CN107999077B - Tri-metal nano-grade Prussian-like blue material and application thereof - Google Patents
Tri-metal nano-grade Prussian-like blue material and application thereof Download PDFInfo
- Publication number
- CN107999077B CN107999077B CN201711310285.9A CN201711310285A CN107999077B CN 107999077 B CN107999077 B CN 107999077B CN 201711310285 A CN201711310285 A CN 201711310285A CN 107999077 B CN107999077 B CN 107999077B
- Authority
- CN
- China
- Prior art keywords
- nano
- trimetal
- prussian
- prussian blue
- blue
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000463 material Substances 0.000 title claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 title abstract description 4
- 239000002184 metal Substances 0.000 title description 3
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229960003351 prussian blue Drugs 0.000 claims abstract description 14
- 239000013225 prussian blue Substances 0.000 claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- UCFIGPFUCRUDII-UHFFFAOYSA-N [Co](C#N)C#N.[K] Chemical compound [Co](C#N)C#N.[K] UCFIGPFUCRUDII-UHFFFAOYSA-N 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- -1 potassium ferricyanide Chemical compound 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 3
- 239000004745 nonwoven fabric Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract 1
- 230000010757 Reduction Activity Effects 0.000 abstract 1
- 229910052700 potassium Inorganic materials 0.000 abstract 1
- 239000011591 potassium Substances 0.000 abstract 1
- 239000000276 potassium ferrocyanide Substances 0.000 abstract 1
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 abstract 1
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 31
- 238000006722 reduction reaction Methods 0.000 description 7
- 230000003712 anti-aging effect Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 239000005060 rubber Substances 0.000 description 5
- 238000010531 catalytic reduction reaction Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 2
- ZFIQGRISGKSVAG-UHFFFAOYSA-N 4-methylaminophenol Chemical compound CNC1=CC=C(O)C=C1 ZFIQGRISGKSVAG-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000000987 azo dye Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 2
- 239000013256 coordination polymer Substances 0.000 description 2
- 229920001795 coordination polymer Polymers 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000988 sulfur dye Substances 0.000 description 2
- IBRKLUSXDYATLG-LURJTMIESA-N (S)-salsolinol Chemical compound OC1=C(O)C=C2[C@H](C)NCCC2=C1 IBRKLUSXDYATLG-LURJTMIESA-N 0.000 description 1
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229930003451 Vitamin B1 Natural products 0.000 description 1
- 239000000980 acid dye Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 125000001769 aryl amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960001506 brilliant green Drugs 0.000 description 1
- HXCILVUBKWANLN-UHFFFAOYSA-N brilliant green cation Chemical compound C1=CC(N(CC)CC)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](CC)CC)C=C1 HXCILVUBKWANLN-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- 239000000982 direct dye Substances 0.000 description 1
- 239000000986 disperse dye Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000037308 hair color Effects 0.000 description 1
- 239000000118 hair dye Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FFXSKLNKKMNFDZ-UHFFFAOYSA-N iron 4-nitrophenol Chemical compound [Fe].[N+](=O)([O-])C1=CC=C(C=C1)O FFXSKLNKKMNFDZ-UHFFFAOYSA-N 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- KBOPZPXVLCULAV-UHFFFAOYSA-N mesalamine Chemical compound NC1=CC=C(O)C(C(O)=O)=C1 KBOPZPXVLCULAV-UHFFFAOYSA-N 0.000 description 1
- 229960004963 mesalazine Drugs 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229960005489 paracetamol Drugs 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229940074569 salsolinol Drugs 0.000 description 1
- IBRKLUSXDYATLG-UHFFFAOYSA-N salsolinol hydrobromide Natural products OC1=C(O)C=C2C(C)NCCC2=C1 IBRKLUSXDYATLG-UHFFFAOYSA-N 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229960003495 thiamine Drugs 0.000 description 1
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000011691 vitamin B1 Substances 0.000 description 1
- 235000010374 vitamin B1 Nutrition 0.000 description 1
Images
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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B01J35/61—
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/25—Reduction
Abstract
The invention discloses a preparation method of a nano-scale trimetal Prussian blue nano-material. The preparation method of the nano-scale Prussian blue-like nano material adopts precursor salt containing metallic element nickel and a proper amount of potassium ferrocyanide and potassium cobaltoside as raw materials, and adopts a coprecipitation method to prepare the nano material; the chemical composition of the nano-scale Prussian blue-like material is NiHCNCOxFe1‑x. The production method is simple, the raw materials are low in price, and the method is suitable for large-scale industrial production. The prepared Prussian-like blue nano material has a nano size and uniform particle size, can be used for reducing p-nitrophenol, and has better p-nitrophenol reduction activity.
Description
Technical Field
The invention belongs to the field of preparation and application of clean and sustainable novel materials, and particularly relates to a nanoscale trimetal Prussian blue nano material and application thereof.
Background
P-aminophenol, english name: para-aminophenol, abbreviated as PAP, of formula: c6H7ON, molecular weight: 109.12. the p-nitrophenol has active chemical property, can carry out various reactions which can occur in phenolic hydroxyl and arylamino, and can also carry out substitution reaction on a benzene ring, so the p-nitrophenol is an important organic chemical raw material and a medical intermediate, and can be widely applied to industries such as medicines, dyes, rubber auxiliaries and the like.
As a medical intermediate, the p-aminophenol is mainly used for producing medicines such as paracetamol, plasma supplement, vitamin B1 and the like in the aspect of medicine; and is also the main raw material of the salsolinol.
In the rubber industry, p-aminophenol is mainly used for producing p-phenylenediamine antioxidants, and the products are matched antioxidants of radial tires with development prospects. The demand for aminophenol has increased in recent years with the rapid increase in domestic tire production. The p-phenylenediamine anti-aging agent is non-toxic, efficient and pollution-free, is a commonly-used excellent anti-aging agent in the rubber industry, gradually replaces an anti-aging agent A and an anti-aging agent D to form a main rubber anti-aging agent variety, has the trend of rapid development, and the future demand is likely to exceed other usage. Therefore, the application prospect of the p-aminophenol in the rubber industry is very wide.
In the dye industry, p-aminophenol can be used as an intermediate of various dyes such as disperse dyes, azo dyes, oxidation dyes, acid dyes, sulfur dyes, hair dyes, direct dyes, neutral dyes and the like, and is a raw material for producing 5-aminosalicylic acid serving as an intermediate of sulfur and azo dyes. The main use of p-aminophenol in China is to produce the sulphur red brown B3R, vulcanized vat black C L G, vulcanized brilliant green GB, vulcanized sapphire blue CV, fur brown, vulcanized new blue FB L and the like.
In the photosensitive material industry, p-aminophenol can be used as a photosensitive chemical to prepare a developer solution metol; 4- (N-methylamino) phenol synthesized from p-aminophenol and its salts inhibit metal corrosion and can also be used as an intermediate of hair coloring agent; the synthesized 4- (N-anilino phenol) can be used as a polymerization inhibitor of vinyl monomers and an antioxidant of lubricating oil; p-aminophenol is used in some developments in the processes of urea addition reaction, acrylonitrile dimerization reaction, and the like; it can also be used to synthesize adhesive, insecticide, additive for petroleum products, herbicide, etc. With the development of fine chemical engineering, other applications of p-aminophenol are being continuously developed, and it is expected that the application field will gradually widen with the continuous and deep research on p-aminophenol.
The main industrial production method of p-aminophenol is a catalytic hydrogenation reduction method of p-nitrophenol, and the specific steps are that the p-aminophenol is used as a raw material, and the p-aminophenol is prepared through hydrogenation reduction reaction under the conditions of catalysts such as Pt, Pd, Ni and the like and certain temperature, pressure and composition. The reaction formula is as follows:
3NaBH4+2 2HO–C6H4–NO2+2H2O→2NaBO2+2 2HO–C6H4–NH2+6H2the method for producing p-nitrophenol ↓ischaracterized by simple process, high quality of the produced finished product, elimination of iron mud pollution in the p-nitrophenol iron powder reduction method, wide development prospect and being the mainstream research direction in the world at present.
The Prussian-like blue particles are an important coordination polymer, and like other coordination polymers, the Prussian-like blue particles have the advantages of extremely large specific surface, very high porosity, uniform and adjustable pore diameter and the like. The great variety of prussian-like blue particles is caused by the fact that in the prussian blue unit cell, transition metal ions occupy two different positions, and different other transition metals can be substituted for the two positions. Their properties are advantageous and deserve intensive research. The method adopts a trimetal nano Prussian-like blue material, and realizes the high-performance p-nitrophenol catalytic reduction reaction by utilizing the properties of high specific surface area, high adsorption capacity and a large number of hydrogenation active sites of a Prussian-like blue nano structure.
Disclosure of Invention
The invention aims to provide a trimetal nanoscale Prussian-like blue material and application thereof aiming at the defects of the prior art.
The purpose of the invention is realized by the following technical scheme: a trimetal nanoscale Prussian-like blue material is prepared by the following steps:
(1) mixing potassium cobalt cyanide: potassium ferricyanide: dissolving nickel nitrate hexahydrate in deionized water according to the mass ratio of 1:3:5.2 to obtain a mixed aqueous solution of three precursors;
(2) dissolving sodium citrate in the mixed aqueous solution of the three precursors in the step 1, standing and reacting for 24 hours; wherein the mass ratio of the sodium citrate to the potassium cobalt cyanide is 8.02: 1.
(3) And (3) cleaning a light yellow product obtained by the reaction in the step (2) by using ethanol, and performing vacuum drying for 24 hours at the temperature of 60 ℃ to obtain the trimetal nano-grade Prussian-blue-like material.
The invention has the beneficial effects that: the invention obtains the trimetal nano Prussian-like blue material by a simple one-step coprecipitation method, and the material can be applied to catalytic hydrogenation reduction reaction of p-nitrophenol. In the aspect of catalytic activity, the trimetal nanoscale Prussian-like blue material has the properties of high porosity, high specific surface area, multiple catalytic reduction active sites and nano-size effect. Compared with the micron-sized Prussian-like blue material obtained by conventional reaction, the material has higher catalytic reduction reaction activity on p-nitrophenol.
Drawings
FIG. 1 is a scanning electron microscope picture of a trimetal nanoscale Prussian-like blue material prepared by the invention.
FIG. 2 is a transmission electron microscope image of the trimetal nanoscale Prussian-like blue material prepared by the present invention.
FIG. 3 is a spectrum diagram of a trimetallic nanoscale Prussian-like blue material prepared by the invention.
FIG. 4 is a reaction curve of catalytic reduction of p-nitrophenol in preparation of a trimetal nanoscale Prussian-like blue material.
Detailed Description
The technical solution of the invention is further illustrated below with reference to examples, which are not to be construed as limiting the technical solution.
Example 1: the preparation of the trimetal nanoscale Prussian-like blue material in the embodiment specifically comprises the following steps:
(1) dissolving 0.033g of potassium cobalt cyanide, 0.1745g of nickel nitrate hexahydrate and 0.099g of potassium ferricyanide in 20m L of deionized water, and stirring by magnetic force to fully dissolve the potassium ferricyanide and the potassium cobaltcyanide to obtain a mixed aqueous solution of three precursors;
(2) 0.2647g of sodium citrate is dissolved in the mixed aqueous solution of the three precursors in the step 1, and the mixture is kept stand and reacted for 24 hours;
(3) and (3) cleaning a light yellow product obtained by the reaction in the step (2) by using ethanol, and performing vacuum drying for 24 hours at the temperature of 60 ℃ to obtain the trimetal nano-grade Prussian blue-like material.
Fig. 1 is a scanning electron microscope image of the trimetal nanoscale prussian blue material prepared by the invention, from which it can be seen that the main morphology of the trimetal nanoscale prussian blue is a nanocube structure with uniform size, and from fig. 1, it can be seen that the average particle size of the trimetal nanoscale prussian blue is 49 nm. FIG. 2 is a transmission electron microscope image of the trimetallic nanoscale Prussian-like blue prepared in the present invention. As can be seen from the figure, the trimetallic nanoscale prussian blue-like nanostructure is a loose and porous nanostructure, and the structure is favorable for the adsorption of reactants and the occurrence of catalytic reaction.
Example 2, in this example, the trimetal nanoscale prussian blue prepared in example 1 is used to prepare a recoverable device, specifically, 3mg of dried trimetal nanoscale prussian blue is added into a deionized water-ethanol mixed solution with a volume ratio of 1.5m L (3: 1), and ultrasonic treatment is performed for half an hour to obtain a suspension, and then a pipetting gun is used to measure the suspension and drip-coat the suspension on a non-woven fabric, and the recovered device of trimetal nanoscale prussian blue is obtained after natural drying.
Example 3: the recyclable device prepared in the embodiment 2 is applied to p-nitrophenol reduction reaction, and specifically comprises the following steps:
inserting the trimetal nano Prussian blue modified non-woven fabric into NaBH4The spectrum detection is carried out in real time in excessive 0.1M p-nitrophenol aqueous solution, the absorption peak at 400nm is the absorption peak of hydrogenated p-aminophenol, the absorption peak is gradually reduced along with the reaction, and finally a curve of the peak intensity along with the time change is obtained, as shown in figure 4. The preparation method of the trimetal nanoscale Prussian-like blue prepared by the method is simple, high in repeatability and strong in operability. As a novel p-nitrophenol reduction catalyst, the catalyst shows extremely high reduction reaction activity.
Claims (1)
1. The nanometer trimetallic Prussian blue nano material is characterized by being prepared by the following steps:
(1) mixing potassium cobalt cyanide: potassium ferricyanide: dissolving nickel nitrate hexahydrate in deionized water according to the mass ratio of 1:3:5.2 to obtain a mixed aqueous solution of three precursors;
(2) dissolving sodium citrate in the mixed aqueous solution of the three precursors in the step (1), standing and reacting for 24 hours; wherein the mass ratio of the sodium citrate to the potassium cobalt cyanide is 8.02: 1;
(3) cleaning a light yellow product obtained by the reaction in the step (2) with ethanol, and performing vacuum drying at 60 ℃ for 24 hours to obtain a trimetal nanoscale Prussian blue material;
the trimetal nano Prussian blue nano material is applied to preparing an electrode, and the preparation method of the electrode comprises the steps of adding 3mg of dried trimetal nano Prussian blue into 1.5m L of deionized water-ethanol mixed solution with the volume ratio of 3:1, carrying out ultrasonic treatment for half an hour to obtain suspension, then measuring the suspension by using a liquid transfer gun, dripping the suspension on non-woven fabrics, and naturally drying to obtain the recyclable trimetal nano Prussian blue device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711310285.9A CN107999077B (en) | 2017-12-11 | 2017-12-11 | Tri-metal nano-grade Prussian-like blue material and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711310285.9A CN107999077B (en) | 2017-12-11 | 2017-12-11 | Tri-metal nano-grade Prussian-like blue material and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107999077A CN107999077A (en) | 2018-05-08 |
| CN107999077B true CN107999077B (en) | 2020-07-10 |
Family
ID=62058246
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711310285.9A Active CN107999077B (en) | 2017-12-11 | 2017-12-11 | Tri-metal nano-grade Prussian-like blue material and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107999077B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993511A (en) * | 2018-06-14 | 2018-12-14 | 五邑大学 | A kind of preparation method of the porous iron-doped nickel oxide elctro-catalyst of superfine nano |
| CN108855159B (en) * | 2018-06-27 | 2021-07-20 | 广东工业大学 | Cobalt phosphide synthesized by prussian blue derivative and preparation method and application thereof |
| CN113104862A (en) * | 2021-03-17 | 2021-07-13 | 山东师范大学 | Method for rapidly preparing Prussian blue or analogues thereof in batches and application of method |
| CN113960140B (en) * | 2021-09-24 | 2023-11-21 | 合肥天一生物技术研究所有限责任公司 | Screen printing electrode for detecting vitamin B1 content in blood plasma |
| CN114438527B (en) * | 2022-02-19 | 2023-05-23 | 福州大学 | Synthesis method and application of trimetallic Prussian blue catalyst |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106470758B (en) * | 2014-06-06 | 2019-07-19 | 国立研究开发法人产业技术综合研究所 | Ammonia adsorbent material |
| CN107253731A (en) * | 2017-07-13 | 2017-10-17 | 大连民族大学 | A kind of high-performance super capacitance electrode material Co Fe Prussian blue analogue nano cubics and its preparation method and application |
-
2017
- 2017-12-11 CN CN201711310285.9A patent/CN107999077B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| "Evaluating Prussian blue analogues M3II[MIII(CN)6]2(MII=Co,Cu,Fe,Mn,Ni;MIII=Co,Fe) as activators for peroxymonosulfate in water";Kun-Yi Andrew Lin,et al;《RSC Adv.》;20160916;全文 * |
| "Prussian blue and its derivatives as electrode materials for electrochemical energy storage";Yuxia Xu，et al;《Energy Storage Materials》;20170607;全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107999077A (en) | 2018-05-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107999077B (en) | Tri-metal nano-grade Prussian-like blue material and application thereof | |
| CN102891016B (en) | A kind of cobalt acid nickel graphene composite material and application thereof and preparation method | |
| CN106732564B (en) | Aromatic hydrogenation rhodium/activated-carbon catalyst preparation method and application | |
| Maslamani et al. | Carboxymethyl cellulose nanocomposite beads as super-efficient catalyst for the reduction of organic and inorganic pollutants | |
| CN103977802B (en) | Nanometer needle-like nickel bag graphite compound particle and its preparation method and application | |
| Li et al. | Enhanced photocatalytic hydrogen production of CdS embedded in cationic hydrogel | |
| CN110283456A (en) | A kind of preparation method of graphene and secondary doping state polyaniline nano-composite material | |
| CN104107691A (en) | Novel Ru/CNTs catalyst used for preparing sorbitol through glucose hydrogenation, and preparation and application method thereof | |
| CN108579815A (en) | A kind of bimetallic organic framework catalyst and its preparation method and application | |
| Vandarkuzhali et al. | Arachis hypogaea derived activated carbon/Pt catalyst: reduction of organic dyes | |
| CN107899581B (en) | Loaded on SiO2Preparation method and application of nickel catalyst on microspheres | |
| Jin et al. | Strong interaction between Au nanoparticles and porous polyurethane sponge enables efficient environmental catalysis with high reusability | |
| CN112663076A (en) | Iron-doped molybdenum diselenide nano material with hollow structure, preparation method thereof and application of iron-doped molybdenum diselenide nano material in electrocatalytic nitrogen reduction | |
| CN104558598A (en) | One-step method for synthesizing poly(m-phenylenediamine) and graphene composite material and application of composite material to electric adsorption of heavy metal ions in water | |
| WO2018133196A1 (en) | Phosphor-doped carbon material hydrogenation catalyst, preparation method therefor and use thereof | |
| Naghash-Hamed et al. | The efficacy of carbon quantum dots decorated magnetic metal ferrite nanocomposites in reducing of 4-nitrophenol | |
| Kong et al. | Templated synthesis of polyaniline nanotubes with Pd nanoparticles attached onto their inner walls and its catalytic activity on the reduction of p-nitroanilinum | |
| CN105080603B (en) | Catalyst for aniline preparation by selective hydrogenation of nitrobenzene as well as preparation method and application method of catalyst | |
| CN103772702A (en) | Poly 1-naphthylamine nano hollow structure and its preparation method | |
| CN104003892A (en) | Catalytic hydrogenation preparation method of 3,5-diaminobenzoic acid | |
| CN111054340A (en) | Catalyst with straw-graphene heterozygote as carrier and zero-valent copper loaded in situ, and preparation method and application thereof | |
| CN104190949A (en) | Method for green synthesis of nano platinum from vitamin C | |
| CN107715870A (en) | A kind of preparation method and application for preparing L aminopropanol ruthenium Pd/carbon catalysts | |
| CN107983297A (en) | A kind of heavy metal absorbent α-Al2O3The preparation method of nano-particle | |
| CN104475136B (en) | A kind of preparation method of Nitrobenzol catalytic hydrogenation catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |