CN103924290B - Co for ammonium perchlorate catalytic decomposition3O4The preparation method of nano thin-film and application - Google Patents
Co for ammonium perchlorate catalytic decomposition3O4The preparation method of nano thin-film and application Download PDFInfo
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- CN103924290B CN103924290B CN201410154278.4A CN201410154278A CN103924290B CN 103924290 B CN103924290 B CN 103924290B CN 201410154278 A CN201410154278 A CN 201410154278A CN 103924290 B CN103924290 B CN 103924290B
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Abstract
The invention discloses a kind of Co for ammonium perchlorate catalytic decomposition3O4The preparation method of nano thin-film and application, described preparation method comprises the following steps: by Co2SO4Solution and NaOH solution mixing, react in microwave, cool down with liquid nitrogen, static rear sucking filtration, wash with frozen water, the filtering residue lyophilization that will be extracted into, and finally, under 300-500 DEG C of condition, annealing obtains monocrystalline (111) face Co3O4Nano thin-film. Adopt this method can obtain the Co in monocrystalline (111) face3O4Nano thin-film, this Co3O4Nano thin-film is applied in ammonium perchlorate catalytic decomposition, it is possible to decrease the decomposition temperature of ammonium perchlorate, decomposition temperature can be reduced to 271 DEG C.
Description
Technical field
The invention belongs to nano science and energetic material field, be specifically related to a kind of Co for ammonium perchlorate catalytic decomposition3O4The preparation method of nano thin-film, the method is the Co of specific morphology and crystal face3O4Synthesis provides a kind of new method, and decomposing for ammonium perchlorate (AP) provides a kind of effective catalyst, and at space industry, particularly composite solidpropellant aspect is widely applied prospect.
Background technology
Ammonium perchlorate (AP) is the important oxidant of composite solidpropellant, and in composite solidpropellant, content reaches more than 70%, and its thermal decomposition characteristic has important impact for the combustion process of propellant. The thermal degradation activation energy of ammonium perchlorate, the thermal decomposition parameter such as speed and high-temperature decomposition temperature and the combustibility of solid propellant, particularly fire speed and there is close relationship. The high-temperature decomposition temperature of ammonium perchlorate is more low, then the ignition delay time of propellant is more short, and combustion speed is more high. Therefore, catalysis AP reduces decomposition temperature is an important matter of science and technology. The thermal decomposition performance of AP can be adjusted by a small amount of catalyst of interpolation, and research shows, the thermal decomposition of AP is had obvious catalytic action by many nano materials such as nano metal, nano transition metal oxides.
Cobalto-cobaltic oxide (Co3O4) it is a kind of important transition metal oxide, it is widely used in the fields such as catalyst, magnetic material, pressure-sensitive ceramic material, anode material for lithium-ion batteries, electrode material for super capacitor, gas sensor sensing element. Research in recent years finds Co3O4AP is decomposed and has good catalytic effect.Synthesize various structure C o at present3O4For the research of catalytic decomposition AP, as (CrystEngComm, 2012,14,7721-7726) such as Wei-YinSun have synthesized the Co of three kinds of different nanostructureds3O4, and have studied AP catalytic effect respectively, XiaohongJiang etc. (JournalofHazardousMaterials225-226 (2012) 124-130) synthesizes nanometer rods, micron particle, is tested by TG and AP is decomposed catalysis characteristics. Co3O4The crystal face of crystal is different, and its catalysis activity is different, and experimental and theoretical computation shows, Co3O4(111) face activity of crystal is the highest, and catalytic effect is best, controls the Co of synthesis particular crystal plane3O4Nanostructured becomes the focus of research, is also technological difficulties. LvBaoliang etc. have synthesized (111) face nano-particle and have studied the catalysis to AP, it is possible to make decomposition temperature be reduced to 300 DEG C. Two-dimensional nano-film material has the physicochemical characteristics of uniqueness, can expose more crystal face simultaneously, if synthesis Co can be controlled3O4Nano thin-film, and make it expose more (111) crystal face, it is possible to catalytic effect can be made better.
Summary of the invention
It is an object of the invention to provide a kind of Co for ammonium perchlorate catalytic decomposition3O4The preparation method of nano thin-film, for controlling synthesis nanostructured Co3O4Thering is provided a kind of new method, decomposing for ammonium perchlorate (AP) provides a kind of effective catalyst.
In order to reach above-mentioned technique effect, the present invention takes techniques below scheme:
A kind of Co for ammonium perchlorate catalytic decomposition3O4The preparation method of nano thin-film, comprises the following steps: by CoSO4Solution and NaOH solution mixing, react in microwave, cool down with liquid nitrogen, static rear sucking filtration, wash with frozen water, the filtering residue lyophilization that will be extracted into, and finally, under 300-500 DEG C of condition, annealing obtains monocrystalline (111) face Co3O4Nano thin-film.
In above-mentioned preparation method, described CoSO4The concentration of solution is 0.001-0.8mol/L.
In above-mentioned preparation method, the concentration of described NaOH solution is 0.001-0.4mol/L.
In above-mentioned preparation method, described CoSO4It is 1:2 with the ratio of the amount of substance of NaOH.
In above-mentioned preparation method, in described microwave, the time of reaction is 5��10min.
In above-mentioned preparation method, the time of described annealing is 1��5h.
Co3O4Nano thin-film is applied to the method for ammonium perchlorate catalytic decomposition, described Co3O4The mass fraction of nano thin-film is 0.1��5%.
The present invention utilizes the layer structure feature of bivalence cobalt basic salt Cox (OH) y (X) z (X represents anion), selects cobaltous sulfate (CoSO4) and sodium hydroxide (NaOH) solution as reactant, under microwave environment reaction generate Cox (OH) y (SO4) z intermediate, continue to be obtained by reacting Co (OH)2, after having reacted, prevent Co (OH) with liquid nitrogen cooling at once2The reunion of nano thin-film, anneals at 300-500 DEG C after lyophilization, obtains the Co in monocrystalline (111) face3O4Nano thin-film.
The present invention compared with prior art, has following beneficial effect:
Adopt this method can obtain the Co in monocrystalline (111) face3O4Nano thin-film, this Co3O4Nano thin-film is applied in ammonium perchlorate catalytic decomposition, it is possible to decrease the decomposition temperature of ammonium perchlorate, decomposition temperature can be reduced to 271 DEG C.
Accompanying drawing explanation
Fig. 1 is the Co of embodiment 4 preparation3O4The SEM figure of nano thin-film;
Fig. 2 is the Co of embodiment 4 preparation3O4The XRD diffraction pattern of nano thin-film;
Fig. 3 is the Co of embodiment 4 preparation3O4TEM, HRTEM, the SAED figure of nano thin-film;
Fig. 4 is the Co of embodiment 4 preparation3O4The DSC figure that nano thin-film catalysis AP decomposes.
Detailed description of the invention
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
Take the CoSO that 10ml concentration is 0.001mol/L4Solution and the NaOH solution mixing that 20ml concentration is 0.001mol/L, react 5min in microwave, solution after reaction is placed in liquid nitrogen cooling, then with about 200ml distilled water wash sucking filtration, filtering residue lyophilization 2 days, finally at Muffle furnace 300 DEG C annealing 2h, obtains monocrystalline Co3O4Nano thin-film. Mixing with a certain amount of AP, make Co3O4Content be 0.1%, test heat analyze, obtain decomposition temperature 340 DEG C.
Embodiment 2:
Take the CoSO that 10ml concentration is 0.001mol/L4Solution and the NaOH solution mixing that 20ml concentration is 0.001mol/L, react 5min in microwave, solution after reaction is placed in liquid nitrogen cooling, then with about 200ml distilled water wash sucking filtration, filtering residue lyophilization 2 days, finally at Muffle furnace 300 DEG C annealing 2h, obtains monocrystalline Co3O4Nano thin-film. Mixing with a certain amount of AP, make Co3O4Content be 0.5%, test heat analyze, obtain decomposition temperature 310 DEG C.
Embodiment 3:
Take the CoSO that 10ml concentration is 0.01mol/L4Solution and the NaOH solution mixing that 10ml concentration is 0.02mol/L, react 5min in microwave, solution after reaction is placed in liquid nitrogen cooling, then with about 200ml distilled water wash sucking filtration, filtering residue lyophilization 2 days, finally at Muffle furnace 500 DEG C annealing 2h, obtains monocrystalline Co3O4Nano thin-film. Mixing with a certain amount of AP, make Co3O4Content be 0.5%, test heat analyze, obtain decomposition temperature 330 DEG C.
Embodiment 4:
Take the CoSO that 10ml concentration is 0.04mol/L4Solution and the NaOH solution mixing that 40ml concentration is 0.02mol/L, react 5min in microwave, solution after reaction is placed in liquid nitrogen cooling, then with about 200ml distilled water wash sucking filtration, filtering residue lyophilization 2 days, finally at Muffle furnace 500 DEG C annealing 2h, obtains monocrystalline Co3O4Nano thin-film. Mixing with a certain amount of AP, make Co3O4Content be 2%, test heat analyze, obtain decomposition temperature 271 DEG C.
Embodiment 5:
Take the CoSO that 10ml concentration is 0.4mol/L4Solution and the NaOH solution mixing that 40ml concentration is 0.2mol/L, react 5min in microwave, solution after reaction is placed in liquid nitrogen cooling, then with about 200ml distilled water wash sucking filtration, filtering residue lyophilization 2 days, finally at Muffle furnace 500 DEG C annealing 2h, obtains monocrystalline Co3O4Nano thin-film. Mixing with a certain amount of AP, make Co3O4Content be 3%, test heat analyze, obtain decomposition temperature 296 DEG C.
Embodiment 6:
Take the CoSO that 10ml concentration is 0.8mol/L4Solution and the NaOH solution mixing that 40ml concentration is 0.4mol/L, react 5min in microwave, solution after reaction is placed in liquid nitrogen cooling, then with about 200ml distilled water wash sucking filtration, filtering residue lyophilization 2 days, finally at Muffle furnace 400 DEG C annealing 2h, obtains monocrystalline Co3O4Nano thin-film. Mixing with a certain amount of AP, make Co3O4Content be 3%, test heat analyze, obtain decomposition temperature 302 DEG C.
Embodiment 7:
Take the CoSO that 10ml concentration is 0.08mol/L4Solution and the NaOH solution mixing that 40ml concentration is 0.04mol/L, react 5min in microwave, solution after reaction is placed in liquid nitrogen cooling, then with about 200ml distilled water wash sucking filtration, filtering residue lyophilization 2 days, finally at Muffle furnace 500 DEG C annealing 2h, obtains monocrystalline Co3O4Nano thin-film.Mixing with a certain amount of AP, make Co3O4Content be 3%, test heat analyze, obtain decomposition temperature 322 DEG C.
Embodiment 8:
Take the CoSO that 10ml concentration is 0.005mol/L4Solution and the NaOH solution mixing that 50ml concentration is 0.002mol/L, react 5min in microwave, solution after reaction is placed in liquid nitrogen cooling, then with about 200ml distilled water wash sucking filtration, filtering residue lyophilization 2 days, finally at Muffle furnace 500 DEG C annealing 2h, obtains monocrystalline Co3O4Nano thin-film. Mixing with a certain amount of AP, make Co3O4Content be 3%, test heat analyze, obtain decomposition temperature 289 DEG C.
The Co of the application3O4The decomposition temperature of AP is adopted following method by nano thin-film: weigh a certain amount of Co3O4Nano thin-film and AP mixing, add ethanol stirring, mix homogeneously, takes 2-3mg after drying and tests TG-DSC, test condition: nitrogen (N2) atmosphere, flow: 50ml/min, heating rate 5-10 DEG C/min, temperature range: 30-550 DEG C.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, above-described embodiment is only the present invention preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, should be appreciated that, those skilled in the art can be designed that a lot of other amendments and embodiment, and these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (2)
1. the Co for ammonium perchlorate catalytic decomposition3O4The preparation method of nano thin-film, it is characterised in that comprise the following steps: by CoSO4Solution and NaOH solution mixing, react in microwave, cool down with liquid nitrogen, static rear sucking filtration, wash with frozen water, the filtering residue lyophilization that will be extracted into, and finally, under 300-500 DEG C of condition, annealing obtains monocrystalline (111) face Co3O4Nano thin-film; Described CoSO4The concentration of solution is 0.001-0.8mol/L; The concentration of described NaOH solution is 0.001-0.4mol/L; Described CoSO4It is 1:2 with the ratio of the amount of substance of NaOH; In described microwave, the time of reaction is 5��10min.
2. the Co for ammonium perchlorate catalytic decomposition according to claim 13O4The preparation method of nano thin-film, it is characterised in that the time of described annealing is 1��5h.
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| CN113563140A (en) * | 2021-07-08 | 2021-10-29 | 南京理工大学 | Application of total-nitrogen high-energy compound in catalysis of thermal decomposition of ammonium perchlorate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498042A (en) * | 2009-03-13 | 2009-08-05 | 南京大学 | Resistance variable oxide material Co3O4 thin film, preparation and use thereof |
| CN101665329A (en) * | 2009-09-14 | 2010-03-10 | 杭州电子科技大学 | Preparation method of tricobalt tetraoxide film |
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| KR100918845B1 (en) * | 2007-10-31 | 2009-09-28 | 인하대학교 산학협력단 | Method for preparation of CO3O4 thin films having mesoporous structure by electrochemical deposition and CO3O4 thin films prepared by the method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498042A (en) * | 2009-03-13 | 2009-08-05 | 南京大学 | Resistance variable oxide material Co3O4 thin film, preparation and use thereof |
| CN101665329A (en) * | 2009-09-14 | 2010-03-10 | 杭州电子科技大学 | Preparation method of tricobalt tetraoxide film |
Non-Patent Citations (2)
| Title |
|---|
| Shape-controlled synthesis of Co3O4 nanostructures derived from coordination polymer precursors and their application to the thermal decomposition of ammonium perchlorate;Jin Li-Na，等;《CrystEngComm》;20120703;第14卷;7721-7726 * |
| Synhtesis and properties of octahedral Co3O4 single-crystalline nanoparticles enclosed by (111) facets;Hai Zhou，等;《CrystEngComn》;20130902;第15卷;正文第2页第6行-第3页第2行，第6页第63行-第75行 * |
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