CN106853984A - A kind of preparation method of the nano oxygen cadmium of special appearance - Google Patents
A kind of preparation method of the nano oxygen cadmium of special appearance Download PDFInfo
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- CN106853984A CN106853984A CN201710107759.3A CN201710107759A CN106853984A CN 106853984 A CN106853984 A CN 106853984A CN 201710107759 A CN201710107759 A CN 201710107759A CN 106853984 A CN106853984 A CN 106853984A
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- cadmium
- nano oxygen
- preparation
- hexagon
- special appearance
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- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Chemical compound [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 72
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 claims abstract description 53
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical group FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 28
- PLLZRTNVEXYBNA-UHFFFAOYSA-L cadmium hydroxide Chemical compound [OH-].[OH-].[Cd+2] PLLZRTNVEXYBNA-UHFFFAOYSA-L 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- AMULVJPCIVLXGR-UHFFFAOYSA-N cadmium(2+) ethanol dinitrate Chemical compound C(C)O.[N+](=O)([O-])[O-].[Cd+2].[N+](=O)([O-])[O-] AMULVJPCIVLXGR-UHFFFAOYSA-N 0.000 claims abstract description 9
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 17
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- HUKFCVYEXPZJJZ-UHFFFAOYSA-N cadmium;hydrate Chemical compound O.[Cd] HUKFCVYEXPZJJZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 230000011218 segmentation Effects 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 35
- 238000000034 method Methods 0.000 abstract description 20
- 239000000843 powder Substances 0.000 abstract description 15
- 239000000243 solution Substances 0.000 description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000005979 thermal decomposition reaction Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 229910052793 cadmium Inorganic materials 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000010835 comparative analysis Methods 0.000 description 4
- 238000004455 differential thermal analysis Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- YKYOUMDCQGMQQO-UHFFFAOYSA-L Cadmium chloride Inorganic materials Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 description 3
- 101000957678 Mus musculus Cytochrome P450 7B1 Proteins 0.000 description 3
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 101000957679 Rattus norvegicus 25-hydroxycholesterol 7-alpha-hydroxylase Proteins 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KHPLPBHMTCTCHA-UHFFFAOYSA-N ammonium chlorate Chemical compound N.OCl(=O)=O KHPLPBHMTCTCHA-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 239000003380 propellant Substances 0.000 description 2
- 241000168486 Causus Species 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910000369 cadmium(II) sulfate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910001914 chlorine tetroxide Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
-
- 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/26—Chromium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation method of the nano oxygen cadmium of special appearance.The method includes：Lithium hydroxide solution is added dropwise in cadmium nitrate ethanol solution, obtained mixed liquor is scrubbed, dry in 10~12h, products therefrom is reacted at 180~200 DEG C, obtains cadmium hydroxide presoma；By obtained cadmium hydroxide presoma baking inphases, nano oxygen cadmium powder is obtained；Gained nano oxygen cadmium is the hexagon cadmium oxide nanometer plate of loose structure.Obtained nano oxygen cadmium powder purity of the invention is high, catalytic performance is high, the catalyst as Performance for Decomposition of Ammonium Perchlorate.Preparation method of the present invention is simple, and low cost is suitable to commercial Application.
Description
Technical field
The present invention relates to a kind of preparation method of the nano oxygen cadmium of the special appearance of high catalytic performance, belong to nano material
Technical field.
Background technology
Cadmium oxide (CdO) is a kind of typical n-type semiconductor, and the difference of its band gap comes from the room of cadmium and oxygen, and
There is close relationship with preparation process.Cadmium oxide is widely used in optoelectronic areas, for example solar cell, phototransistor,
Photodiode, transparency electrode, gas sensor etc..Meanwhile, cadmium oxide also is used as the thermal decomposition catalyst of ammonium perchlorate.It is high
Ammonium chlorate (AP), molecular formula is NH4ClO4, colourless or white orthogonal or acicular crystal.Have a hygroscopicity, heat resolve, by causus or
Clashing to set off an explosion, and belong to strong oxidizer, be commonly used for propellant.Decomposition temperature and decomposition rate of ammonium perchlorate etc.
There is substantial connection with the combustibility of rocket solid propellant in parameter.Therefore, the gold that pattern is different, microstructure is special is prepared
Category oxide-based nanomaterial, it is always focus of concern therefrom to filter out the catalyst with excellent properties.
In recent years, nanometer cadmium hydroxide Cd (OH) of different-shape is prepared using different methods2, by being calcined dehydration,
Obtain the existing document report of research of nanometer CdO.Wherein, the research of six side's CdO nanometer plates with anisotropic structure causes
The great interest of people.For example, Liu Junbo etc. utilizes hydro-thermal method, by cadmium nitrate Cd (NO3)2Solution is mixed with potassium hydroxide KOH solution
Close, add appropriate mineralizer NaNO3, 12h, synthesis hexagon Cd (OH) are reacted in 200-250 DEG C of baking oven2Nanometer plate.It is not added with
Mineralizer NaNO3, then without hexagon Cd (OH)2Generation.Refer to《Jilin University's journal (Edition)》, 2009,47 (3):605-
608.The report of hexagon CdO is not prepared in text, without catalytic performance test yet.
Shi Weidong etc. utilize hydro-thermal method, by CdCl2Solution mixes with NaOH solution, is placed in reactor, in 140
DEG C reaction 12h, it is scrubbed, dry, be obtained hexagon Cd (OH)2Nanometer plate, then by 350 DEG C of roasting 3h, obtain hexagon CdO
Nanometer plate.Hexagon Cd (OH) prepared by the method2Nanometer plate, surface is smooth, and the length of side is 45 ± 5nm, and thickness is about 20nm,
Wherein there is the Cd (OH) of not full-grown hexagon2.Above-mentioned hexagon Cd (OH)2Nanometer plate is calcined 3h by 350 DEG C, all
It is converted into CdO.Nanometer CdO now maintains hexagon nanometer plate pattern, and surface is smooth, but the length of side reduces, while having one
A little CdO nanometer plate structure collapses, pattern is damaged.The hexagon nanometer CdO prepared in text does not carry out catalytic property test.Referring to
Crystal Growth&Design,2006,6(4):915-918。
CN 102432061A prepare Cd (OH) in disclosing a kind of simple dicyandiamide solution2With the side of CdO hexagonal nano disks
Method, using solvent-thermal method, respectively with CdCl2、Cd(NO3)2、Cd(CH3CH2COO)2、CdSO4It is cadmium source and NaOH in water and second two
Fully reacted in the mixed solution of alcohol；Then 4h being reacted under uniform temperature (160~200 DEG C) in drying box, to obtain brownish red molten
Liquid；It is vacuum dried at 60 DEG C, obtains Cd (OH)2Brown-red powder.In 220 DEG C of high-temperature calcination 24h, CdO white powders are obtained, its
Microscopic appearance is the nanometer plate of hexagon.Obtained CdO nanometers of panel surface is smooth, the length of side be 100nm~2 μm, thickness be 50~
100nm, but size is not uniform enough, and pattern is also not regular enough.Equally, also without the testing research of associated catalytic performance.
During hexagon CdO nanometer plates are prepared disclosed in the prior art, mineralizer is added the need for having；When long the need for having
Between high-temperature calcination；The hexagon Cd (OH) of some preparations2Nanometer plate thinner thickness, hexagon CdO nanometers is converted into roasting
During disk, cause the structure collapses of product, pattern is damaged, and then has influence on its chemical property.Therefore, need badly and seek a kind of easy system
For the method for the hexagon CdO nanometer plates to Performance for Decomposition of Ammonium Perchlorate with preferable catalytic performance.The present invention is proposed for this.
The content of the invention
The present invention is in view of the shortcomings of the prior art, there is provided a kind of special appearance for Catalytic Performance for Decomposition of Ammonium Perchlorate is received
The preparation method of rice cadmium oxide.The method of the present invention has successfully synthesized pattern rule, the hexagon CdO nanometer plates of loose structure
Powder body material, and prove that there is preferable catalytic performance to the thermal decomposition of ammonium perchlorate through experimental test.
Technical scheme is as follows：
A kind of preparation method of the special appearance nano oxygen cadmium of high catalytic performance, including step is as follows：
(1) cadmium nitrate is dissolved in absolute ethyl alcohol, forms cadmium nitrate ethanol solution；Lithium hydroxide is dissolved in redistilled water
In, form lithium hydroxide solution；Under agitation, lithium hydroxide solution is added dropwise in cadmium nitrate ethanol solution, is formed
Uniform mixed liquor, continues to stir 30~90min；
(2) mixed liquor obtained in step (1) is placed in reactor, in 10~12h of reaction at 180~200 DEG C；Gained is produced
Thing is scrubbed, dry, obtains cadmium hydroxide presoma；
(3) cadmium hydroxide presoma obtained in step (2) is placed in Muffle furnace, successively 160~220 DEG C, 280~
Baking inphases at a temperature of 340 DEG C, obtain nano oxygen cadmium；Gained nano oxygen cadmium is the hexagon CdO nanometer plates of loose structure.
According to the present invention, the hexagon CdO nanometer plates of the loose structure of the nano oxygen cadmium assemble shape by small cubes
The length of side into, small cubes is 230~260nm, length of side 500nm~1 μm of the hexagon nanometer plate, and thickness is 230
~270nm.
According to currently preferred, the cadmium nitrate described in step (1) is four water cadmium nitrates.
According to currently preferred, in step (1), mol ratio=1 of cadmium nitrate and lithium hydroxide:2.3~2.7；Enter one
Step is preferred, mol ratio=1 of the cadmium nitrate and lithium hydroxide:2.5；Cadmium nitrate can be to product shape with the amount ratio of lithium hydroxide
Looks bring material impact.
, according to the invention it is preferred to, the continuation mixing time described in step (1) is 50~70min, further preferably
, continuation mixing time is 60min.
According to currently preferred, the washing described in step (2) is to use redistilled water, absolute ethanol washing successively.
According to currently preferred, the drying temperature described in step (2) is 80~90 DEG C, and drying time is 20~38h；
It is further preferred that drying temperature is 85 DEG C, 30h is dried.
According to currently preferred, the baking inphases described in step (3) are 180~220 DEG C of 1~1.5h of roasting, then
280-320 DEG C of 2~2.5h of roasting；Further preferred 80-100 DEG C of baking inphases temperature difference is preferred.Most preferably, described point
Section is roasted to 200 DEG C of roasting 1h, then 300 DEG C of roasting 2h.The mode of the sintering temperature and two-stage roasting is also to prepare pattern
Rule, porous hexagon cadmium oxide nanometer plate key factor.
According to currently preferred, cadmium hydroxide presoma obtained in step (2) is hexagonal crystal phase, and shape characteristic is surface
The cadmium hydroxide nanometer plate of smooth, regular hexagonal, 400~900nm of the length of side, thickness is 210~300nm.Further preferably
, the cadmium hydroxide nanometer plate length of side of the hexagon is 500~800nm, and thickness is 230~280nm.
The cadmium hydroxide presoma is placed in Muffle furnace, by double roasting, cadmium oxide powder is obtained.The cadmium oxide is
Cube crystalline phase, shape characteristic is by the porous hexagon cadmium oxide nanometer plate of small cubes assembling formation rule.Small cubes
The length of side is 230~260nm, and length of side 500nm~1 μm of the hexagon nanometer plate being assembled into, thickness is 230~270nm.Further
Preferably, the length of side of small cubes is 250~260nm, the 700~900nm of the length of side of the hexagon nanometer plate being assembled into, and thickness is
250~260nm.
Application of the cadmium oxide nanometer plate of special appearance prepared by the present invention in terms of Catalytic Performance for Decomposition of Ammonium Perchlorate.This hair
The cadmium oxide nanometer plate of the special appearance of bright preparation is used as Performance for Decomposition of Ammonium Perchlorate catalyst.
The present invention tests the hexagon CdO nanometer plates of loose structure to height using TG-DTA analysis method (TG-DTA)
The thermal decomposition catalytic performance of ammonium chlorate, catalytic performance measurement result shows that the hexagon of loose structure prepared by the present invention is aoxidized
Cadmium nanometer plate has preferable catalytic property, can be used as the High Efficiency Thermal decomposition catalyst application of ammonium perchlorate.
Technical characterstic of the invention and excellent results：
Present invention cadmium nitrate and lithium hydroxide are smooth through solvent thermal reaction generation surface, the hexagon hydrogen-oxygen of the close rule of matter
Cadmium presoma, then through the roasting of double different temperatures, obtains nano oxygen cadmium powder, and microscopic appearance is by small cube
The porous hexagon cadmium oxide nanometer plate of body assembling formation rule.The hydrogen-oxygen of the hexagonal configuration of the close rule of matter prepared by the present invention
The characteristics of cadmium presoma is uniform in size, and thickness is thicker, so during roasting dehydration is changed into cadmium oxide, can be formed
Porous microstructure, can keep complete hexagonal configuration again.The special microscopic appearance is that it has preferably catalysis
The premise of performance.
Nano oxygen cadmium prepared by the inventive method has advantages below：
1st, obtained cadmium hydroxide presoma is hexagonal crystal phase, and diffraction maximum is consistent with standard card (PDF#31-0228), nothing
Other impurities are present, and purity is high.Its microscopic appearance feature is that surface is smooth, the hexagon of the close rule of matter.
2nd, the obtained nano oxygen cadmium of the present invention is cube crystalline phase, and diffraction maximum is consistent with standard card (PDF#65-2908),
Its microscopic appearance feature is by the porous hexagon cadmium oxide nanometer plate of small cubes assembling formation rule.
It is 3rd, of the invention with lithium hydroxide as raw material compared with NaOH and potassium hydroxide raw material that prior art is used,
Because lithium hydroxide is slightly soluble in water and ethanol, when being reacted with the ethanol solution of cadmium nitrate, a large amount of precipitations will not be at once produced, can be with
The nucleus of fine uniform is formed, slowly aggregation growth, is conducive to the generation of uniform products；In addition, the present invention is it has surprisingly been found that hydrogen
The ability of lithia absorbing carbon dioxide in building-up process is slightly worse compared with NaOH and potassium hydroxide, is thus susceptible to prepared high-purity
The nano oxygen cadmium product of degree.
4th, the nano oxygen cadmium powder property stabilization obtained by the present invention, catalytic performance is good, for the low temperature of ammonium perchlorate
Decompose, pyrolytic all has stable high catalytic performance.Particularly have to the low-temperature decomposition of ammonium perchlorate unexpected
Efficient catalytic is acted on, and ammonium perchlorate can be made to have stronger low-temperature decomposition effect at 280~330 DEG C.
5th, preparation method of the present invention is simple, and reaction temperature is not high, low for equipment requirements, and raw material is easy to get, cheap, is adapted to
Batch production.
6th, the inventive method prepare nano oxygen cadmium in addition to as catalyst, also with anti-microbial property and air-sensitive performance.
Brief description of the drawings
Fig. 1 is the x-ray diffraction pattern of the nanometer cadmium hydroxide powder and nano oxygen cadmium powder prepared using this method
Figure.Wherein, (a) nanometer cadmium hydroxide；(b) nano oxygen cadmium.
Fig. 2 is the stereoscan photograph of nanometer cadmium hydroxide powder prepared by embodiment 1.
Fig. 3 is the stereoscan photograph of nano oxygen cadmium powder prepared by embodiment 1.
Fig. 4 is that nano oxygen cadmium powder prepared by embodiment 1 thermally decomposes the TG-DTA figure being catalyzed to ammonium perchlorate
Spectrum.
Fig. 5 is the TG-DTA collection of illustrative plates of ammonium perchlorate itself thermal decomposition.For comparative analysis.
Specific embodiment
With reference to embodiment, the present invention will be further described, but institute's protection domain not limited to this of the present invention.
The TG-DTA analysis instrument used in embodiment is that the HCT-1 type microcomputers of the permanent scientific instrument factory production in Beijing are poor
Thermobalance.
Term explanation：Differential thermal analysis (Differential Thermal Analysis) is abbreviated as DTA.DTG
(Thermogravimetry) it is abbreviated as TG；TG-DTA analysis method is abbreviated as TG-DTA.
The preparation method of embodiment 1, a kind of special appearance nano oxygen cadmium of high catalytic performance, including step is as follows：
(1) the water cadmium nitrates of 0.7712g (2.5mmol) four are weighed to be dissolved in 50mL absolute ethyl alcohols, cadmium nitrate ethanol is formed molten
Liquid.Weigh 0.2623g (6.25mmol) lithium hydroxide to be dissolved in 20mL redistilled waters, form lithium hydroxide solution.
Under agitation, lithium hydroxide solution is added dropwise in cadmium nitrate ethanol solution, after being added dropwise to complete, is continued
Stirring 60min.
(2) step (1) gained mixed liquor is placed in reactor, 12h is reacted at 200 DEG C.Products therefrom is successively with secondary
Distilled water, absolute ethanol washing, 85 DEG C dry 30h, obtain cadmium hydroxide presoma；Its microscopic appearance is characterized as that surface is smooth, matter
The hexagon of close rule.The length of side is 500~800nm, and thickness is 230~280nm.As shown in Figure 2.
(3) cadmium hydroxide presoma obtained in step (2) is placed in Muffle furnace, 200 DEG C of roasting 1h, then 300 DEG C of roastings
2h is burnt, nano oxygen cadmium powder is obtained, its microscopic appearance is characterized as by the porous hexagon oxygen of small cubes assembling formation rule
Cadmium nanometer plate.The length of side of small cubes is 250~260nm, and the length of side of nanometer plate is 700~900nm, thickness is 250~
260nm.As shown in Figure 3.Hexagon cadmium oxide nanometer plate pattern is complete, even particle size distribution.
Embodiment 1 obtains nano oxygen cadmium powder, as the nano oxygen cadmium catalyst of Performance for Decomposition of Ammonium Perchlorate.Urge
Change property test experiments as follows：
1. 100mg ammonium perchlorate is weighed in mortar, the nano oxygen cadmium catalyst 4mg prepared in embodiment 1 is added, and is ground
After mill is allowed to well mixed, used as sample 1, being placed in HCT-1 type microcomputer differential thermal balances carries out thermogravimetric and differential thermal analysis, and test is received
The catalytic performance of rice cadmium oxide.
Note：The nano oxygen cadmium catalyst amount of addition is different, and the thermal decomposition catalytic property to ammonium perchlorate has an impact.One
As for, consumption is bigger, and catalytic performance is better.Catalytic effect of the different nano-metal-oxides to Performance for Decomposition of Ammonium Perchlorate
It is different.
2. 100mg ammonium perchlorate is weighed as sample 2, and being placed in HCT-1 type microcomputer differential thermal balances carries out thermogravimetric and differential thermal
Analysis, tests its own thermolysis property.
3. by step 1., the step 2. thermogravimetric of two samples and differential thermal collection of illustrative plates comparative analysis, observation adds nano oxygen cadmium
After catalyst, the situation of change of the heat decomposition temperature of ammonium perchlorate and the power of exothermic peak, and then evaluate the catalysis of nano oxygen cadmium
The catalytic performance of agent.The heat decomposition temperature of ammonium perchlorate is lower, and the intensity of exothermic peak is higher, represents the thermocatalytic of nano oxygen cadmium
Performance is better.
The TG-DTA collection of illustrative plates of sample 1 is as shown in Figure 4；The TG-DTA collection of illustrative plates of sample 2 is as shown in Figure 5；
It can be seen from DTA differential thermals collection of illustrative plates (Fig. 4 and Fig. 5) comparative analysis according to two above sample, two samples are at 245 DEG C
Nearby there is an endothermic peak, be assigned as turn brilliant process that pure ammonium perchlorate is changed into cubic crystal by rhomboidal crystal, addition is received
Rice cadmium oxide catalyst does not influence on this crystalline transformation process, and this point is consistent with the result by references that early stage is reported.Add
After nano oxygen cadmium, original ammonium perchlorate is respectively reduced in 317 DEG C of low-temperature decomposition temperature and 415 DEG C of high-temperature decomposition temperature
Have obviously to the low and high temperature thermal decomposition process of ammonium perchlorate to 304 DEG C and 385 DEG C, i.e. hexagon cadmium oxide nanometer plate
Catalytic action so that the low-temperature decomposition temperature of ammonium perchlorate reduces 13 DEG C, and high-temperature decomposition temperature then reduces 30 DEG C；And chlorine high
The Exotherm amount of sour ammonium is significantly increased, and high temperature exothermic amount reduces, and illustrates hexagon cadmium oxide nanometer plate to ammonium perchlorate
The catalytic efficiency of low temperature thermal decomposition is particularly evident, presents its very excellent catalytic performance, and this characteristic is conducive to it solid
Preferably played a role in body propellant.It follows that the present embodiment 1 prepare hexagon cadmium oxide nanometer plate have it is excellent
The catalytic effect of low-temperature decomposition ammonium perchlorate.
It can be seen from TG thermogravimetrics collection of illustrative plates (Fig. 4 and Fig. 5) comparative analysis according to two above sample, pure ammonium perchlorate 300~
345 DEG C of shallower weightlessness, corresponding to the weaker low-temperature decomposition of ammonium perchlorate；It is obvious quick at 345~425 DEG C
Weightlessness, corresponding to the stronger pyrolytic of ammonium perchlorate.And after adding hexagon cadmium oxide nanometer plate, ammonium perchlorate is 280
~330 DEG C of obvious rapid weight loss, corresponding to the stronger low-temperature decomposition of ammonium perchlorate；It is shallower at 330~410 DEG C
Weightlessness, corresponding to the weaker pyrolytic of ammonium perchlorate.This also absolutely proves hexagon cadmium oxide nanometer plate to perchloric acid
The low-temperature decomposition of ammonium has obviously catalytic action.It is consistent with DTA differential thermal pattern analysis results.
Embodiment 2, as described in Example 1 method prepare hexagon cadmium oxide nanometer plate, and sequence of steps is constant, four for weighing
The mass conservation of water cadmium nitrate, is still the water cadmium nitrates (2.5mmol) of 0.7712g tetra-.Institute's difference is,
In step (1), the lithium hydroxide for weighing is 0.2413g (5.75mmol).The mol ratio of cadmium nitrate and lithium hydroxide
=1:2.3；After lithium hydroxide solution is added dropwise in cadmium nitrate ethanol solution, continuation mixing time is 50min.
In step (2), product drying condition dries 36h for 80 DEG C.
In step (3), the roasting condition of cadmium hydroxide presoma is：180 DEG C of roasting 1h, then 320 DEG C are calcined 2h.
Obtained hexagon cadmium oxide nanometer plate.The length of side of small cubes is 230~260nm, and the length of side of nanometer plate is 500
~750nm, thickness is 230~250nm.Hexagon cadmium oxide nanometer plate pattern is complete.
Catalytic property test result discovery, hexagon obtained in embodiment 2 are carried out with TG-DTA analysis method (TG-DTA)
Cadmium oxide nanometer plate has obvious catalytic action to the low and high temperature thermal decomposition process of ammonium perchlorate.The low temperature of ammonium perchlorate can be made
Decomposition temperature and high-temperature decomposition temperature reduce 10 DEG C and 23 DEG C respectively.Equally, to the Exotherm catalytic effect of ammonium perchlorate
It is substantially better than high temperature exothermic.
Embodiment 3, as described in Example 1 method prepare hexagon cadmium oxide nanometer plate, and sequence of steps is constant, four for weighing
The mass conservation of water cadmium nitrate, institute's difference is：
In step (1), the lithium hydroxide for weighing is 0.2832g (6.75mmol)；The mol ratio of cadmium nitrate and lithium hydroxide
=1:2.7.After lithium hydroxide solution is added dropwise in cadmium nitrate ethanol solution, continue to stir 70min.
In step (2), product drying condition dries 24h for 90 DEG C.
In step (3), the roasting condition of cadmium hydroxide presoma is：220 DEG C of roasting 70min, then 320 DEG C of roastings
100min.Obtained hexagon cadmium oxide nanometer plate.The length of side of small cubes is 240~260nm, and the length of side of nanometer plate is
800nm~900nm, thickness is 250~270nm.Hexagon cadmium oxide nanometer plate pattern is complete.
Catalytic property test result discovery, hexagon obtained in embodiment 3 are carried out with TG-DTA analysis method (TG-DTA)
Cadmium oxide nanometer plate also has obvious catalytic action to the low and high temperature thermal decomposition process of ammonium perchlorate.The low of ammonium perchlorate can be made
Warm decomposition temperature and high-temperature decomposition temperature reduce 11 DEG C and 25 DEG C respectively.Equally, the Exotherm to ammonium perchlorate is catalyzed effect
Fruit is substantially better than high temperature exothermic.
Embodiment 4, as described in Example 1 method prepare hexagon cadmium oxide nanometer plate, and institute's difference is：
In step (3), the roasting condition of cadmium hydroxide presoma is：220 DEG C of roasting 1h, then 280 DEG C are calcined 2h.
Obtained hexagon cadmium oxide nanometer plate.The length of side of small cubes is 250~260nm, and the length of side of nanometer plate is
800nm~1 μm, thickness is 240~270nm.Pattern is intact but has very small amount side damaged.
Catalytic property test result discovery, hexagon obtained in embodiment 4 are carried out with TG-DTA analysis method (TG-DTA)
Cadmium oxide nanometer plate also has obvious catalytic action to the low and high temperature thermal decomposition process of ammonium perchlorate.The low of ammonium perchlorate can be made
Warm decomposition temperature and high-temperature decomposition temperature reduce 9 DEG C and 24 DEG C respectively.Equally, to the Exotherm catalytic effect of ammonium perchlorate
It is substantially better than high temperature exothermic.
Claims (10)
1. a kind of preparation method of special appearance nano oxygen cadmium, including step is as follows：
(1) cadmium nitrate is dissolved in absolute ethyl alcohol, forms cadmium nitrate ethanol solution；Lithium hydroxide is dissolved in redistilled water,
Form lithium hydroxide solution；Under agitation, lithium hydroxide solution is added dropwise in cadmium nitrate ethanol solution, forms uniform
Mixed liquor, continue stir 30~90min；
(2) mixed liquor obtained in step (1) is placed in reactor, in 10~12h of reaction at 180~200 DEG C；Products therefrom is passed through
Wash, dry, obtain cadmium hydroxide presoma；
(3) cadmium hydroxide presoma obtained in step (2) is placed in Muffle furnace, successively at 160~220 DEG C, 280~340 DEG C
At a temperature of baking inphases, obtain nano oxygen cadmium；Gained nano oxygen cadmium is the hexagon CdO nanometer plates of loose structure.
2. the preparation method of special appearance nano oxygen cadmium as claimed in claim 1, it is characterised in that the nano oxygen cadmium
The hexagon CdO nanometer plates of loose structure assembled by small cubes and formed, the length of side of the small cubes is 230~260nm,
Length of side 500nm~1 μm of the hexagon nanometer plate, thickness is 230~270nm；Preferably, the length of side of the small cubes is
250~260nm, the 700~900nm of the length of side of the hexagon nanometer plate being assembled into, thickness are 250~260nm.
3. the preparation method of special appearance nano oxygen cadmium as claimed in claim 1, it is characterised in that described in step (1)
Cadmium nitrate is four water cadmium nitrates.
4. the preparation method of special appearance nano oxygen cadmium as claimed in claim 1, it is characterised in that in step (1), nitric acid
Mol ratio=1 of cadmium and lithium hydroxide:2.3~2.7；It is preferred that, mol ratio=1 of the cadmium nitrate and lithium hydroxide:2.5.
5. the preparation method of special appearance nano oxygen cadmium as claimed in claim 1, it is characterised in that described in step (1)
Continuation mixing time is 50~70min, it is preferred that continuation mixing time is 60min.
6. the preparation method of special appearance nano oxygen cadmium as claimed in claim 1, it is characterised in that described in step (2)
Washing is to use redistilled water, absolute ethanol washing successively；Preferably, the drying temperature described in step (2) is 80~90 DEG C,
Drying time is 20~38h.
7. the preparation method of special appearance nano oxygen cadmium as claimed in claim 1, it is characterised in that described in step (3)
Baking inphases are 180~220 DEG C of 1~1.5h of roasting, then 280-320 DEG C of 2~2.5h of roasting；Preferably, described segmentation roasting
It is 200 DEG C of roasting 1h to burn, then 300 DEG C of roasting 2h.
8. the preparation method of special appearance nano oxygen cadmium as claimed in claim 1, it is characterised in that hydrogen obtained in step (2)
Cadmium oxide presoma is hexagonal crystal phase, and shape characteristic is for surface is smooth, regular hexagonal cadmium hydroxide nanometer plate, the length of side
400~900nm, thickness is 210~300nm；Preferably, the cadmium hydroxide nanometer plate length of side of the hexagon be 500~
800nm, thickness is 230~280nm.
9. the preparation method of special appearance nano oxygen cadmium as claimed in claim 1, it is characterised in that oxygen obtained in step (3)
Cadmium powder is cube crystalline phase.
10. the special appearance nano oxygen cadmium prepared by any one of claim 1-9 is used as Performance for Decomposition of Ammonium Perchlorate catalyst.
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| CN110357146A (en) * | 2019-07-26 | 2019-10-22 | 南京理工大学 | A kind of batch preparation of nanometer of cadmium hydroxide or nano oxygen cadmium |
| WO2021109853A1 (en) * | 2019-12-03 | 2021-06-10 | 中国科学院深圳先进技术研究院 | Cadmium hydride porous material, preparation method for same, and negative electrode and battery comprising same |
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