CN109174131A - The molybdenum disulfide nano floral material and its synthetic method of nickel cobalt modification and application - Google Patents
The molybdenum disulfide nano floral material and its synthetic method of nickel cobalt modification and application Download PDFInfo
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- CN109174131A CN109174131A CN201810994407.9A CN201810994407A CN109174131A CN 109174131 A CN109174131 A CN 109174131A CN 201810994407 A CN201810994407 A CN 201810994407A CN 109174131 A CN109174131 A CN 109174131A
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- nickel cobalt
- molybdenum
- molybdenum disulfide
- nickel
- disulfide nano
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 64
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 44
- 230000004048 modification Effects 0.000 title claims abstract description 40
- 238000012986 modification Methods 0.000 title claims abstract description 40
- 238000010189 synthetic method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011733 molybdenum Substances 0.000 claims abstract description 19
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 19
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000005864 Sulphur Substances 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 241000446313 Lamella Species 0.000 claims abstract description 3
- 229910052729 chemical element Inorganic materials 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- 239000003054 catalyst Substances 0.000 claims description 14
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 10
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 8
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 8
- 239000011609 ammonium molybdate Substances 0.000 claims description 8
- 229940010552 ammonium molybdate Drugs 0.000 claims description 8
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 5
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 238000004073 vulcanization Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- SHWZFQPXYGHRKT-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;nickel Chemical compound [Ni].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O SHWZFQPXYGHRKT-FDGPNNRMSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- STZJANGYOWJEPH-UHFFFAOYSA-N carbonic acid;molybdenum Chemical compound [Mo].OC(O)=O STZJANGYOWJEPH-UHFFFAOYSA-N 0.000 claims description 2
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 235000007686 potassium Nutrition 0.000 claims description 2
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 claims 1
- 229940011182 cobalt acetate Drugs 0.000 claims 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims 1
- SZKXDURZBIICCF-UHFFFAOYSA-N cobalt;pentane-2,4-dione Chemical compound [Co].CC(=O)CC(C)=O SZKXDURZBIICCF-UHFFFAOYSA-N 0.000 claims 1
- 238000006392 deoxygenation reaction Methods 0.000 claims 1
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 claims 1
- 229940053662 nickel sulfate Drugs 0.000 claims 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 28
- 238000000034 method Methods 0.000 description 26
- 230000015572 biosynthetic process Effects 0.000 description 24
- 238000003786 synthesis reaction Methods 0.000 description 23
- 229910052759 nickel Inorganic materials 0.000 description 14
- 239000002057 nanoflower Substances 0.000 description 13
- 229910017052 cobalt Inorganic materials 0.000 description 8
- 239000010941 cobalt Substances 0.000 description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 238000005984 hydrogenation reaction Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- MYAQZIAVOLKEGW-UHFFFAOYSA-N DMDBT Natural products S1C2=C(C)C=CC=C2C2=C1C(C)=CC=C2 MYAQZIAVOLKEGW-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241001481828 Glyptocephalus cynoglossus Species 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- 239000012456 homogeneous solution Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- -1 Dimethyl Dibenzothiophene Chemical compound 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- DOIKGWMZXKJLJV-UHFFFAOYSA-N [W].[Mo](=S)=S Chemical compound [W].[Mo](=S)=S DOIKGWMZXKJLJV-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- IYYZUPMFVPLQIF-UHFFFAOYSA-N dibenzothiophene sulfoxide Natural products C1=CC=C2C3=CC=CC=C3SC2=C1 IYYZUPMFVPLQIF-UHFFFAOYSA-N 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- XDAHMMVFVQFOIY-UHFFFAOYSA-N methanedithione;sulfane Chemical compound S.S=C=S XDAHMMVFVQFOIY-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/51—
-
- B01J35/61—
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/20—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only oxygen atoms as heteroatoms
- C07C1/22—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only oxygen atoms as heteroatoms by reduction
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2527/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- C07C2527/02—Sulfur, selenium or tellurium; Compounds thereof
- C07C2527/04—Sulfides
- C07C2527/047—Sulfides with chromium, molybdenum, tungsten or polonium
- C07C2527/051—Molybdenum
-
- 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
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The molybdenum disulfide nano floral material and its synthetic method of nickel cobalt modification and application, are related to molybdenum disulfide nano floral material.The chemical element group of the molybdenum disulfide nano floral material of nickel cobalt modification becomes nickel cobalt, molybdenum and sulphur, in class flower ball-shaped pattern, bouquet is made of laminar structured, and nickel cobalt is uniformly distributed on molybdenum disulfide lamella, nanometer flower diameter is 50~800nm, and the nanoscale twins on bouquet are with a thickness of 2~10nm.Molybdenum source and nickel cobalt source are dissolved in the water, mixed solution is obtained；Vulcanizing agent and reducing agent are added in mixed solution, forms suspension after dispersion；Suspension is transferred to hydrothermal reaction kettle, it is cooling after heating reaction；The black solid obtained in hydrothermal reaction kettle is taken out after cooling, is centrifuged, is washed, after vacuum drying, obtains the molybdenum disulfide nano floral material of the nickel cobalt modification of different-shape size.
Description
Technical field
The present invention relates to molybdenum disulfide nano floral materials, more particularly, to the molybdenum disulfide nano floral material of nickel cobalt modification
And its synthetic method and application.
Background technique
As a kind of typical transition metal stratiform compound, molybdenum disulfide has class graphene hexagonal closs packing stratiform knot
Structure, molybdenum/sulphur layer alternately exist, and form the sandwich of class " sandwich ", and interlayer is combined with Van der Waals force, are total in layer by strong
Valence link and ionic bond are connected, and this changeable Atomic coordinate Structure and electronic structure makes it with excellent catalysis, lubrication
And photoelectric properties, become one of the material being concerned.But there are specific surface areas that low, pattern can not for conventional body phase molybdenum disulfide
Control, the problems such as unit area active site quantity is low, limit its application in terms of catalysis.Due to the property of sulfide catalyst
There can be close ties with its appearance structure, and appearance structure is directly determined by preparation method, therefore passes through pattern and structure
Regulation synthesis multidimensional structure molybdenum disulfide, to further increase its specific surface area and active site quantity, this is vulcanization
One of the research hotspot of object nano material.
Currently, having the synthesis of more document and patent report molybdenum disulfide nano floral material.Chinese patent
CN105347401B synthesizes molybdenum disulfide nano flower of uniform morphology using soft template method, but template is expensive, at the later period
It manages complex, it is difficult to realize large-scale production.Chinese patent CN103613137B is received using hydrothermal method synthesis of carbon/molybdenum disulfide
Popped rice, whole process are fully sealed, and can synthesize the higher molybdenum disulfide material of purity, but the nano flower pattern of this method synthesis compared with
Unevenly, and bouquet is larger, and specific surface area and voidage are not obviously improved.Chinese patent CN106994357A discloses one
The molybdenum disulfide material of kind witch culture, increases the defect sites of molybdenum disulfide by witch culture, so that its electrolysis water activity is improved,
The tungsten molybdenum disulfide nano flower of mixing of this method synthesis is made of laminated structure, diameter 100nm or so, but when originals such as cation doping/nickel
The period of the day from 11 p.m. to 1 a.m, hetero atom play the influence of obstruction to the formation of molybdenum disulfide, so that material specific surface area reduces, live to influence reaction
Property [Chemical Engineering Science, 2012,79:1-7；Advanced Materials, 2016,28:9006-
9011]。
Summary of the invention
It is an object of the invention to for active sites on current molybdenum disulfide catalyst there are specific surface areas small, unit area
The defects of point Limited Number and poor synthesis pattern controllability, provides three-dimensional for the molybdenum disulfide of controlledly synthesis nickel cobalt modification
Nano flower effectively improves the molybdenum disulfide nano flower material of hydrodesulfurization/deoxy performance nickel cobalt modification of molybdenum disulfide catalyst
Material and its synthetic method and application.
The chemical element group of the molybdenum disulfide nano floral material of the nickel cobalt modification becomes nickel cobalt, molybdenum and sulphur, in class flower
Spherical morphology, bouquet are made of laminar structured, and nickel cobalt is uniformly distributed on molybdenum disulfide lamella, nanometer flower diameter be 50~
800nm, the nanoscale twins on bouquet are with a thickness of 2~10nm.
The synthetic method of the molybdenum disulfide nano floral material of nickel cobalt modification the following steps are included:
1) molybdenum source and nickel cobalt source are dissolved in the water, obtain mixed solution；
2) vulcanizing agent and reducing agent are added in mixed solution, forms suspension after dispersion；
3) suspension is transferred to hydrothermal reaction kettle, it is cooling after heating reaction；
4) black solid obtained in hydrothermal reaction kettle is taken out after cooling, is centrifuged, washed, after vacuum drying,
Obtain the molybdenum disulfide nano floral material of the nickel cobalt modification of different-shape size.
In step 1), the nickel cobalt source can be selected from nickel nitrate (cobalt), nickel acetate (cobalt), nickel sulfate (cobalt), nickel chloride
At least one of (cobalt), nickel acetylacetonate (cobalt) etc.；The molybdenum source can be selected from ammonium molybdate, sodium molybdate, potassium molybdate, molybdenum oxide,
At least one of molybdenum pentachloride, carbonic acid molybdenum, ammonium thiomolybdate etc.；In the mixed solution molar concentration of molybdenum can 0.01~
The molar ratio of 1mol/L, nickel cobalt and molybdenum can be 0.05~1.
In step 2), the vulcanizing agent can be selected from elemental sulfur, ammonium sulfide, vulcanized sodium, potassium sulfide, thiocarbamide, thioacetyl
At least one of amine, carbon disulfide and hydrogen sulfide etc.；The reducing agent can be selected from sodium borohydride, hydrazine hydrate, hydroxylamine hydrochloride etc.
At least one of；The vulcanizing agent and reducing agent addition amount can be the molar ratio 1.5~5 of sulphur and molybdenum, and reducing agent and molybdenum rub
You are than being 5~40.
In step 3), the hydrothermal reaction kettle reaction temperature can be 140~240 DEG C, preferably 160~200 DEG C；The water
The time of thermal response can be 24~240h, preferably 60~160h.
In step 4), water and ethanol washing is can be used in the washing.
The molybdenum disulfide nano floral material of the nickel cobalt modification can be used as catalyst and react in hydrodesulfurization or hydrogenation deoxidation
Middle application, the temperature of the reaction can be 220~350 DEG C, and the pressure of hydrogen can be 1~5MPa.
The present invention is provided for disadvantage present in above-mentioned molybdenum disulfide morphology controllable synthetic method and deficiency using hydro-thermal
There is vulcanization one-step synthesis the nickel cobalt of controllable three-dimensional nanostructure to adulterate molybdenum disulfide material, and is applied to and urges
Change hydrodesulfurization/deoxidation field, the molybdenum disulfide nano flower of nickel cobalt doping controllable, edge active site with appearance structure
The molybdenum disulfide nano floral material of the nickel cobalt modification for the features such as more, catalytic activity is high, reaction stability is good and its synthetic method with
Using.
The present invention can continuously adjust control nickel cobalt doping obtained by changing predecessor concentration in hydrothermal solution
The pattern of molybdenum disulfide, nano-scale size, to influence active site quantity on sulfide catalyst unit area, and final
Change the catalytic performance of catalyst.Compared with other sulfide technologies of preparing, synthesis condition can be simply adjusted, is realized to vulcanization
The regulation of object material microstructure improves specific surface area, the active site quantity of sulfide material, increases reactant and work
The advantages that effective contact area in property site.In terms of being catalyzed reaction stability, due to the feature on molybdenum disulfide structure and morphology,
Stacking agglomeration of the catalyst in long-time use process is advantageously reduced, to have good stability.
The invention has the benefit that concentration of the present invention by molybdenum and nickel cobalt predecessor in adjusting hydrothermal system, it can be real
Now the size to nanometer bouquet and flower piece thickness carry out controllable continuous modulation；This method can synthesize regular appearance and more uniform
Nano flower, the nanometer sheet thickness assembled is small, specific surface area with higher and biggish porosity, and has a large amount of Surface Edge
The exposure of edge active site, thus excellent catalytic performance is shown in hydrodesulfurization and hydrogenation deoxidation reaction.
Detailed description of the invention
Fig. 1 is the electron microscope of the molybdenum disulfide nano floral material embodiment of nickel cobalt of the present invention modification.
Fig. 2 is the scanning electron microscope (SEM) photograph that hydrothermal synthesis nickel cobalt adulterates molybdenum disulfide nano flower in the embodiment of the present invention 1~4.
Fig. 3 is the transmission electron microscope picture that hydrothermal synthesis nickel cobalt adulterates molybdenum disulfide nano flower in the embodiment of the present invention 1~4.
Specific embodiment
The molybdenum disulfide three-dimensional manometer floral material that nickel cobalt involved in the present invention is modified with comparative example by the following examples
Controlledly synthesis and its application be further described, referring to Fig. 1.
Embodiment 1
Ammonium molybdate 2.0g is weighed, nickel nitrate 1.64g is dissolved in 18mL water, forms homogeneous solution.In whipping process, it is added
10mL hydrazine hydrate solution (85%) is uniformly mixed.1.45g elemental sulfur is weighed, above-mentioned solution is added, carries out ultrasound 30min.Then
Obtained mixed liquor is put into polytetrafluoroethyllining lining container, baking oven is put into and carries out hydro-thermal reaction.Hydrothermal temperature is 180
DEG C, the hydro-thermal time is 72h.It is cooled down after reaction, the mixed liquor after taking out reaction is separated, washed, and obtained black is solid
Body is handled for 24 hours in 60 DEG C of vacuum ovens, the final molybdenum disulfide three-dimensional manometer floral material for obtaining nickel modification.This method synthesis
Material scanning nuclear microprobe figure respectively as shown in Fig. 2 (a) and Fig. 3 (a).It can be seen from the figure that using our legal system
Standby nickel modification molybdenum disulfide nano flower-shape looks are uniform, and bouquet size is about 520nm, and formed flower piece thickness is about
7.0nm。
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, except that the dosage of each predecessor: ammonium molybdate 1.0g, nickel nitrate
0.494g, elemental sulfur 0.725g.The scanning nuclear microprobe figure of the material of this method synthesis is respectively such as Fig. 2 (b) and Fig. 3 (b) institute
Show.It can be seen from the figure that the nickel modification molybdenum disulfide nano flower-shape looks using this method preparation are uniform, bouquet size is about
For 260nm, formed flower piece thickness is about 5.2nm.
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, except that the dosage of each predecessor: ammonium molybdate 0.5g, nickel nitrate
0.41g, elemental sulfur 0.36g.The scanning nuclear microprobe figure of the material of this method synthesis is respectively as shown in Fig. 2 (c) and Fig. 3 (c).
It can be seen from the figure that the nickel modification molybdenum disulfide nano flower-shape looks using this method preparation are uniform, bouquet size is about
150nm, formed flower piece thickness is about 4.0nm.
Embodiment 4
Embodiment 4 is substantially the same manner as Example 1, except that the dosage of each predecessor: ammonium molybdate 0.2g, nickel nitrate
0.098g, elemental sulfur 0.145g.The scanning nuclear microprobe figure of the material of this method synthesis is respectively such as Fig. 2 (d) and Fig. 3 (d) institute
Show.It can be seen from the figure that the nickel modification molybdenum disulfide nano flower-shape looks using this method preparation are uniform, bouquet size is about
For 120nm, formed flower piece thickness is about 2.5nm.
Embodiment 5
Embodiment 5 is substantially the same manner as Example 1, except that vulcanizing agent uses ammonium sulfide, 45wt.% ammonium sulfide is water-soluble
Liquid additional amount is 4.28g.Uniform using the nickel modification molybdenum disulfide nano flower-shape looks of this method synthesis, bouquet size is about
550nm, formed flower piece thickness is about 7.0nm.
Embodiment 6
Embodiment 6 is substantially the same manner as Example 1, except that reducing agent uses hydroxylamine hydrochloride, analyzes pure hydrochloric acid azanol
Additional amount is 10mL.Uniform using the nickel modification molybdenum disulfide nano flower-shape looks of this method synthesis, bouquet size is about
500nm, formed flower piece thickness is about 6.8nm.
Embodiment 7
Embodiment 7 is substantially the same manner as Example 1, except that hydrothermal temperature is adjusted to 200 DEG C.Using this method
The nickel modification molybdenum disulfide nano flower-shape looks of synthesis are uniform, and bouquet size is about 700nm, and formed flower piece thickness is about
9nm。
Embodiment 8
Embodiment 8 is substantially the same manner as Example 1, except that the hydro-thermal reaction time is adjusted to 168h.Using this method
The nickel modification molybdenum disulfide nano flower-shape looks of synthesis are uniform, and bouquet size is about 520nm, and formed flower piece thickness is about
7.0nm。
Embodiment 9
Embodiment 9 is substantially the same manner as Example 2, except that substituting nickel nitrate, cobalt nitrate additional amount using cobalt nitrate
For 0.824g.Uniform using the cobalt modification molybdenum disulfide nano flower-shape looks of this method synthesis, bouquet size is about 250nm,
Formed flower piece thickness is about 5.3nm.
Embodiment 10
Embodiment 10 is substantially the same manner as Example 2, except that substituting nickel nitrate, cobalt nitrate additional amount using cobalt nitrate
For 0.824g, ammonium molybdate is substituted using molybdenum oxide, molybdenum oxide additional amount is 0.816g.Two sulphur are modified using the cobalt of this method synthesis
Change molybdenum nano flower pattern is uniform, and bouquet size is about 230nm, and formed flower piece thickness is about 5.0nm.
Comparative example 1
Ammonium molybdate 2.0g is weighed, nickel nitrate 1.64g is dissolved in 18mL water, forms homogeneous solution.Heating water bath to 90 DEG C,
It is stirred continuously until forming collosol and gel.Gained colloidal sol is put into baking oven dry 12h at 110 DEG C, then in air atmosphere
500 DEG C of roasting 5h.Finally by obtained solid powder in 15%H2S/H2The lower 400 DEG C of vulcanizing treatment 4h of the atmosphere of gaseous mixture, to obtain
Obtain the molybdenum disulfide nano material of nickel modification.Pattern using the nickel modification molybdenum disulfide nano material of this method preparation is in particle
Shape, nano particle size are about 30nm.
Comparative example 2
It weighs nickel nitrate 1.64g to be dissolved in 3mL water, be impregnated on the molybdenum oxide of 1.63g several times, be then put into baking oven and exist
Dry 12h at 110 DEG C, then in 15%H2S/H2The lower 400 DEG C of vulcanizing treatment 4h of the atmosphere of gaseous mixture, to obtain nickel modification
Molybdenum disulfide body phase material.
Embodiment 11
Examples 1 to 8 and the obtained sulfide material of comparative example 1 and 2 are applied to hydrodesulfurization reaction as catalyst
Performance evaluation.Dimethyl Dibenzothiophene containing 0.2wt.%4,6- (DMDBT) is being added just in 100mL stainless steel cauldron
Tetradecane solution 40mL and above-mentioned sulfide catalyst 0.1g.Reaction kettle is sealed into access hydrogen, and for several times with helium purge
To drain air.Reaction kettle is heated under lasting stirring condition, when reaching 300 DEG C of reaction temperature of setting, is filled with hydrogen
It is 4.0MPa to gross pressure.It keeps temperature constant at 300 DEG C in reaction process, keeps constant reaction pressure in 4.0MPa or so.
Separated in time acquisition reaction solution carries out gas chromatographic analysis in reaction process, and evaluation results are shown in Table 1.
Embodiment 12
The obtained sulfide material of embodiment 9 and 10 is applied to the performance evaluation of hydrogenation deoxidation reaction as catalyst.
Evaluation procedure is substantially the same manner as Example 11, except that model reaction object uses the decahydronaphthalene of the p-methyl phenol containing 3wt.%
Solution, reaction evaluating the results are shown in Table 2.
Table 1
Table 2
As shown in Table 1, using the nickel modification molybdenum disulfide nano flower catalyst and reference of method provided by the present invention synthesis
Nanocatalyst compare, DMDBT hydrodesulfurization reaction activity is significantly improved, especially embodiment 3 and embodiment 4 is mentioned
The sulphur that can be realized at 300 DEG C in DMDBT for catalyst substantially completely removes.As shown in Table 2, using side provided by the present invention
The cobalt modification molybdenum disulfide nano flower catalyst of method synthesis equally shows excellent hydrogenation deoxidation activity, and methylbenzene selective is high
Up to 98%.To sum up, compared with prior art, the nickel cobalt modification molybdenum disulfide nano flower catalysis of method synthesis provided by the present invention
Agent has a clear superiority in hydrodesulfurization and hydrogenation deoxidation reaction.
Claims (10)
1. the molybdenum disulfide nano floral material of nickel cobalt modification, it is characterised in that its chemical element group becomes nickel cobalt, molybdenum and sulphur, is in
Class flower ball-shaped pattern, bouquet are made of laminar structured, and nickel cobalt is uniformly distributed on molybdenum disulfide lamella, and nanometer flower diameter is
50~800nm, the nanoscale twins on bouquet are with a thickness of 2~10nm.
2. the synthetic method of the molybdenum disulfide nano floral material of nickel cobalt as described in claim 1 modification, it is characterised in that including with
Lower step:
1) molybdenum source and nickel cobalt source are dissolved in the water, obtain mixed solution；
2) vulcanizing agent and reducing agent are added in mixed solution, forms suspension after dispersion；
3) suspension is transferred to hydrothermal reaction kettle, it is cooling after heating reaction；
4) black solid obtained in hydrothermal reaction kettle is taken out after cooling, is centrifuged, washed, after vacuum drying, obtain
The molybdenum disulfide nano floral material of the nickel cobalt modification of different-shape size.
3. the synthetic method of the molybdenum disulfide nano floral material of nickel cobalt modification as claimed in claim 2, it is characterised in that in step
1) in, the nickel cobalt source be selected from nickel nitrate, cobalt nitrate, nickel acetate, cobalt acetate, nickel sulfate, cobaltous sulfate, nickel chloride, cobalt chloride,
At least one of nickel acetylacetonate, acetylacetone cobalt；The molybdenum source is selected from ammonium molybdate, sodium molybdate, potassium molybdate, molybdenum oxide, five
At least one of molybdenum chloride, carbonic acid molybdenum, ammonium thiomolybdate.
4. the synthetic method of the molybdenum disulfide nano floral material of nickel cobalt modification as claimed in claim 2, it is characterised in that in step
1) in, 0.01~1mol/L of molar concentration of molybdenum in the mixed solution, the molar ratio of nickel cobalt and molybdenum is 0.05~1.
5. the synthetic method of the molybdenum disulfide nano floral material of nickel cobalt modification as claimed in claim 2, it is characterised in that in step
2) in, the vulcanizing agent is selected from elemental sulfur, ammonium sulfide, vulcanized sodium, potassium sulfide, thiocarbamide, thioacetamide, carbon disulfide, vulcanization
At least one of hydrogen；The reducing agent is selected from least one of sodium borohydride, hydrazine hydrate, hydroxylamine hydrochloride.
6. the synthetic method of the molybdenum disulfide nano floral material of nickel cobalt modification as claimed in claim 2, it is characterised in that in step
2) in, the vulcanizing agent and reducing agent addition amount are the molar ratio 1.5~5 of sulphur and molybdenum, the molar ratio of reducing agent and molybdenum is 5~
40。
7. the synthetic method of the molybdenum disulfide nano floral material of nickel cobalt modification as claimed in claim 2, it is characterised in that in step
3) in, the reaction temperature of the hydrothermal reaction kettle is 140~240 DEG C, preferably 160~200 DEG C；The time of the hydro-thermal reaction is
24~240h, preferably 60~160h.
8. the synthetic method of the molybdenum disulfide nano floral material of nickel cobalt modification as claimed in claim 2, it is characterised in that in step
4) in, the washing uses water and ethanol washing.
9. the molybdenum disulfide nano floral material of nickel cobalt modification as described in claim 1 in hydrodesulfurization or adds hydrogen as catalyst
It is applied in deoxygenation.
10. application as claimed in claim 9, it is characterised in that the temperature of the reaction is 220~350 DEG C, and the pressure of hydrogen is 1
~5MPa.
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