CN106000413A - Method for preparing molybdenum doped akaganeite nanoparticles - Google Patents
Method for preparing molybdenum doped akaganeite nanoparticles Download PDFInfo
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- CN106000413A CN106000413A CN201610418162.6A CN201610418162A CN106000413A CN 106000413 A CN106000413 A CN 106000413A CN 201610418162 A CN201610418162 A CN 201610418162A CN 106000413 A CN106000413 A CN 106000413A
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- akaganeite
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 37
- 239000011733 molybdenum Substances 0.000 title claims abstract description 36
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title abstract description 6
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 title abstract 7
- 238000002360 preparation method Methods 0.000 claims abstract description 30
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 14
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 7
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 7
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 7
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 9
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims description 8
- XUFUCDNVOXXQQC-UHFFFAOYSA-L azane;hydroxy-(hydroxy(dioxo)molybdenio)oxy-dioxomolybdenum Chemical compound N.N.O[Mo](=O)(=O)O[Mo](O)(=O)=O XUFUCDNVOXXQQC-UHFFFAOYSA-L 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 150000002505 iron Chemical class 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims 1
- 235000011149 sulphuric acid Nutrition 0.000 claims 1
- 239000001117 sulphuric acid Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 32
- 239000003054 catalyst Substances 0.000 abstract description 14
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 235000003891 ferrous sulphate Nutrition 0.000 abstract description 5
- 239000011790 ferrous sulphate Substances 0.000 abstract description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 60
- 239000012153 distilled water Substances 0.000 description 30
- 238000003756 stirring Methods 0.000 description 30
- 239000000284 extract Substances 0.000 description 10
- 238000001027 hydrothermal synthesis Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 238000001556 precipitation Methods 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000000852 hydrogen donor Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 3
- 239000009671 shengli Substances 0.000 description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910003153 β-FeOOH Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- BHHGNNGTNDLKSU-UHFFFAOYSA-N benzenesulfonic acid;molybdenum Chemical compound [Mo].OS(=O)(=O)C1=CC=CC=C1 BHHGNNGTNDLKSU-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001833 catalytic reforming Methods 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 239000005078 molybdenum compound Substances 0.000 description 1
- 150000002752 molybdenum compounds Chemical class 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical class C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 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
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/881—Molybdenum and iron
-
- B01J35/40—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a method for preparing molybdenum doped akaganeite nanoparticles and belongs to the technical field of preparation of novel functional nano materials. The method for preparing the molybdenum doped akaganeite nanoparticles comprises the steps that an ammonium molybdate water solution is added into a molysite water solution, reacting is carried out for 24 hours or above at the temperature of 180 DEG C to 200 DEG C, the reaction liquid is centrifuged, washed and dried, and then the molybdenum doped akaganeite nanoparticles are obtained. The molar ratio of ammonium molybdate to molysite is 1:(20-50), and molysite is ferric trichloride or ferrous sulfate. The method for preparing the molybdenum doped akaganeite nanoparticles has the advantages that the process and equipment are simple, the raw materials are cheap and available, cost is high, and the yield is high, and is suitable for large-scale industrial production, the prepared molybdenum doped akaganeite nanoparticles are small in dimension, uniform in particle size and even in molybdenum dispersion, and an ideal effect can be achieved when the molybdenum doped akaganeite nanoparticles serve as a catalyst for hydrothermal catalytic viscosity reduction of thickened oil.
Description
Technical field
The invention belongs to novel function nanometer material preparation field, be specifically related to a kind of molybdenum doping kaganeite nanometer micro-
The preparation method of grain.
Background technology
Molybdenum element is to constitute some hydrogenation, dehydrogenation, hydrogenation deoxidation and the basis of Hydrobon catalyst.In recent years,
The compound of molybdenum serves preferable catalytic effect during viscous crude catalytic reforming.But in actual applications, molybdenum compound is general
Store-through is in relatively costly problem, such as, benzenesulfonic acid molybdenum belong to amphipathic metallo-chelate [Enery Fuels 2010,24,
1502-1510], preparation benzenesulfonic acid price used is higher.Compared with the catalyst such as ferrum oxide, nickel oxide, non-loaded pure two sulfur
Changing molybdenum, also there is relatively costly problem in molybdenum trioxide [Ind. Eng. Chem. Res. 2015,54,10645-10655].
Loading molybdenum catalyst can effectively improve the dispersibility of molybdenum and reduce the cost of catalyst, thus has the most wide
Scape is produced in application.Therefore, the supported molybdenum catalyst preparing a kind of economy and good dispersion is a kind of direction of research at present.
As a kind of adsorbent and electrode material, kaganeite (β-FeOOH) one receives much concern always.β-FeOOH
The hydrated ferric oxide. of a kind of chloride hollandite type structure, have high-specific surface area and small duct [J. Phys. Chem. C,
2012,116 (3), 2303-2312], there is the advantage such as high adsorption capacity, inexpensive, environmental protection, therefore can urge as molybdenum
The ideal carrier of agent.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of molybdenum doping kaganeite nanoparticle.
Based on above-mentioned purpose, the present invention by the following technical solutions:
The preparation method of a kind of molybdenum doping kaganeite nanoparticle, adds to ammonium molybdate aqueous solution in molysite aqueous solution,
At a temperature of 180-200 DEG C react more than 24h, reactant liquor by centrifugation, washing, i.e. obtain molybdenum doping kaganeite nanometer after drying
Microgranule；Wherein ammonium molybdate and iron salt mol ratio are 1:(20-50), described iron salt is ferric chloride or ferrous sulfate.
Described ammonium molybdate is one or both combination in ammonium dimolybdate and ammonium heptamolybdate.
This preparation method has technique, equipment is simple, cheaper starting materials is easy to get, low cost, productivity high, is suitable for big rule
The commercial production of mould, obtained molybdenum doping kaganeite nanoparticle yardstick is little, homogeneous grain diameter, molybdenum are uniformly dispersed, as
The catalyst of thick oil hydrothermal catalytic viscosity reduction can obtain ideal effect.
Accompanying drawing explanation
Fig. 1 is powder x-ray diffraction (XRD) collection of illustrative plates of embodiment 1 product；
Fig. 2 is the infrared spectrum of embodiment 1 product；
Fig. 3 is transmission electron microscope (TEM) photo of embodiment 1 product；
Fig. 4 is the x-ray photoelectron spectroscopy (Mo 3 of embodiment 1 productdXPS spectrum)；
Fig. 5 is embodiment 1 product catalytic viscosity reduction result figure to the viscous crude of Shengli Oil Field.
Detailed description of the invention
With specific embodiment, technical scheme is described below, but protection scope of the present invention is not limited to this.
Embodiment 1
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
0.112 g(0.090mmol is added in 100mL beaker) ammonium heptamolybdate, it is subsequently adding 25mL distilled water, stirs under room temperature
20min is allowed to be completely dissolved, and is denoted as solution A；Another addition 0.61g (2.25mmol) ferric chloride (FeCl36H2O) in 200mL beaker, adds
Entering 75mL distilled water, stirring 10min is allowed to be completely dissolved, and is denoted as solution B；Use pipette, extract solution A, be slowly dropped to solution
In B, stir 25min, obtain brown color clear solution C, then solution C is transferred in 200mL hydrothermal reaction kettle, at 180 DEG C
Reaction 24h, after reaction terminates, naturally cools to room temperature, centrifugal, centrifugal gained precipitation distilled water wash 5 times, and in an oven 80
DEG C be dried 12 hours, obtain 0.30g brown solid powder.
Fig. 1 is the XRD figure spectrum of embodiment 1 product, in figure 11.89,17.02,26.97,34.35,35.32,
Diffraction maximum at 39.48,43.33,44.50,46.86,52.63,56.48,61.45,65.14,68.42 with
The standard card (JCPDS card number, 13-0157) of kaganeite (β-FeO (OH)) matches, the most corresponding positive policy ferrum
Feature diffraction crystal face (110) in ore deposit, (200), (310), (400), (211), (301), (321), (510), (411), (600),
(521), (002), (541), (312).As seen from Figure 1, XRD result shows that prepared product agent structure is positive policy ferrum
, there is not the diffraction maximum of raw material in ore deposit.
Fig. 2 is the infrared spectrum of embodiment 1 product, wave number (cm-1) at 1626,1397,841,807, occur that 4 peaks are
The absworption peak of typical kaganeite (β-FeO (OH))；The strong peak occurred at 715 is Mo O vibration absorption peak, at 671 is
The absworption peak of hexa-coordinate Mo (O)；916, the out-of-plane bending vibration that 2 peaks are O H at 465.Do not find MoO3Absorption vibration
Peak, illustrates that molybdenum atom enters kaganeite lattice, forms molybdenum doping kaganeite.
Fig. 3 is the TEM photo of embodiment 1 product, it can be seen that prepared molybdenum doping kaganeite nanoparticle grain
Footpath is uniform, and mean diameter is about 40nm.
Fig. 4 is the Mo 3 of embodiment 1 productdXPS spectrum.Mo 3 on productd 3/2With Mo 3d 5/2Combination can be respectively
235.5eV and 232.4eV, shows that Mo ion is with Mo6+It is present in its surface.
Fig. 5 is the catalytic viscosity reduction effect to the super-viscous oil of Shengli Oil Field of embodiment 1 product.Super-viscous oil is from China's Shengli Oil
Field, recording viscosity at 50 DEG C is 155657 mPa s.Course of reaction is as follows: by 50 grams of viscous crude, 0.1 gram of catalyst (i.e. embodiment 1
The product prepared) and 1.5 mL tetrahydronaphthalenes (as hydrogen donor) join in 200 mL reactors, at 200 DEG C, reaction is 24 little
Time, take out after being cooled to room temperature.Then gluing at Brookfield DV-III type viscometer able to programme its 50 DEG C is utilized
Angle value.Viscosity break ratio () it is defined as follows:
,
Here、WithAfter representing the front viscosity number of viscosity break ratio, reaction and reaction respectively, viscosity number (is at 50 DEG C survey
Fixed).
As shown in Fig. 5 No. 4, under this catalyst and hydrogen donor effect, thick oil viscosity from reaction before 155657
Pa s (50 C) drops to 47831 Pa s, viscosity break ratio=69.3%。
Contrast and experiment: i.e. under same experiment condition, is not added with catalyst and hydrogen donor, and the viscosity break ratio of this viscous crude is
12.1%(Fig. 5, No. 1)；Only adding catalyst, viscosity break ratio is 19.3%(Fig. 5, No. 2)；Only adding hydrogen donor, viscosity break ratio is 62.5%(figure
5, No. 3).Therefore, add only 0.2%(mass percent) catalyst make the viscosity break ratio of this viscous crude carry with compared with during catalyst
High by 37.3%；It is simultaneously introduced catalyst and hydrogen donor, viscosity break ratio can be made to improve 82.5%, demonstrate good catalysis potential.
Embodiment 2
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
In 100mL beaker, add 0.056 g (0.045mmol) ammonium heptamolybdate, be subsequently adding under 25mL distilled water, room temperature and stir
Mix 20min to be allowed to be completely dissolved, be denoted as solution A；Another addition 0.61g (2.25mmol) ferric chloride (FeCl36H2O) in 200mL beaker,
Being subsequently adding 75mL distilled water, stirring 10min is allowed to be completely dissolved, and is denoted as solution B；Use pipette, extract solution A, be slowly added dropwise
In solution B, stir 25min, obtain brown color clear solution C, then solution C is transferred in 200mL hydrothermal reaction kettle,
React after 24h at 180 DEG C, naturally cool to room temperature, centrifugal, precipitation distilled water wash 5 times, in an oven 80 DEG C to be dried 12 little
Time, obtain 0.28g brown solid powder.
Embodiment 3
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
In 100mL beaker, add 0.070 g (0.056mmol) ammonium heptamolybdate, be subsequently adding under 25mL distilled water, room temperature and stir
Mix 20min to be allowed to be completely dissolved, be denoted as solution A；Another addition 0.61g (2.25mmol) ferric chloride (FeCl36H2O) in 200mL beaker,
Being subsequently adding 75mL distilled water, stirring 10min is allowed to be completely dissolved, and is denoted as solution B；Use pipette, extract solution A, be slowly added dropwise
In solution B, stir 25min, obtain brown color clear solution C, then solution C is transferred in 200mL hydrothermal reaction kettle,
React after 24h at 200 DEG C, naturally cool to room temperature, centrifugal, precipitation distilled water wash 5 times, in an oven 80 DEG C to be dried 12 little
Time, obtain 0.29g brown solid powder.
Embodiment 4
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
In 100mL beaker, add 0.015 g (0.045mmol) ammonium dimolybdate, be subsequently adding under 25mL distilled water, room temperature and stir
Mix 20min to be allowed to be completely dissolved, be denoted as solution A；Another addition 0.61g (2.25mmol) ferric chloride (FeCl36H2O) in 200mL beaker,
Being subsequently adding 75mL distilled water, stirring 10min is allowed to be completely dissolved, and is denoted as solution B；Use pipette, extract solution A, be slowly added dropwise
In solution B, stir 25min, obtain brown color clear solution C, then solution C is transferred in 200mL hydrothermal reaction kettle,
React after 48h at 180 DEG C, naturally cool to room temperature, centrifugal, precipitation distilled water wash 5 times, in an oven 80 DEG C to be dried 12 little
Time, obtain 0.28g brown solid powder.
Embodiment 5
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
In 100mL beaker, add 0.030 g (0.09mmol) ammonium dimolybdate, be subsequently adding 25mL distilled water, stir under room temperature
20min is allowed to be completely dissolved, and is denoted as solution A；Another 0.61g (2.25mmol) ferric chloride (FeCl36H2O) that adds in 200mL beaker, so
Rear addition 75mL distilled water, stirring 10min is allowed to be completely dissolved, and is denoted as solution B；Use pipette, extract solution A, be slowly dropped to
In solution B, stir 25min, obtain brown color clear solution C, then solution C is transferred in 200mL hydrothermal reaction kettle, 200
After reacting 24h at DEG C, naturally cooling to room temperature, centrifugal, precipitation uses distilled water wash 5 times, and 80 DEG C are dried 12 hours in an oven,
Obtain 0.30g brown solid powder.
Embodiment 6
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
In 100mL beaker, add 0.019 g (0.056mmol) ammonium dimolybdate, be subsequently adding under 25mL distilled water, room temperature and stir
Mix 20min to be allowed to be completely dissolved, be denoted as solution A；Another addition 0.61g (2.25mmol) ferric chloride (FeCl36H2O) in 200mL beaker,
Being subsequently adding 75mL distilled water, stirring 10min is allowed to be completely dissolved, and is denoted as solution B；Use pipette, extract solution A, be slowly added dropwise
In solution B, stir 25min, obtain brown color clear solution C, then solution C is transferred in 200mL hydrothermal reaction kettle,
React after 36h at 190 DEG C, naturally cool to room temperature, centrifugal, precipitation distilled water wash 5 times, in an oven 80 DEG C to be dried 12 little
Time, obtain 0.29g brown solid powder.
Embodiment 7
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
0.015 g (0.045mmol) ammonium dimolybdate and 0.056g (0.045mmol) ammonium heptamolybdate is added in 100mL beaker,
It is subsequently adding 25mL distilled water, stirs 20min under room temperature and be allowed to be completely dissolved, be denoted as solution A；Another addition in 200mL beaker
0.61g (2.25mmol) ferric chloride (FeCl36H2O), is subsequently adding 75mL distilled water, and stirring 10min is allowed to be completely dissolved, and is denoted as solution
B；Use pipette, extract solution A, be slowly dropped in solution B, stir 25min, obtain brown color clear solution C, then by molten
Liquid C is transferred in 200mL hydrothermal reaction kettle, after reacting 24h, naturally cools to room temperature at 200 DEG C, centrifugal, precipitation distilled water
Washing 5 times, 80 DEG C are dried 12 hours in an oven, obtain 0.30g brown solid powder.
Embodiment 8
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
In 100mL beaker, add 0.112g (0.09mmol) ammonium heptamolybdate, be subsequently adding 25mL distilled water, stir under room temperature
20min is allowed to be completely dissolved, and is denoted as solution A；Another addition 0.63g (2.25mmol) ferrous sulfate in 200mL beaker, then adds
Entering 75mL distilled water, stirring 10min is allowed to be completely dissolved, and is denoted as solution B；Use pipette, extract solution A, be slowly dropped to solution
In B, stir 25min, obtain brown color clear solution C, then solution C is transferred in 200mL hydrothermal reaction kettle, at 180 DEG C
After reaction 24h, naturally cooling to room temperature, centrifugal, precipitation uses distilled water wash 5 times, and 80 DEG C are dried 12 hours in an oven,
0.30g brown solid powder.
Embodiment 9
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
In 100mL beaker, add 0.030g (0.09mmol) ammonium dimolybdate, be subsequently adding 25mL distilled water, stir under room temperature
20min is allowed to be completely dissolved, and is denoted as solution A；Another addition 0.63g (2.25mmol) ferrous sulfate in 200mL beaker, then adds
Entering 75mL distilled water, stirring 10min is allowed to be completely dissolved, and is denoted as solution B；Use pipette, extract solution A, be slowly dropped to solution
In B, stir 25min, obtain brown color clear solution C, then solution C is transferred in 200mL hydrothermal reaction kettle, at 200 DEG C
After reaction 24h, naturally cooling to room temperature, centrifugal, precipitation uses distilled water wash 5 times, and 80 DEG C are dried 12 hours in an oven,
0.29g brown solid powder.
Embodiment 10
A kind of preparation method of molybdenum doping kaganeite nanoparticle, preparation process is as follows:
0.019 g (0.056mmol) ammonium dimolybdate and 0.056g (0.045mmol) ammonium heptamolybdate is added in 100mL beaker,
It is subsequently adding 25mL distilled water, stirs 20min under room temperature and be allowed to be completely dissolved, be denoted as solution A；Another addition in 200mL beaker
0.63g (2.25mmol) ferrous sulfate, is subsequently adding 75mL distilled water, and stirring 10min is allowed to be completely dissolved, and is denoted as solution B；With
Pipette, extract solution A, is slowly dropped in solution B, stirs 25min, obtains brown color clear solution C, then solution C turned
Move in 200mL hydrothermal reaction kettle, after reacting 36h at 190 DEG C, naturally cool to room temperature, centrifugal, precipitation distilled water wash 5
Secondary, 80 DEG C are dried 12 hours in an oven, obtain 0.28g brown solid powder.
Claims (2)
1. the preparation method of a molybdenum doping kaganeite nanoparticle, it is characterised in that: ammonium molybdate aqueous solution is added to ferrum
In saline solution, at a temperature of 180-200 DEG C react more than 24h, reactant liquor by centrifugation, washing, i.e. obtain molybdenum doping after drying
Kaganeite nanoparticle；Wherein ammonium molybdate and iron salt mol ratio are 1:(20-50), described iron salt is ferric chloride or sulphuric acid
Ferrous.
2. the preparation method of molybdenum doping kaganeite nanoparticle as claimed in claim 1, it is characterised in that: described molybdic acid
Ammonium is one or both combination in ammonium dimolybdate and ammonium heptamolybdate.
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| CN114574265A (en) * | 2022-05-05 | 2022-06-03 | 新乡市瑞丰新材料股份有限公司 | Molybdenum sulfonate compound and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10510524A (en) * | 1994-12-14 | 1998-10-13 | シエル・インターナシヨネイル・リサーチ・マーチヤツピイ・ベー・ウイ | Large particle dehydrogenation catalyst and method |
| JP2013240789A (en) * | 2007-05-03 | 2013-12-05 | Basf Corp | Catalyst, its preparation and use |
| CN104785272A (en) * | 2015-04-20 | 2015-07-22 | 神华集团有限责任公司 | Iron-based catalyst and preparation method thereof |
| CN104826662A (en) * | 2015-05-06 | 2015-08-12 | 北京中科诚毅科技发展有限公司 | Iron catalyst for slurry reactor hydrogenation, preparation, design method, and applications thereof |
| CN104888797A (en) * | 2015-06-10 | 2015-09-09 | 神华集团有限责任公司 | Iron-based catalyst and preparation method thereof |
-
2016
- 2016-06-15 CN CN201610418162.6A patent/CN106000413B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10510524A (en) * | 1994-12-14 | 1998-10-13 | シエル・インターナシヨネイル・リサーチ・マーチヤツピイ・ベー・ウイ | Large particle dehydrogenation catalyst and method |
| JP2013240789A (en) * | 2007-05-03 | 2013-12-05 | Basf Corp | Catalyst, its preparation and use |
| CN104785272A (en) * | 2015-04-20 | 2015-07-22 | 神华集团有限责任公司 | Iron-based catalyst and preparation method thereof |
| CN104826662A (en) * | 2015-05-06 | 2015-08-12 | 北京中科诚毅科技发展有限公司 | Iron catalyst for slurry reactor hydrogenation, preparation, design method, and applications thereof |
| CN104888797A (en) * | 2015-06-10 | 2015-09-09 | 神华集团有限责任公司 | Iron-based catalyst and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114574265A (en) * | 2022-05-05 | 2022-06-03 | 新乡市瑞丰新材料股份有限公司 | Molybdenum sulfonate compound and preparation method and application thereof |
| CN114574265B (en) * | 2022-05-05 | 2022-08-12 | 新乡市瑞丰新材料股份有限公司 | Molybdenum sulfonate compound and preparation method and application thereof |
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