CN105664976A - Supported two-dimensional layered molybdenum sulfide composite material and preparation method and application thereof - Google Patents
Supported two-dimensional layered molybdenum sulfide composite material and preparation method and application thereof Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 36
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 230000009467 reduction Effects 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 11
- 239000002105 nanoparticle Substances 0.000 claims description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- 238000005119 centrifugation Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 229960004756 ethanol Drugs 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 6
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 6
- 239000011609 ammonium molybdate Substances 0.000 claims description 6
- 229940010552 ammonium molybdate Drugs 0.000 claims description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052753 mercury Inorganic materials 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 3
- 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
- 229950000845 politef Drugs 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 3
- 238000001816 cooling Methods 0.000 claims 2
- 241000446313 Lamella Species 0.000 claims 1
- 229910000033 sodium borohydride Inorganic materials 0.000 claims 1
- 239000012279 sodium borohydride Substances 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 abstract description 25
- 239000003054 catalyst Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 11
- 229910052737 gold Inorganic materials 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 239000002082 metal nanoparticle Substances 0.000 abstract description 6
- 229910052709 silver Inorganic materials 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000010531 catalytic reduction reaction Methods 0.000 abstract description 2
- -1 compound molybdenum sulfide Chemical class 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000004480 active ingredient Substances 0.000 abstract 2
- 239000002135 nanosheet Substances 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- 239000011157 advanced composite material Substances 0.000 description 28
- 238000006555 catalytic reaction Methods 0.000 description 21
- 239000010931 gold Substances 0.000 description 15
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- UKJLNMAFNRKWGR-UHFFFAOYSA-N cyclohexatrienamine Chemical group NC1=CC=C=C[CH]1 UKJLNMAFNRKWGR-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000003317 industrial substance Substances 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002696 acid base indicator Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000003907 antipyretic analgesic agent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229960005489 paracetamol Drugs 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- 239000011684 sodium molybdate Substances 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
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000009044 synergistic interaction Effects 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 210000001186 vagus nerve Anatomy 0.000 description 1
- 238000003911 water pollution 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
-
- B01J35/393—
-
- B01J35/396—
-
- B01J35/613—
-
- B01J35/647—
-
- B01J35/651—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C215/00—Compounds containing amino and hydroxy groups bound to the same carbon skeleton
- C07C215/74—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton
- C07C215/76—Compounds containing amino and hydroxy groups bound to the same carbon skeleton having hydroxy groups and amino groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton of the same non-condensed six-membered aromatic ring
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The invention belongs to a supported two-dimensional layered molybdenum sulfide composite material and discloses a noble metal (Ag, Au)-supported composite nano-catalytic material and its application in catalytic reduction of p-nitrophenol. The two-step synthetic technology is adopted in the invention. Firstly, molybdenum sulfide nanosheet with a porous ultrathin structure is synthesized by a hydrothermal method; then, by an ultraviolet reduction technology, noble metal nanoparticles are supported onto the surface of the two-dimensional layered compound molybdenum sulfide with a sandwich structure, and agglomeration phenomenon during the noble metal preparation process can be effectively avoided by the combination of nano confinement growth effects; and finally, noble metal nanoparticles with uniform size distribution are obtained. According to the supported catalyst system, the metal catalytic active center and a carrier together form a catalyst due to localized surface plasma resonance effect of noble metal active ingredients and synergistic effect between noble metal active ingredients and the carrier.
Description
Technical field
The invention belongs to nano material preparation technology and field of energy source environment protection, be specifically related to a kind of noble-metal-supported Novel composite nano catalyst and catalysis paranitrophenol (4-NP) reduction in application.
Background technology
Along with economic fast development; the a large amount of pollutant generated in industry and agricultural production bring great pollution to water body and ecological environment; the phenomenon environmental crisis making current hydropenia becomes more acute; and cause the organic pollution of water pollution all progressively increasing with the situation of 1000 kinds every year, wherein the material containing phenols is exactly very harmful one. Paranitrophenol is industrially the extremely intractable phenols organic pollution of one, it is easy to absorbed by the skin histology of people and lung, human body and ecological environment all can be brought great harm. , also there is ferrihemochrome disease and dyspnea in results of animal: nervus centralis and vagus nerve ending have stimulation and inhibitory action.
Para-aminophenol is a kind of critically important industrial chemicals, suffers from being widely applied very much at industrial circles such as chemical industry, medicine, fuel, rubber and oil dopes. Para-aminophenol is a kind of critically important industrial chemicals, suffers from extremely being widely applied at industrial circles such as chemical industry, medicine, fuel, rubber and oil dopes. Industrial and laboratory research finds that it is a kind of extremely effective and captivation measure that paranitrophenol is reduced into p-aminophenyl sweet smell. Therefore, the Substance Transformation that human body has with environment high risks is become the chemical intermediate that can be utilized, the protection of industrial expansion and environment all will be had great meaning and value.
Noble metal nanometer material is due to surface Raman enhancement effect, the dimensional effect of near infrared light thermal therapeutical effect and its uniqueness, it is made to become one of study hotspot in the last few years, owing to the Financial cost of major part noble metal is higher, researcher generally noble metal nano particles is dispersed in generally have bigger specific surface area and on the special carrier of better adsorption function, realize effective dispersion of noble metal, this load type catalyst system, metal active composition and carrier collectively form the entirety of catalyst, carrier is mainly metal active particle stretcher on the skeleton of carrier, prevent between the metallic formed, the free reunion caused between metallic, cause the activity reduction of catalyst, and then catalysis activity is produced negatively influencing.
Summary of the invention
It is an object of the invention to provide advanced composite material (ACM) of a kind of catalytic degradation paranitrophenol and preparation method thereof, and be applied to catalysis paranitrophenol reduction reaction, its preparation method is rationally simple, and catalysed reductive can be stable, and recall reduction efficiency is efficient.
The present invention adopts the molybdenum sulfide ultrathin nanometer sheet of Hydrothermal Synthesis, utilizes the molybdenum sulfide ultrathin nanometer sheet of synthesis under hydrothermal condition to have loose structure. then configure in certain density solution at precious metal salt, utilize ultraviolet light reduction technique, in conjunction with a nanometer principle for confinement growth, uniform for noble metal nano particles load is grown in molybdenum sulfide ultrathin nanometer sheet loose structure, finally obtain metal active composition and composite catalyst that carrier collectively forms, this kind of metal active composition and carrier collectively form catalyst, due to noble metal dispersion uniformly and and carrier molybdenum sulfide between Synergistic interaction, avoid reduction and the catalyst poisoning of noble metal active center catalysis activity, so that this novel two-dimensional layer molybdenum sulfide composite shows great catalysis activity in the reaction of catalysis reduction paranitrophenol.
For achieving the above object, the technical scheme that this discovery adopts is:
A kind of support type two-dimensional layer molybdenum sulfide composite, this composite is Ag load molybdenum sulfide ultrathin nanometer sheet, and described molybdenum sulfide nanometer sheet is to have loose structure, and its pore size is 5nm-100nm, and specific surface area is 10m2/ g～40m2/ g; Described Ag is nano-particle, is grown in the loose structure of molybdenum sulfide nanometer sheet uniformly, and Ag nano-particle is of a size of 2nm-6nm. The load capacity of Ag is 1wt%～40wt%. It is preferably 1wt%, 2wt%, 4wt%, 5wt%, 10wt%. It is 5wt% by the load capacity of more preferably Ag.
Described composite can also be Au load molybdenum sulfide ultrathin nanometer sheet; Described Au is nano-particle, and homoepitaxial is in the loose structure of molybdenum sulfide ultrathin nanometer sheet, and the nanoparticle size of Au is 3nm-9nm. The preparation method of the NEW TYPE OF COMPOSITE function nano catalyst with circulation catalysis of carried noble metal of the present invention includes several steps:
(1) ammonium molybdate is dissolved in a certain amount of deionized water, and 5min is until all dissolving in stirring, is subsequently adding a certain amount of thiourea, and stirring 30min is until whole white solids dissolves, and forms nattier blue solution.
(2) the light blue solution obtained in step (1) is transferred in the inner liner of reaction kettle of 5mL politef, reactor is transferred to insulation 24h in the thermostatic drying chamber of 140 DEG C～220 DEG C, after naturally cool to room temperature, the mixing liquid of black will be obtained, the mixed liquor product obtained is after 6000r/min～9000r/min centrifugation, adopting distilled water and dehydrated alcohol to wash respectively successively three times, the black product obtained can obtain molybdenum sulfide ultrathin nanometer sheet material at 60 DEG C～100 DEG C baking temperatures.
(3) molybdenum sulfide ultrathin nanometer sheet powder step (2) obtained joins in the mixed solution that deionized water is 1:1～1:10 with ethanol volume, add the certain density silver nitrate solution of 0.1mL～4mL, ultrasonic disperse a period of time, the mercury lamp that power is 500W is utilized to utilize ultraviolet light reduction to obtain the mixing liquid of black, after the mixed liquor product obtained is performing centrifugal separation on, adopting distilled water and dehydrated alcohol to wash respectively successively three times, the black solid product obtained can obtain Ag load molybdenum sulfide ultrathin nanometer sheet composite after drying.
In above-mentioned steps (1), the ammonium molybdate of addition and the mol ratio of thiourea are 1:20-40 (being preferably 1:30). The molybdenum source of step (1) can also change sodium molybdate into, and sulfur source therein can also change sodium sulfide or thioacetamide into.
In above-mentioned steps (3), the molybdenum sulfide ultrathin nanometer sheet powder obtained is joined in the mixed solution of deionized water and ethanol, wherein, the volume of deionized water and ethanol is 10mL, the molybdenum sulfide ultrathin nanometer sheet powder added is 95mg, the concentration of silver nitrate solution is 5mg/L, the ultrasonic disperse time is 30min, the mercury lamp that power is 500W is utilized to utilize ultraviolet light reduction to obtain the mixing liquid of brown, the time of institute's illumination is 4h, the black mixed liquor product obtained is after 6000r/min～9000r/min centrifugation, distilled water and dehydrated alcohol is adopted to wash three times respectively successively, the black product obtained can obtain Ag load molybdenum sulfide ultrathin nanometer sheet composite at 60 DEG C～90 DEG C baking temperatures.
The present invention also provides for a kind of application by above-mentioned support type two-dimensional layer molybdenum sulfide composite on degraded paranitrophenol. Concretely comprise the following steps composite and be added in the solution of the paranitrophenol that concentration is 5mg/L～20mg/L in the ratio of 0.15g/L～0.5g/L, and by than row add certain mass potassium borohydride, reaction carries out under dark room conditions, reaction temperature is room temperature, response time is 3min～5min, can complete the reduction of whole paranitrophenols.
Catalytic reduction method described in above-mentioned steps, described adds by being 0.3g/L～0.5g/L than the row potassium borohydride concentration joined in reactant liquor.
Described paranitrophenol is used as the raw material of dyestuff intermediate, medicine and pesticide and is used as acid-base indicator and analytical reagent, is a kind of very intractable containing one of phenolic comp ' ds pollution in industrial wastewater. 4-nitrophenol (4-NP) is classified as priority pollutants by Environmental Protection Agency (EPA), it is a kind of good and very attractive measure that paranitrophenol is reduced into p-aminophenyl sweet smell, chemistry transfer is the selection reducing its environmental toxicity, the antipyretic analgesic acetaminophen of para-aminophenol derivative synthesis as far back as the forties Britain just begin to promote the use of, the industrial demand to para-aminophenol (4-AP) is continuously increased, believe along with the industrial growth requirement of development of society, the preparation scheme of para-aminophenol and technique can the more next moon important, therefore paranitrophenol is made this reaction of para-aminophenol there is extremely important academic significance and environment protection significance.
The present invention adopts two step synthesis technology, molybdenum sulfide nanometer sheet first with water heat transfer porous superthin structure, then ultraviolet light reduction technique is utilized, noble metal nano particles is loaded to the surface of the two-dimensional layer compound molybdenum sulfide with sandwich structure, can effectively avoid the agglomeration in noble metal preparation process in conjunction with nanometer confinement growth effects, finally obtain the noble metal nano particles that size distribution is homogeneous. This load type catalyst system, metal catalytic activity center and carrier collectively form catalyst, due to the cooperative effect between local surface plasma resonance effect and noble metal active composition and the carrier of noble metal active composition, greatly improve the catalytic efficiency of catalyst, and reduce paranitrophenol in catalysis and show extremely efficient and stable catalysis activity.
Accompanying drawing explanation
Fig. 1: the X-ray diffractogram of the advanced composite material (ACM) of the carried noble metal silver prepared for embodiment 2.
Fig. 2: the X-ray diffractogram of the advanced composite material (ACM) of the carried noble metal gold prepared for embodiment 3.
Fig. 3: the transmission electron microscope picture of the advanced composite material (ACM) of the carried noble metal silver prepared for embodiment 2.
Fig. 4: the grain size distribution of the advanced composite material (ACM) that load capacity is 5wt% of the carried noble metal silver prepared for embodiment 2.
Fig. 5: the transmission electron microscope picture of the advanced composite material (ACM) of the carried noble metal gold prepared for embodiment 3.
Fig. 6: the grain size distribution of the advanced composite material (ACM) that load capacity is 5wt% of the carried noble metal gold prepared for embodiment 3.
Fig. 7: for the advanced composite material (ACM) catalysis reduction paranitrophenol uv-visible absorption spectra phenogram of the carried noble metal silver that embodiment 2 prepares.
Fig. 8: for the advanced composite material (ACM) catalysis reduction paranitrophenol uv-visible absorption spectra phenogram of the carried noble metal gold that embodiment 3 prepares.
Fig. 9: for the advanced composite material (ACM) catalysis reduction paranitrophenol color variation diagram of the carried noble metal silver that embodiment 2 prepares
Figure 10: for the advanced composite material (ACM) catalysis reduction paranitrophenol color variation diagram of the carried noble metal gold that embodiment 3 prepares
Detailed description of the invention:
Below in conjunction with being embodied as case row, the present invention is expanded on further, it should be understood that these embodiments are merely to illustrate the present invention rather than restriction the scope of the present invention, after having read the present invention, the amendment of the various equivalent form of values of the present invention is all fallen within the application claims limited range by those skilled in the art.
Embodiment 1
1) being dissolved in the deionized water of 35ml by the ammonium molybdate of 1mmol, stirring 5min is until all dissolving the solution A forming transparent and homogeneous.
2) thiourea of 30mmol is joined in solution A, and stir 30min mix homogeneously, form homogeneous light blue solution B.
3) above-mentioned solution B being transferred in 50mL teflon-lined reactor, be warmed up to 220 DEG C, constant temperature time is 24h, then naturally cools to room temperature.
4) obtaining the mixing liquid of black, and after 9000r/min centrifugation 15min, adopt distilled water and dehydrated alcohol to wash respectively successively three times, the black product obtained can obtain molybdenum sulfide ultrathin nanometer sheet material at 80 DEG C of baking temperatures.
Embodiment 2
1) using the molybdenum sulfide ultrathin nanometer sheet that obtains in embodiment 1 as carrier masterplate, the molybdenum sulfide ultrathin nanometer sheet of 95mg is joined in the deionized water of 20mL and the mixed solution of dehydrated alcohol, wherein the volume ratio of deionized water and dehydrated alcohol is 1:1, it is subsequently adding the salpeter solution of the 5mg/L of 1mL, by above-mentioned mixing liquid ultrasonic 30min, then darkroom stirring 30min, forms the suspension A that mixing is homogeneous.
2) above-mentioned suspended liquid A being transferred in the quartz test tube of photochemical reactor, when stirring, utilize the mercury lamp that power is 500W to utilize irradiation under ultraviolet ray 4h, reduction obtains the mixing liquid B of black.
3) the mixing product liquid B of the black obtained, after 9000r/min centrifugation 15min, adopts deionized water and dehydrated alcohol to wash respectively three times successively, and the black product obtained can obtain AgMoS at 80 DEG C of baking temperatures2Advanced composite material (ACM).
The support type two-dimensional layer molybdenum sulfide (AgMoS of the precious metals ag load of above-mentioned preparation2) X ray diffracting spectrum of composite is as it is shown in figure 1, its diffraction maximum is consistent with molybdenum sulfide standard diagram.
The support type two-dimensional layer molybdenum sulfide (AgMoS of the precious metals ag load of above-mentioned preparation2) the transmission electron microscope picture of composite is as it is shown on figure 3, it can be seen that Ag nano particles grows in molybdenum sulfide ultrathin nanometer sheet material surface and duct uniformly.
The support type two-dimensional layer molybdenum sulfide (AgMoS of the precious metals ag load of above-mentioned preparation2) composite Ag nano-particle particle size distribution as shown in Figure 4, size is 2nm～6nm.
The advanced composite material (ACM) of above-mentioned preparation is carried out 2 catalysis reduction of paranitrophenol, by 150mgAgMoS2It is in the solution that 300mL concentration is the paranitrophenol of 14mg/L that composite is added to concentration, and add 150mg potassium borohydride, reaction carry out when room nature light or dark, reaction temperature is room temperature. Take out supernatant test at regular intervals, utilize ultra-violet and visible spectrophotometer (UV-2550), the catalysis reduction situation of paranitrophenol is detected by measuring the solution absorbance at maximum absorption wavelength (400nm) place, react through 5min, the catalysis reduction of paranitrophenol 100% can be completed, by experimental data is researched and analysed discovery, above-mentioned reaction is first order kinetics reaction, and catalysis rate of reduction is main relevant with the concentration of reacting substance.
Embodiment 3
1) using the molybdenum sulfide ultrathin nanometer sheet that obtains in embodiment 1 as carrier masterplate, the molybdenum sulfide ultrathin nanometer sheet of 95mg is joined in the deionized water of 20mL and the mixed solution of ethanol, wherein the volume ratio of deionized water and ethanol is 1:1, it is subsequently adding the sodium chloraurate solution of the 5mg/L of 1mL, by above-mentioned mixing liquid ultrasonic 30min, then darkroom stirring 30min, forms the suspension A that mixing is homogeneous.
2) above-mentioned suspended liquid A being transferred in the quartz test tube of photochemical reactor, when stirring, utilize the mercury lamp that power is 500W to utilize irradiation under ultraviolet ray 4h, reduction obtains the mixing liquid B of black. 3) by mixed liquor product obtained above after 9000r/min centrifugation 15min, adopting distilled water and dehydrated alcohol to wash respectively successively three times, the black product obtained can obtain AuMoS at 80 DEG C of baking temperatures2Advanced composite material (ACM).
Graphite-phase nitrogen carbide (the AuMoS of the noble metal Au load of above-mentioned preparation2) X ray diffracting spectrum of composite as in figure 2 it is shown, its diffraction maximum is consistent with graphite-phase nitrogen carbide and cube golden standard diagram, illustrate that product is graphite-phase nitrogen carbide and the complex of gold.
The support type two-dimensional layer molybdenum sulfide (AuMoS of the noble metal Au load of above-mentioned preparation2) composite transmission electron microscope picture as it is shown in figure 5, it can be seen that nanometer Au evengranular growth MoS2Surface and duct in.
The support type two-dimensional layer molybdenum sulfide (AuMoS of the noble metal Au load of above-mentioned preparation2) composite Au nano-particle particle size distribution as shown in Figure 6, size is 3nm～9nm.
Utilize the above-mentioned support type two-dimensional layer molybdenum sulfide (AuMoS preparing noble metal Au load2) composite carry out paranitrophenol catalysis reduction, by 150mgAuMoS2It is in the solution that 300mL concentration is the paranitrophenol of 14mg/L that composite is added to concentration, and add 150mg potassium borohydride, reaction carry out when room nature light or dark, reaction temperature is room temperature. Take out supernatant test at regular intervals, utilize ultra-violet and visible spectrophotometer, catalysis situation is judged at the absorbance of maximum absorption wavelength (400nm) by measuring solution, elapsed time is 4min reaction, the catalysis reduction of paranitrophenol 100% can be completed, by experimental data is researched and analysed discovery, above-mentioned reaction is first order kinetics reaction, and catalysis rate of reduction is main relevant with the concentration of reacting substance.
Claims (10)
1. a novel load noble metal two-dimensional layer molybdenum sulfide composite, it is characterised in that this composite is the molybdenum sulfide of Ag load; Described molybdenum sulfide is flaky nanometer structure, and lamella is sized to 100nm-200nm, and specific surface area is 10m2/ g～40m2/ g; Described Ag be nano-particle homoepitaxial in the surface and duct of molybdenum sulfide nanometer sheet, the nanoparticle size of Ag is 2nm-6nm.
2. the support type two-dimensional layer type molybdenum sulfide composite described in claims 1, it is characterised in that the load capacity of Ag is 0.5wt%～40wt%.
3. the support type two-dimensional layer type molybdenum sulfide composite described in claim 1, it is characterised in that described composite can also be Au load two-dimensional layer type molybdenum sulfide; Described Au is nano-particle, and homoepitaxial is in the surface and duct of two-dimensional layer type molybdenum sulfide, and the nanoparticle size of Au is 3nm-9nm.
4. the preparation method of support type two-dimensional layer type molybdenum sulfide composite described in any one of claim 1-3, it is characterised in that comprise the steps:
(1) ammonium molybdate is dissolved in a certain amount of deionized water, and stirring obtains the ammonium molybdate solution of 25g/L～40g/L to all dissolvings, is subsequently adding a certain amount of thiourea, and stirring 30min, until all solids dissolves, finally obtains solution azury; Wherein ammonium molybdate is 1:20-40 with the mol ratio of thiourea.
(2) the light blue solution obtained in step (1) is transferred in the reactor that politef is liner of 50mL, it is heated to 140 DEG C～220 DEG C with 6 DEG C/min～20 DEG C of heating rate/min, and it is incubated 12h～24h, and the straight room temperature of natural cooling, obtain black mixed liquor;
(3) by the black mixed liquor product that obtains in step (2) after 6000r/min～9000r/min centrifugation, and adopt distilled water and dehydrated alcohol to wash respectively successively three times, the pressed powder obtained 60 DEG C～80 DEG C of baking temperatures two-dimensional layer type molybdenum sulfide nanometer sheet;
(4) two-dimensional layer type molybdenum sulfide nanometer sheet powder step (3) obtained joins in the mixed solution that deionized water is 1:1～1:10 with ethanol volume, add the silver nitrate solution that concentration is 5mg/L of 0.1mL～4mL, ultrasonic disperse 30min, the hydrargyrum lamp using power to be 500W, ultraviolet light reduction is utilized to obtain the mixing liquid of black, the mixed liquor product obtained is after 6000r/min～9000r/min centrifugation, distilled water and dehydrated alcohol is adopted to wash three times respectively successively, the black powder obtained can obtain carried noble metal two-dimensional layer molybdenum sulfide composite at 60 DEG C～90 DEG C baking temperatures.
5. the preparation method of the molybdenum sulfide composite of support type two-dimensional layer type described in claims 4, it is characterised in that in step (4), described silver nitrate may be replaced by sodium chloraurate.
6. the preparation method of carried noble metal two-dimensional layer molybdenum sulfide composite described in claims 4, it is characterized in that, with the heating rate heating direct 220 DEG C of 10 DEG C/min in step (2), and it is incubated 24h, the straight room temperature of natural cooling, obtains two-dimensional layer type molybdenum sulfide ultrathin nanometer sheet then through step (3).
7. the preparation method of the molybdenum sulfide composite of support type two-dimensional layer type described in claims 4, it is characterized in that, in step (4), the two-dimensional layer molybdenum sulfide nanometer sheet powder obtained is joined in the mixed solution of deionized water and ethanol, wherein, the volume ratio of deionized water and ethanol is respectively 10mL and 10mL, add the silver nitrate solution that concentration is 5mg/L of 1mL, then dimension layered-type molybdenum sulfide ultrathin nanometer sheet is joined ultrasonic disperse 30min in above-mentioned mixed solution, the mercury lamp that power is 500W is utilized to utilize ultraviolet light reduction to obtain the mixing liquid of black, the mixed liquor product obtained is after 9000r/min centrifugation, distilled water and dehydrated alcohol is adopted to wash three times respectively successively, the black product obtained can obtain Ag load two-dimensional layer molybdenum sulfide composite at 80 DEG C of baking temperatures.
8. the application on degraded paranitrophenol of the support type two-dimensional layer type molybdenum sulfide composite described in any one of claim 1-7.
9. the application described in claim 8, it is characterized in that, concrete steps include as follows: be added in the solution of the paranitrophenol that concentration is 5mg/L～20mg/L by support type two-dimensional layer type molybdenum sulfide composite in the ratio of 0.15g/L～0.5g/L, add a certain amount of potassium borohydride or sodium borohydride solids powder, reaction carries out under dark room conditions, reaction temperature is room temperature, and the response time is 3min～5min, can complete the reduction of whole paranitrophenols.
10. the application described in claim 9, it is characterised in that potassium borohydride concentration is 0.3g/L～0.5g/L.
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