CN117843046A - Preparation method of high-purity nano nickel oxide - Google Patents
Preparation method of high-purity nano nickel oxide Download PDFInfo
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- CN117843046A CN117843046A CN202410013216.5A CN202410013216A CN117843046A CN 117843046 A CN117843046 A CN 117843046A CN 202410013216 A CN202410013216 A CN 202410013216A CN 117843046 A CN117843046 A CN 117843046A
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- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 91
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 26
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- 230000032683 aging Effects 0.000 claims abstract description 18
- 150000002815 nickel Chemical class 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000012065 filter cake Substances 0.000 claims abstract description 13
- 239000012266 salt solution Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- -1 polyoxyethylene Polymers 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- VQBIMXHWYSRDLF-UHFFFAOYSA-M sodium;azane;hydrogen carbonate Chemical compound [NH4+].[Na+].[O-]C([O-])=O VQBIMXHWYSRDLF-UHFFFAOYSA-M 0.000 claims description 2
- GGHPAKFFUZUEKL-UHFFFAOYSA-M sodium;hexadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCOS([O-])(=O)=O GGHPAKFFUZUEKL-UHFFFAOYSA-M 0.000 claims description 2
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims description 2
- 238000001914 filtration Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 6
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of high-purity nano nickel oxide. The method comprises the steps of obtaining nano nickel oxide precursor slurry by utilizing a nickel salt solution and a precipitant solution through a multiphase interface reactor under the action of a surfactant; aging the nano nickel oxide precursor slurry, filtering and washing to obtain a nano nickel oxide precursor filter cake, drying the filter cake in a drying oven, and roasting in a muffle furnace to obtain the nano nickel oxide with the average particle size of 50-100 nm. The nano nickel oxide prepared by the method is simple in preparation method, easy to apply in industrialization, uniform in particle size of the prepared product and better in comprehensive performance.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of nano nickel oxide, in particular to a preparation method of high-purity nano nickel oxide.
Background
The nano material is a material with granularity controlled between 1 and 100nm, has characteristics different from atoms and crystals, and has physical and chemical characteristics which are not possessed by a plurality of bulk materials. Nickel oxide is a typical P-type semiconductor, has good heat-sensitive and gas-sensitive properties, is a very promising functional material, and is widely applied to industries such as metallurgy, chemistry, electronics and the like.
Nickel oxide is an oxidation catalyst with good catalytic performance. Ni (Ni) 2+ The catalyst has 3d orbit, has preferential adsorption tendency to multi-electron oxygen, has activation effect to other reducing gases and has catalysis effect to oxidation of the reducing gases. The nano nickel oxide has great attention in the field of catalysis because of its large surface area, short intracrystalline diffusion channel, rich active sites, high surface atomic ratio and surface energy, and much higher activity and selectivity than the traditional catalyst. In recent years, renewable energy sources such as biomass are developed and utilized through thermal decomposition technology, fossil raw materials are replaced to a certain extent, nickel oxide is used as a catalyst with excellent cost performance, and the yield and efficiency of biomass gasification and pyrolysis can be improved. The preparation method of nickel oxide mainly includes solid phase method, liquid phase method and gas phase method. The solid phase method has the advantages of low cost, high yield, easy control of reaction conditions, and the like, but has the defects of high energy consumption, low efficiency, large product particle size, easy oxidative deformation and agglomeration of particles, and the like. The liquid phase method for preparing the nano nickel oxide has the characteristics of easy preparation in nucleation and growth processes, high cost, non-uniform particle size and the like. The gas phase method has the characteristics of high yield, high productivity, difficult shape control and the like.
The superfine particle size of the nano nickel oxide changes the surface structure and the crystal structure, so that the surface effect, the small-size effect, the quantum size effect, the macroscopic quantum tunneling effect and the like are generated, and the nano nickel oxide has excellent catalytic performance and electrical performance. Therefore, the preparation and application research of nano nickel oxide has become one of the important research subjects in the field of material science.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity nano nickel oxide, and the prepared sample has the particle size reaching the nano size, and the product has good batch stability and excellent performance.
In order to achieve the above purpose, the preparation method of the high-purity nano nickel oxide provided by the invention comprises the following steps:
(1) The nickel salt solution, the precipitant solution and the surfactant solution are input into a multiphase interface reactor in parallel flow, the reaction is carried out at normal temperature and normal pressure under the stirring state, the nano nickel oxide precursor slurry is obtained through overflow of a discharge port, the flow rate of the materials input into the multiphase interface reactor is set to be 100-500ml/min, the rotating speed is set to be 1000-5000r/min, the concentration of the nickel salt solution is 0.5mol/L-2mol/L, the equivalent concentration ratio of the precipitant solution to the nickel salt solution is 1.1-2.0, and the amount of the surfactant substance is 0.02% -1.0% of the amount of the nickel ion substance;
(2) Aging the nano nickel oxide precursor slurry obtained in the step (1) at the temperature of 20-65 ℃ for 1-6 hours to obtain the nano nickel oxide precursor aged slurry;
(3) Centrifuging and washing the aged slurry of the nano nickel oxide precursor obtained in the step (2) to obtain a nano nickel oxide precursor filter cake;
(4) Drying the nano nickel oxide precursor filter cake obtained in the step (3) at the temperature of 60-100 ℃ for 8-24 hours to obtain a nano nickel oxide precursor;
(5) Roasting and grinding the nano nickel oxide precursor obtained in the step (4), wherein the roasting temperature is 400-800 ℃, and the roasting time is 2-4 hours, so that the nano nickel oxide with the average particle size of 50-100 nm is obtained.
The nickel salt solution in the step (1) is prepared from nickel salt, wherein the nickel salt is one or a combination of a plurality of nickel sulfate, nickel nitrate or nickel chloride.
The precipitant in the step (1) is one or a combination of more of sodium hydroxide, ammonia water, sodium carbonate and ammonium bicarbonate.
The surfactant solution in the step (1) is one or a combination of more of sodium oleate, sodium dodecyl sulfate, sodium hexadecyl sulfate, sodium octadecyl sulfate, sodium dodecyl benzene sulfonate, tween 80 and alkylphenol polyoxyethylene.
The ageing temperature in the step (2) is 20-65 ℃ and the ageing time is 2-4 h.
And (3) drying in the step (4) at 80 ℃ for 12 hours.
And (3) roasting at 600 ℃ for 3 hours in the step (5).
The preparation method of the high-purity nano nickel oxide has the beneficial effects that: the method comprises the steps of obtaining nano nickel oxide precursor slurry by utilizing a nickel salt solution and a precipitant solution through a multiphase interface reactor under the action of a surfactant; aging the nano nickel oxide precursor slurry, filtering and washing to obtain a nano nickel oxide precursor filter cake, and placing the filter cake in a baking oven for baking, and roasting in a muffle furnace to obtain the nano nickel oxide with the average particle size of 50-100 nm. The nano nickel oxide prepared by the invention has the advantages of simple preparation method, easy industrialization application, uniform particle diameter of the nano nickel oxide, excellent comprehensive performance and specific surface area 63.045 m 2 The purity (calculated by nickel oxide) of the nano nickel oxide prepared by the invention reaches 97.0 percent.
Drawings
FIG. 1 is an SEM photograph of a sample of example 2;
fig. 2 shows XRD detection results of the sample of example 2.
Detailed Description
Example 1
The invention relates to a preparation method of high-purity nano nickel oxide, which comprises the following steps:
(1) Preparing a nickel salt solution with the concentration of 0.8mol/L, a precipitator solution and a surfactant solution, wherein the equivalent concentration ratio of the precipitator solution to the nickel salt solution is 1:1, adding 0.02% of the amount of a surfactant substance into a multiphase interface reactor in parallel flow, reacting at normal temperature and normal pressure under a stirring state, and overflowing through a discharge hole to obtain nano nickel oxide precursor slurry, wherein the flow of the material input into the multiphase interface reactor is set to be 100ml/min, and the rotating speed is set to be 1000r/min;
(2) Aging the nano nickel oxide precursor slurry obtained in the step (1) to obtain a nano nickel oxide precursor aging slurry; wherein the aging temperature is 20 ℃ and the aging time is 2 hours;
(3) Centrifuging and washing the aged slurry of the nano nickel oxide precursor obtained in the step (2) to obtain a nano nickel oxide precursor filter cake;
(4) Drying the nano nickel oxide precursor filter cake obtained in the step (3) to obtain a nano nickel oxide precursor; wherein the drying temperature is 65 ℃ and the drying time is 9 hours;
(5) Roasting the nano nickel oxide precursor obtained in the step (4) at the temperature of 500 ℃ for 3.5 hours to obtain the nano nickel oxide with the average particle size of 50-100 nm.
Example 2
The invention relates to a preparation method of high-purity nano nickel oxide, which comprises the following steps:
(1) Preparing 1L of nickel chloride solution with the concentration of 1.0mol/L, 1L of sodium carbonate solution with the concentration of 1.1mol/L and 1L of sodium oleate solution with the concentration of 0.005mol/L, and adding three-phase solution into a multiphase interface reactor in parallel to react, wherein the flow rate of the material input into the multiphase interface reactor is set to 400ml/min, and the rotating speed is set to 4000r/min;
(2) Aging the nano nickel oxide precursor slurry obtained in the step (1), wherein the aging conditions are as follows: the temperature is 25 ℃ and the time is 3 hours, and the nano nickel oxide aged slurry is obtained;
(3) Centrifugally filtering, washing and washing the nano nickel oxide aged slurry obtained in the step (2) until no chloride ions exist (no precipitate exists in qualitative detection of silver nitrate solution);
(4) Drying the nano nickel oxide precursor filter cake obtained in the step (3), wherein the drying conditions are as follows: obtaining a nano nickel oxide precursor at 80 ℃ for 12 hours;
(5) Roasting the nano nickel oxide precursor obtained in the step (3),the roasting conditions are as follows: at 600deg.C for 3 hr to obtain nano nickel oxide with average particle diameter of 50-100 nm, as shown in SEM picture of sample in figure 1, XRD detection result of sample in figure 2 shows that specific surface area is 63.045 m 2 Per g, and the purity of the obtained nano nickel oxide (calculated as nickel oxide) is 97.0%.
Example 3
The invention relates to a preparation method of high-purity nano nickel oxide, which comprises the following steps:
(1) Preparing 1.0mol/L nickel chloride solution 1L, 1.1mol/L ammonium bicarbonate solution 1L and 0.005mol/L sodium dodecyl sulfate solution 1L, adding three-phase solution into a multiphase interface reactor in parallel flow mode for reaction, wherein the flow rate of the material input into the multiphase interface reactor is set to 400ml/min, and the rotating speed is set to 4000r/min;
(2) Aging the nano nickel oxide precursor slurry obtained in the step (1), wherein the aging conditions are as follows: the temperature is 25 ℃ and the time is 3 hours, and the nano nickel oxide aged slurry is obtained;
(3) Centrifugally filtering, washing and washing the nano nickel oxide aged slurry obtained in the step (2) until no chloride ions exist (no precipitate exists in qualitative detection of silver nitrate solution);
(4) Drying the nano nickel oxide precursor filter cake obtained in the step (3), wherein the drying conditions are as follows: obtaining a nano nickel oxide precursor at 80 ℃ for 12 hours;
(5) Roasting the nano nickel oxide precursor obtained in the step (3), wherein the roasting conditions are as follows: 600 ℃ for 3 hours to obtain the nano nickel oxide with the average particle diameter of 50nm-100 nm.
Example 4
The invention relates to a preparation method of high-purity nano nickel oxide, which comprises the following steps:
(1) Preparing 1L of nickel sulfate solution with the concentration of 1.0mol/L, 1L of sodium hydroxide with the concentration of 1.1mol/L and 1L of sodium oleate with the concentration of 0.005mol/L, adding three-phase solution into a multiphase interface reactor in parallel to react, wherein the flow rate of the material input into the multiphase interface reactor is set to 400ml/min, and the rotating speed is set to 4000r/min;
(2) Aging the nano nickel oxide precursor slurry obtained in the step (1), wherein the aging conditions are as follows: the temperature is 25 ℃ and the time is 3 hours, and the nano nickel oxide aged slurry is obtained;
(3) Centrifugally filtering, washing and washing the nano nickel oxide aged slurry obtained in the step (2) until no chloride ions exist (no precipitate exists in qualitative detection of silver nitrate solution);
(4) Drying the nano nickel oxide precursor filter cake obtained in the step (3), wherein the drying conditions are as follows: obtaining a nano nickel oxide precursor at 80 ℃ for 12 hours;
(5) Roasting the nano nickel oxide precursor obtained in the step (3), wherein the roasting conditions are as follows: the nano nickel oxide with the average grain diameter of 50nm-100nm is obtained after 3 hours at 700 ℃.
Claims (7)
1. A preparation method of high-purity nano nickel oxide is characterized in that: the method comprises the following steps:
(1) The nickel salt solution, the precipitant solution and the surfactant solution are input into a multiphase interface reactor in parallel flow, the reaction is carried out at normal temperature and normal pressure under the stirring state, the nano nickel oxide precursor slurry is obtained through overflow of a discharge port, the flow rate of the materials input into the multiphase interface reactor is set to be 100-500ml/min, the rotating speed is set to be 1000-5000r/min, the concentration of the nickel salt solution is 0.5mol/L-2mol/L, the equivalent concentration ratio of the precipitant solution to the nickel salt solution is 1.1-2.0, and the amount of the surfactant substance is 0.02% -1.0% of the amount of the nickel ion substance;
(2) Aging the nano nickel oxide precursor slurry obtained in the step (1) at the temperature of 20-65 ℃ for 1-6 hours to obtain the nano nickel oxide precursor aged slurry;
(3) Centrifuging and washing the aged slurry of the nano nickel oxide precursor obtained in the step (2) to obtain a nano nickel oxide precursor filter cake;
(4) Drying the nano nickel oxide precursor filter cake obtained in the step (3) at the temperature of 60-100 ℃ for 8-24 hours to obtain a nano nickel oxide precursor;
(5) Roasting and grinding the nano nickel oxide precursor obtained in the step (4), wherein the roasting temperature is 400-800 ℃, and the roasting time is 2-4 hours, so that the nano nickel oxide with the average particle size of 50-100 nm is obtained.
2. The method for preparing high-purity nano nickel oxide according to claim 1, wherein the method comprises the following steps: the nickel salt solution in the step (1) is prepared from nickel salt, wherein the nickel salt is one or a combination of a plurality of nickel sulfate, nickel nitrate or nickel chloride.
3. The method for preparing high-purity nano nickel oxide according to claim 1, wherein the method comprises the following steps: the precipitant in the step (1) is one or a combination of more of sodium hydroxide, ammonia water, sodium carbonate and ammonium bicarbonate.
4. The method for preparing high-purity nano nickel oxide according to claim 1, wherein the method comprises the following steps: the surfactant solution in the step (1) is one or a combination of more of sodium oleate, sodium dodecyl sulfate, sodium hexadecyl sulfate, sodium octadecyl sulfate, sodium dodecyl benzene sulfonate, tween 80 and alkylphenol polyoxyethylene.
5. The method for preparing high-purity nano nickel oxide according to claim 1, wherein the method comprises the following steps: the ageing temperature in the step (2) is 20-65 ℃ and the ageing time is 2-4 h.
6. The method for preparing high-purity nano nickel oxide according to claim 1, wherein the method comprises the following steps: and (3) drying in the step (4) at 80 ℃ for 12 hours.
7. The method for preparing high-purity nano nickel oxide according to claim 1, wherein the method comprises the following steps: and (3) roasting at 600 ℃ for 3 hours in the step (5).
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177305A (en) * | 2007-11-14 | 2008-05-14 | 四川大学 | Method for preparing high specific surface area meso-porous nickelous oxide |
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| JP2018024550A (en) * | 2016-08-10 | 2018-02-15 | 住友金属鉱山株式会社 | Nickel oxide fine powder and production method of the same |
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-
2024
- 2024-01-04 CN CN202410013216.5A patent/CN117843046A/en active Pending
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|---|
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