdenum disulfide nano-composite material.
Comparative example 5：
This comparative example provides a kind of method for preparing molybdenum bisuphide-ferriferrous oxide composite material, and the method includes following
Step：
Step one is identical with the step of embodiment 1 one.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Dry gel powder is loaded burning boat and is placed in tube furnace, is passed through argon, is warming up to 1300 DEG C, react by step 5
Take out product to be ground after cooling to room temperature after 15min with the furnace, that is, obtain molybdenum bisuphide-ferriferrous oxide composite material.
Obtained in this comparative example, molybdenum bisuphide-ferriferrous oxide composite material occurs molybdenum bisuphide block as comparative example 1
Body is piled up, and does not find the appearance of graphene-structured, is not belonging to class Graphene molybdenum disulfide nano-composite material.
Claims (10)
1. a kind of method that protein matter reduction prepares class Graphene molybdenum bisuphide-ferriferrous oxide composite material, its feature
It is that the method is comprised the following steps：
Step one, molybdenum disulfide powder is added in intercalation solution carries out intercalation, filters, dries, obtain after the completion of reaction
To intercalation molybdenum disulfide powder；
Described intercalation solution is the mixed solution of potassium chlorate, sodium nitrate, concentrated sulphuric acid and hydrogen peroxide composition；
Described molybdenum disulfide powder is double with potassium chlorate, sodium nitrate, the concentrated sulphuric acid of mass concentration 98% and mass concentration 30%
Proportion relation between oxygen water is 1g：(1～4) g：(0.5～2) g：(9～40) mL：(4～20) mL；
Step 2, intercalation molybdenum disulfide powder obtained in step one is mixed and stirred for uniformly with protein matter and water, dry,
Grinding, obtains precursor powder；
Described intercalation molybdenum disulfide powder and the proportion relation between protein matter and water are 2g：(0.25～1.25) g：(5
～30) g；
Step 3, is added to the water after ferric nitrate is mixed with citric acid, carries out chelatropic reaction, obtains sol solution；
Described ferric nitrate, the proportion relation between citric acid and deionized water are 1g：(0.8～1.2) g:(1～3) g；
Step 4, adds precursor powder in sol solution, obtains mixed gel, be dried after stirring mixing, and grinding is done
Gel powder；
Proportion relation between described sol solution and precursor powder is：100g：(1.7～5.5) g；
Step 5, dry gel powder carry out reduction reaction under a shielding gas, cool down after reaction completely, take out product, grind
Class Graphene molybdenum bisuphide-ferriferrous oxide composite material is obtained after mill.
2. the method for claim 1, it is characterised in that described protein matter is TYR, tryptophan, phenylpropyl alcohol ammonia
Acid or threonine.
3. the method for claim 1, it is characterised in that described molybdenum disulfide powder and potassium chlorate, sodium nitrate, quality
Proportion relation between the hydrogen peroxide of the concentrated sulphuric acid and mass concentration 30% of concentration 98% is 1g：2g：1g：23mL：7mL.
4. the method for claim 1, it is characterised in that described intercalation molybdenum disulfide powder and protein matter and water
Between proportion relation be 2g：0.5g：15g.
5. the method for claim 1, it is characterised in that in step one, the process of described intercalation is：By two sulfur
Change during molybdenum powder adds mixed solution, be heated to 10～30 DEG C of 1～3h of reaction, then at 30～70 DEG C and stir 20～50min,
10～30min of stirring reaction at 75～100 DEG C, then sucking filtration, drying, obtains intercalation molybdenum disulfide powder.
6. the method for claim 1, it is characterised in that in step 2, described intercalation molybdenum disulfide powder, protide
After material and water mixing and stirring, it is dried through 6～24h at a temperature of 50～100 DEG C in drying baker, grinding, before obtaining
Drive body powder.
7. the method for claim 1, it is characterised in that in step 3, the detailed process of chelatropic reaction is：By ferric nitrate
Be added to the water after mixing with citric acid, add ammonia the pH of reaction system to be adjusted 6.5～7.5, stir chela at 45～80 DEG C
4～6h of reaction is closed, sol solution is obtained.
8. the method for claim 1, it is characterised in that in step 4, add precursor powder in sol solution,
2～3.5h is stirred at 45～80 DEG C and obtains mixed gel, obtain xerogel after 7～15h being dried at 90～130 DEG C, will be dry solidifying
Glue is ground to 200 mesh and sieves and obtains dry gel powder.
9. the method for claim 1, it is characterised in that in step 5, the process of described reduction reaction is：By step
In four, the dry gel powder of gained loads burning boat, is put in tube furnace, and being continually fed into protective atmosphere carries out reduction reaction, has reacted
Reduzate is taken out after cooling to room temperature into after with the furnace, that is, obtains class Graphene molybdenum bisuphide-bismuth molybdate composite；
When described protein matter is TYR, the temperature of reduction reaction is 280～400 DEG C, temperature retention time is 40～
90min；When described protein matter is tryptophan, the temperature of reduction reaction is 240～320 DEG C, temperature retention time is 30～
80min；When described protein matter is Phenylalanine, the temperature of reduction reaction is 250～320 DEG C, temperature retention time is 50～
120min；When described protein matter is threonine, the temperature of reduction reaction is 200～300 DEG C, temperature retention time is 40～
120min。
10. the method as described in claim 1 to 9 any claim, it is characterised in that described protective atmosphere be nitrogen or
Argon.
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| CN110498487A (en) * | 2019-09-06 | 2019-11-26 | 西安建筑科技大学 | A kind of preparation method, product and its application of the modified bismuth molybdate optoelectronic pole of cetyl trimethylammonium bromide |
| CN112973738A (en) * | 2021-02-05 | 2021-06-18 | 江苏大学 | Magnetic self-assembly MoS2@Fe3O4@Cu2Preparation method and application of O photocatalyst |
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