CN115650320A - Preparation method of nano nickel sulfide - Google Patents
Preparation method of nano nickel sulfide Download PDFInfo
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- CN115650320A CN115650320A CN202211325409.1A CN202211325409A CN115650320A CN 115650320 A CN115650320 A CN 115650320A CN 202211325409 A CN202211325409 A CN 202211325409A CN 115650320 A CN115650320 A CN 115650320A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 238000002360 preparation method Methods 0.000 title abstract description 19
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 63
- 239000011593 sulfur Substances 0.000 claims abstract description 63
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 56
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 48
- 239000000839 emulsion Substances 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000004094 surface-active agent Substances 0.000 claims abstract description 33
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 28
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 22
- 239000002101 nanobubble Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims description 110
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- 239000000047 product Substances 0.000 claims description 26
- 238000001914 filtration Methods 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 24
- 239000002244 precipitate Substances 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- 239000003960 organic solvent Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 230000005587 bubbling Effects 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 11
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 claims description 8
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 239000005416 organic matter Substances 0.000 claims description 6
- -1 polyoxyethylene lauryl ether Polymers 0.000 claims description 5
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 claims description 5
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- ODJQKYXPKWQWNK-UHFFFAOYSA-N 3,3'-Thiobispropanoic acid Chemical compound OC(=O)CCSCCC(O)=O ODJQKYXPKWQWNK-UHFFFAOYSA-N 0.000 claims description 4
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- 239000003490 Thiodipropionic acid Substances 0.000 claims description 4
- JMGZBMRVDHKMKB-UHFFFAOYSA-L disodium;2-sulfobutanedioate Chemical compound [Na+].[Na+].OS(=O)(=O)C(C([O-])=O)CC([O-])=O JMGZBMRVDHKMKB-UHFFFAOYSA-L 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims description 4
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- 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 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 235000019303 thiodipropionic acid Nutrition 0.000 claims description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 3
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 3
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 3
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011859 microparticle Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 16
- 239000001257 hydrogen Substances 0.000 abstract description 16
- 239000004005 microsphere Substances 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 6
- 238000004945 emulsification Methods 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 3
- 238000003860 storage Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- MVPPADPHJFYWMZ-IDEBNGHGSA-N chlorobenzene Chemical group Cl[13C]1=[13CH][13CH]=[13CH][13CH]=[13CH]1 MVPPADPHJFYWMZ-IDEBNGHGSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the technical field of hydrogen energy, in particular to a preparation method of nano nickel sulfide. The preparation method of the nano nickel sulfide comprises the following steps: s1, preparing a microemulsion solution of an active sulfur-nickel-containing component; s2, preparing a particle emulsion solution; s3, carrying out a hydrothermal reaction; and S4, ultrasonic cleaning. The invention has reasonable design and simple and convenient operation, the polar component is added into the nonpolar solution (surfactant), under the action of the nano bubble generator, the nonpolar component forms a large amount of fine microspheres in the polar component under the emulsification action of the surfactant, and the nickel-containing component and the sulfur-containing component are wrapped in the polar component to be used as a micro reaction unit, and in a hydrothermal reaction kettle, the high-temperature and high-pressure environment can promote the reaction of sulfur and nickel in the micro reaction unit and finally destroy the microspheres; strong acid is generated in the reaction process, nickel sulfide is re-dissolved, and excessive strong acid is reacted by solid hydroxide, so that the reaction is normally carried out.
Description
Technical Field
The invention relates to the technical field of hydrogen energy, in particular to a preparation method of nano nickel sulfide.
Background
The underground storage of hydrogen is continuously explored and researched by various countries, artificial gas prepared by mixing 50-60% of hydrogen and methane is injected into an underground storage in the early stage, and the underground storage of pure hydrogen (95% of hydrogen and 3-4% of carbon dioxide) is also developed in the later stage, wherein the research and practice of the underground storage of hydrogen in European and American countries such as France, germany, britain, united states and the like are more, and the research of China in the aspect is relatively less. At present, in order to deal with the energy crisis, energy strategic reserve strategies are actively implemented by all countries, an underground salt cavern reserve bank is the most important ring in energy strategic reserve work, and a salt rock underground reserve bank has the advantages of large storage capacity, high peak regulation speed, safety, economy and the like, is an internationally recognized underground storage place with the best strategic energy sources such as natural gas, petroleum and the like, and in recent years, the construction of an underground salt cavern hydrogen storage system is rapidly developed in China, so that the underground salt cavern hydrogen storage system has very important guiding significance for the storage and application of hydrogen in the future of China.
Because the amount of hydrogen used in the salt cavern hydrogen storage is very large, a hydrogen production method which can produce hydrogen in large scale and has low price is needed. In the prior art, hydrogen is produced by hydrolysis, and an electrode in a hydrogen production system plays an important role. The existing electrode has high content of noble metal and high cost, so the electrode with low power consumption and strong stability needs to be developed.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects in the prior art and provides a preparation method of nano nickel sulfide.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 190-220 ℃, and the reaction time is 18-20 h;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing by water; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
Further, in the S1, the molar ratio of the sulfur-containing component to the nickel source is 1: a, B is less than or equal to 3.
Further, the volume ratio of the microemulsion solution of the active sulfur-containing nickel component in the S2 to the polar component is 1.
Further, 1g of solid sodium hydroxide was added to each 50ml of the microparticle emulsion solution in the S3.
Further, the sulfur-containing component in the S1 is a sulfur-containing carbon oxygen organic matter capable of decomposing to generate hydrogen sulfide gas; the nickel source is one or more of nickel sulfate, nickel chloride, nickel sulfamate, nickel bromide and nickel nitrate; the surfactant is a high temperature stable surfactant.
Further, the polar component in the S2 is a high-boiling polar organic matter.
Further, the sulfur-containing component is one or more of thioacetamide, thioacetic acid and thiodipropionic acid.
Further, the surfactant is one or more of polyoxyethylene lauryl ether, fatty alcohol polyoxyethylene ether, disodium sulfosuccinate monoester and sodium dodecyl benzene sulfonate.
Further, the polar component is one or more of toluene, p-xylene, n-heptane, chlorobenzene, o-dichlorobenzene and isooctane.
Further, the organic solvent in S4 is one or more of ethanol, acetone, ethyl acetate, n-hexane, and dichloromethane.
The invention has the beneficial effects that: the invention has reasonable design and simple and convenient operation, polar components are added into a nonpolar solution (surfactant), under the action of a nano bubble generator, the nonpolar components form a large amount of fine microspheres in the polar components under the emulsification action of the surfactant, and a nickel-containing component and a sulfur-containing component are wrapped in the polar components to be used as a tiny reaction unit, and in a hydrothermal reaction kettle, the sulfur and nickel in the tiny reaction unit are promoted to react and finally destroy the microspheres under the high-temperature and high-pressure environment; strong acid is generated in the reaction process, nickel sulfide is re-dissolved, and excessive strong acid is reacted by solid hydroxide, so that the reaction is normally carried out.
Drawings
The invention is further illustrated by the following examples in conjunction with the drawings.
FIG. 1 is a particle size distribution diagram of nano nickel sulfide prepared in example 1;
FIG. 2 is a particle size distribution diagram of nano nickel sulfide prepared in comparative example 3;
FIG. 3 is a particle size distribution diagram of nano nickel sulfide prepared in comparative example 4;
fig. 4 is the microscopic morphology of the nano nickel sulfide prepared in example 1 under an electron microscope.
Detailed Description
The present invention will now be described in further detail with reference to the accompanying drawings and preferred embodiments. These drawings are simplified schematic views illustrating only the basic structure of the present invention in a schematic manner, and thus show only the constitution related to the present invention.
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution; compared with stirring and emulsification, a large amount of tiny gas flow bubbles generated by the nano gas generator can enable nonpolar microspheres in the polar component to be formed more quickly and uniformly, and the particle size formed by the microspheres is smaller;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 190-220 ℃, and the reaction time is 18-20 h;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
The finished product of the nano nickel sulfide is stored in ethanol or pure water solution without drying and storing. If the nano nickel sulfide is stored in a dry state, the nano nickel sulfide finished product can generate agglomeration phenomenon because the particles are too fine.
In the S1, the molar ratio of the sulfur-containing component to the nickel source is 1: a, B is less than or equal to 3.
The volume ratio of the active sulfur-containing nickel component microemulsion solution to the polar component in S2 is 1.
In S3, 1g of solid sodium hydroxide is added into each 50ml of particle emulsion solution, and the solution is directly settled without stirring.
The sulfur-containing component in the S1 is sulfur-containing carbon-oxygen organic matter capable of decomposing to generate hydrogen sulfide gas; the nickel source is one or more of nickel sulfate, nickel chloride, nickel sulfamate, nickel bromide and nickel nitrate; the surfactant is a high temperature stable surfactant.
And the polar component in the S2 is a high-boiling-point polar organic matter.
The sulfur-containing component is one or more of thioacetamide, thioacetic acid and thiodipropionic acid.
The surfactant is one or more of polyoxyethylene lauryl ether, fatty alcohol polyoxyethylene ether, disodium sulfosuccinate monoester and sodium dodecyl benzene sulfonate.
The polar component is one or more of toluene, p-xylene, n-heptane, chlorobenzene, o-dichlorobenzene and isooctane.
The organic solvent in S4 is one or more of ethanol, acetone, ethyl acetate, n-hexane and dichloromethane.
Example 1
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution; the molar ratio of the sulfur-containing component to the nickel source is 1: b is less than or equal to 3;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution; the volume ratio of the active sulfur-containing nickel component microemulsion solution to the polar component is 1;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 190 ℃ and the reaction time is 20 hours; 1g of solid sodium hydroxide is added into every 50ml of particle emulsion solution, and the mixture is directly settled without stirring;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
The sulfur-containing component in S1 is thioacetamide; the nickel is original nickel sulfate; the surfactant is polyoxyethylene lauryl ether; the polar component in S2 is toluene; the organic solvent in S4 is ethanol.
Example 2
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution; the molar ratio of the sulfur-containing component to the nickel source is 1: b is less than or equal to 2.7;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution; the volume ratio of the active sulfur-containing nickel component microemulsion solution to the polar component is 1;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 200 ℃, and the reaction time is 18h; 1g of solid sodium hydroxide is added into every 50ml of particle emulsion solution, and the solution is directly settled without stirring;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing by water; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
The sulfur-containing component in S1 is thioacetic acid; the nickel is original nickel chloride; the surfactant is fatty alcohol-polyoxyethylene ether; the polar component in the S2 is p-xylene; the organic solvent in S4 is acetone.
Example 3
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution; the molar ratio of the sulfur-containing component to the nickel source is 1: b is less than or equal to 2;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution; the volume ratio of the active sulfur-containing nickel component microemulsion solution to the polar component is 1;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 220 ℃, and the reaction time is 18h; 1g of solid sodium hydroxide is added into every 50ml of particle emulsion solution, and the solution is directly settled without stirring;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing by water; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
The sulfur-containing component in the S1 is thiodipropionic acid; the nickel is original nickel sulfamate; the surfactant is disodium sulfosuccinate monoester; s2, the polar component is n-heptane; the organic solvent in S4 is ethyl acetate.
Example 4
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution; the molar ratio of the sulfur-containing component to the nickel source is 1: b is less than or equal to 1.5;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution; the volume ratio of the active sulfur-containing nickel component microemulsion solution to the polar component is 1;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 210 ℃, and the reaction time is 18.5 hours; 1g of solid sodium hydroxide is added into every 50ml of particle emulsion solution, and the mixture is directly settled without stirring;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing by water; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
The sulfur-containing component in the S1 is thioacetamide; the nickel source is nickel bromide; the surfactant is sodium dodecyl benzene sulfonate; s2, the polar component is chlorobenzene; the organic solvent in S4 is n-hexane.
Example 5
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution; the molar ratio of the sulfur-containing component to the nickel source is 1: a, B is less than or equal to 1;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution; the volume ratio of the active sulfur-containing nickel component microemulsion solution to the polar component is 1;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 195 ℃ and the reaction time is 19 hours; 1g of solid sodium hydroxide is added into every 50ml of particle emulsion solution, and the solution is directly settled without stirring;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
The sulfur-containing component in S1 is thioacetic acid; the nickel is original nickel nitrate; the surfactant is polyoxyethylene lauryl ether; the polar component in S2 is o-dichlorobenzene; the organic solvent in S4 is dichloromethane.
Comparative example 1
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing the sulfur-containing component, the nickel source and the solvent water to obtain an active sulfur-containing nickel component microemulsion solution;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 190-220 ℃, and the reaction time is 18-20 h;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
Comparative example 2
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution;
s2, preparing a particle emulsion solution: putting the active sulfur-nickel-containing component microemulsion solution prepared in the S1 into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 190-220 ℃, and the reaction time is 18-20 h;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing by water; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
Comparative example 3
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component micro-emulsion solution prepared in the S1, and uniformly stirring to obtain a mixed solution;
s3, hydrothermal reaction: adding the mixed solution prepared by the step S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 190-220 ℃, and the reaction time is 18-20 hours;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing by water; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
Comparative example 4
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 into a hydrothermal reaction kettle, wherein the reaction temperature is 190-220 ℃, and the reaction time is 18-20 h;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
Comparative example 5
A preparation method of nano nickel sulfide specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the step S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution;
and S3, standing for 24h.
As can be seen from fig. 1 to 4, the expressions of example 1 and comparative examples 1 to 5 are shown in the following table:
in conclusion, the preparation method of the nano nickel sulfide has reasonable design and simple and convenient operation, the polar component is added into the nonpolar solution (the surfactant), under the action of the nano bubble generator, the nonpolar component forms a large amount of fine microspheres in the polar component under the emulsification action of the surfactant, the nickel-containing component and the sulfur-containing component are wrapped in the polar component to be used as a tiny reaction unit, and in the hydrothermal reaction kettle, the sulfur and the nickel in the tiny reaction unit are promoted to react and finally destroy the microspheres in the high-temperature and high-pressure environment; strong acid is generated in the reaction process, nickel sulfide is re-dissolved, and excessive strong acid is reacted by solid hydroxide, so that the reaction is normally carried out.
While particular embodiments of the present invention have been described in the foregoing specification, various modifications, alterations and adaptations to those embodiments have been described herein without departing from the spirit and scope of the invention.
Claims (10)
1. A method for preparing nano nickel sulfide is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, preparing an active sulfur-nickel-containing component microemulsion solution: mixing a sulfur-containing component, a nickel source, a surfactant and solvent water to obtain an active sulfur-containing nickel component microemulsion solution;
s2, preparing a particle emulsion solution: adding a polar component into the active sulfur-nickel-containing component microemulsion solution prepared in the S1, uniformly stirring to obtain a mixed solution, putting the mixed solution into a nano bubble generator, and bubbling for 10min to obtain a particle emulsion solution;
s3, hydrothermal reaction: adding the particle emulsion solution prepared by the S2 and solid sodium hydroxide into a hydrothermal reaction kettle, wherein the reaction temperature is 190-220 ℃, and the reaction time is 18-20 h;
s4, ultrasonic cleaning: s3, after the reaction is finished, filtering and taking out the precipitate, ultrasonically cleaning the precipitate for 5-10 min by using an organic solvent, filtering and washing by water; and repeating the ultrasonic cleaning and the water washing for 2-3 times to obtain a finished product of the nano nickel sulfide, and storing the finished product of the nano nickel sulfide in ethanol or pure water solution.
2. The method for preparing nano nickel sulfide as claimed in claim 1, wherein the method comprises the following steps: in the S1, the molar ratio of the sulfur-containing component to the nickel source is 1, the molar ratio of the sulfur-containing component to the surfactant is 3: a and B are less than or equal to 3.
3. The method for preparing nano nickel sulfide as claimed in claim 1, wherein the method comprises the following steps: the volume ratio of the active sulfur-containing nickel component microemulsion solution to the polar component in S2 is 1.
4. The method for preparing nano nickel sulfide as claimed in claim 1, wherein the method comprises the following steps: 1g of solid sodium hydroxide is added to 50ml of the microparticle emulsion solution in the S3.
5. The method for preparing nano nickel sulfide as claimed in claim 1, wherein the method comprises the following steps: the sulfur-containing component in the S1 is a sulfur-containing carbon-oxygen organic matter capable of decomposing to generate hydrogen sulfide gas; the nickel source is one or more of nickel sulfate, nickel chloride, nickel sulfamate, nickel bromide and nickel nitrate; the surfactant is a high temperature stable surfactant.
6. The method for preparing nano nickel sulfide as claimed in claim 1, wherein the method comprises the following steps: and the polar component in the S2 is a high-boiling-point polar organic matter.
7. The method for preparing nano nickel sulfide as claimed in claim 5, wherein the method comprises the following steps: the sulfur-containing component is one or more of thioacetamide, thioacetic acid and thiodipropionic acid.
8. The method for preparing nano nickel sulfide as claimed in claim 5, wherein the method comprises the following steps: the surfactant is one or more of polyoxyethylene lauryl ether, fatty alcohol-polyoxyethylene ether, disodium sulfosuccinate monoester and sodium dodecyl benzene sulfonate.
9. The method for preparing nano nickel sulfide as claimed in claim 6, wherein the method comprises the following steps: the polar component is one or more of toluene, p-xylene, n-heptane, chlorobenzene, o-dichlorobenzene and isooctane.
10. The method for preparing nano nickel sulfide as claimed in claim 6, wherein the method comprises the following steps: the organic solvent in S4 is one or more of ethanol, acetone, ethyl acetate, n-hexane and dichloromethane.
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| Title |
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| 郎雷鸣: "不同形貌硫化镍纳米材料的可控合成及电化学性能研究", 南京晓庄学院学报, vol. 1, no. 06, pages 60 - 64 * |
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