CN1556031A - Burning synthesis method of NiAl2O4 spinelle powder - Google Patents
Burning synthesis method of NiAl2O4 spinelle powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 34
- 229910003303 NiAl2O4 Inorganic materials 0.000 title claims abstract description 31
- 238000001308 synthesis method Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000004202 carbamide Substances 0.000 claims abstract description 28
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 16
- 239000011029 spinel Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 42
- 239000002994 raw material Substances 0.000 claims description 24
- 238000005049 combustion synthesis Methods 0.000 claims description 20
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 19
- 229910000943 NiAl Inorganic materials 0.000 claims description 18
- 238000002485 combustion reaction Methods 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 229910002651 NO3 Inorganic materials 0.000 claims description 11
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 11
- 239000000446 fuel Substances 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 239000012047 saturated solution Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 abstract description 29
- 230000008569 process Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000009841 combustion method Methods 0.000 abstract 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000013078 crystal Substances 0.000 description 16
- 238000004519 manufacturing process Methods 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- XEVRDFDBXJMZFG-UHFFFAOYSA-N carbonyl dihydrazine Chemical compound NNC(=O)NN XEVRDFDBXJMZFG-UHFFFAOYSA-N 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 230000002269 spontaneous effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000001321 HNCO Methods 0.000 description 1
- OWIKHYCFFJSOEH-UHFFFAOYSA-N Isocyanic acid Chemical compound N=C=O OWIKHYCFFJSOEH-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002306 biochemical method Methods 0.000 description 1
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010959 commercial synthesis reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 125000001153 fluoro group Chemical class F* 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- -1 nickel aluminate Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical compound CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
Abstract
A process for synthesizing NiAl2O4 spinel powder by combustion method includes proportionally mixing the nickel nitrate, aluminium nitrate and urea to obtain mixture solution, putting it in preheated furnace, and quick burning the become foamed NiAl2O4. Its advantages are high purity (95-98%), high speed, and large specific surface area (8-150 sq.m/g).
Description
Technical Field
The invention belongs to the field of preparation of inorganic non-metallic materials. In particular to a NiAl fuel using urea2O4A combustion synthesis method of spinel powder.
Background
Nickel aluminium spinel (NiAl)2O4) The spinel material is a spinel material of transition group metal ions, shows good chemical stability and thermal stability under acidic and alkaline conditions, is regarded as a very effective catalyst material, and is applied to a plurality of chemical processes. In recent years, NiAl has been discovered2O4Spinels also have another potential use (e.g. the document "Qiu zhuxian, Research and Development of inert cathode and Anode in Aluminum Electrolysis [ J]]Light metal 2000 (9): 30-35' and "Qiazhuian. world Aluminum Industry and Development Trend of New technology [ J]Nonferrous Metals smearing, 2000, 29 (2): 1-6'), which is used as an inert anode material of an industrial aluminum electrolysis cell instead of graphite. This is because there are serious problems with the use of graphite as the anode: firstly, graphite reacts with fluorine salt in electrolyte and oxygen released in the electrolytic reaction process in the electrolytic process to cause the consumption of an electrode, the consumption rate of a graphite anode is 0.8-1.0 mm/h, and 400-600 kg of high-quality graphite is consumed for producing one ton of aluminum; secondly, harmful gases such as CO and carbon fluoride are released in the reactions, so that environmental pollution is caused, and the health of workers is seriously influenced; thirdly, due to electrode consumption and poor wettability of the graphite electrode and aluminum, a larger electrode distance needs to be kept between the electrodes, so that 0.5-0.6V overvoltage is generated, the current efficiency is low, and the electrodes do not participate in reaction in the electrolysis process after the inert anode is adopted, so that consumption is avoided; and only oxygen is released in the electrolytic reaction; at the same time, the anode gap can be properly reducedAnd meanwhile, the overvoltage is reduced, and the current efficiency is improved, so that the inert anode has great advantages in the aspects of economy and environment protection compared with a graphite anode.
NiAl2O4Spinel is a candidate for an inert anode because it has the following characteristics:
(1).NiAl2O4has high thermal stability at the electrolysis temperature (about 1000 ℃) of aluminum.
(2).NiAl2O4Has good corrosion resistance and can not react with the electrolyte.
(3).NiAl2O4The solubility in the electrolyte is very low, and the pollution to the electrolytic aluminum product is low.
(4).NiAl2O4The composite material electrode with metal has very high conductivity, and also has certain strength and corrosion resistance.
The above advantages lead to NiAl2O4The study of inert based anodes has received considerable attention. Synthesis of high-performance NiAl at low cost2O4Spinel powder is also a primary problem in the preparation of inert electrodes.
NiAl2O4The preparation method comprises a solid-phase reaction method, a sol-gel method, an ultrasonic coprecipitation method and a carbazide liquid-phase combustion synthesis method. In "Han.YS, Li.JB, et al, The efficiencies of The sinteringproperty and reactive material ratio on The production of an organic luminescent fertilizer, RARE METAL MAT ENG, 2002 (31): 214-216 suppl.1 ", the solid-phase reaction method is to use NiO and Al2O3Ball milling and mixing the powder according to the equal molar ratio, calcining at the temperature of more than 1300 ℃ for about 4 hours to synthesize NiAl2O4The method has the advantages of simple operation, uniform product powder granularity, high energy consumption and long production period. In the literature "c.o Are" n, m.pe ň arroya, Mentrdsuit et al, High surface area salts precursors a sol-gel method, colloid surf.a.2001 (180): 253 ~ 258' middle reportThe sol-gel method is that isopropoxide of Ni and Al is dissolved in isopropanol to prepare gel, and then the gel is calcined at 500 ℃ for 4 hours to obtain NiAl2O4The powder obtained by the method has good activity, very large specific surface area, low production efficiency and high raw material cost. In the document "P.Jecanandam, Yu.Koltypin et al.preparation of nanosized nickel aluminate by a biochemical method, Mater.Sci.Eng.B.2002 (90): 125-132', an ultrasonic coprecipitation method adopts a mixed solution of nitrates of Ni and Al and urea as a raw material, the mixed solution is firstly placed in an Ar atmosphere for purification for 15 minutes, then ultrasonic action is carried out for 4 hours in the Ar atmosphere, and the obtained gel is calcined for 14 hours at 950 ℃ to form NiAl2O4And (3) powder. The powder obtained by the method is in a nanometer level, has very high activity, but is too complex tooperate and has relatively high cost. In the literature "Kingsley, j.j., Suresh, k., Patil, k.c., commercial synthesis fine-particulate metals, j.mater.sci., 1990 (25): 1305-1312' report that the liquid-phase combustion synthesis method of carbazide uses the mixed solution of nitrates of Ni and Al and carbazide as raw material, the mixed solution is placed in a preheated furnace to initiate liquid spontaneous combustion, and the nitric acid of Ni and Al causes spontaneous combustion in the combustion processSalt reaction to produce NiAl2O4And (3) obtaining the product. The method has the advantages of short production period, simple operation and small product granularity, but the production cost of the product is higher due to the high price of the carbohydrazine.
Among the above methods, the liquid phase combustion synthesis method has the advantages of simple production equipment, short production period, low energy consumption, uniform and fine powder particles of the product, high sintering activity and the like, and is suitable for industrial production of high-performance powder. But in the synthesis of NiAl2O4In the powder process, the high-price carbazide is used as a combustion improver, so that the manufacturing cost is increased, and the industrial application of the powder is limited. While the liquid phase combustion synthesis method generally uses inexpensive urea as a fuel to reduce production costs, the inventors of the above-mentioned carbahydrazine liquid phase combustion synthesis method have also tried to prepare NiAl using urea as a fuel2O4Powders, but they could not be obtainedNiAl2O4They concluded that urea is not considered suitable for NiAl2O4Due to the over-high combustion temperature of urea, NiAl is generated2O4And (5) decomposing.
Disclosure of Invention
The invention provides a NiAl2O4The combustion synthesis method of the spinel powder is characterized by comprising the following steps: the NiAl is synthesized by adopting a liquid-phase combustion synthesis method and urea as a fuel2O4The spinel powder is prepared by the following steps:
1) mixing nitrate containing Ni and Al and urea with Ni2+∶Al3+∶NH2CONH21: 2: 3-10 mol ratio;
2) dissolving the raw materials into distilled water, and uniformly stirring to prepare a saturated solution;
3) the crucible containing the mixed solution is placed into a heating furnace preheated to the temperature of 370-2O4A product;
4) rolling crushed the foam-like combustion synthetic product and sieving to obtain the final product NiAl2O4And (3) powder.
The invention has the beneficial effects that: 1. the reaction adopts urea as fuel, and the cost of raw materials is low. 2. The reaction is directly heated in the air. The reaction equipment is simple and the operation is convenient. 3. The preheating temperature of the reaction is lower, the main reaction is completed instantly, the energy consumption is low, and the production cost is low. 4. The purity of the product powder is high and can reach 98 percent. 4. The product has fine crystal grains and large specific surface area. The size of the single crystal is from 11nm to 50nm, and the specific surface area is from 8m2G to 150m2/g。
Drawings
FIG. 1 is an XRD pattern of partial products obtained at different preheatingtemperatures
Detailed Description
The invention provides a NiAl2O4A combustion synthesis method of spinel powder. The NiAl is synthesized by adopting a liquid-phase combustion synthesis method and urea as a fuel2O4The spinel powder is prepared by the following steps:
1) mixing nitrate containing Ni and Al and urea with Ni2+∶Al3+∶NH2CONH21: 2: 3-10 mol ratio;
2) dissolving the raw materials into distilled water, and uniformly stirring to prepare a saturated solution;
3) the crucible containing the mixed solution is placed into a heating furnace preheated to the temperature of 370-2O4A product;
4) rolling crushed the foam-like combustion synthetic product and sieving to obtain the final product NiAl2O4And (3) powder.
Our studies show that when Ni (NO) is used3·6H2O，Al(NO3)3·9H2O and NH2CONH2When used as a raw material, the mixed liquid is heated in a furnace and then first decomposed, wherein urea is decomposed into biuret, ammonia gas and (HNCO)3Trimer, nitrate of Ni and Al decomposing into amorphous NiO and Al2O3And NO2The gas, the decomposed product of urea and the nitrogen oxide are subjected to gas phase combustion reaction, and the NiO and Al are caused to emit great heat2O3A chemical combination reaction is carried out to generate NiAl2O4. The chemical reaction formula is as follows:
according to the reaction principle, the nitrate raw material used in the invention can be selected from anhydrous nitrate or hydrous nitrate as long as the molar ratio Ni is ensured2+∶Al3+1: 2; the urea plays the role of combustion improver in the reaction process, and when the addition amount is small, the heat emitted by combustion is small, so that amorphous NiO and Al generated by decomposing nitrate are insufficient2O3A chemical combination reaction is carried out to generate NiAl2O4When the amount is too large, the yield is affected by excessive gas evolution. When using Ni (NO)3·6H2O，Al(NO3)3·9H2When O is used as the raw material, Ni (NO) is suitably added3·6H2O∶Al(NO3)3·9H2O∶NH2CONH2The molar ratio of the components is 1: 2 to (5-8).
When the preheating temperature of the heating furnace is lower than 370 ℃, the powder obtained after combustion is Al2O3And NiO does not yield NiAl2O4The product, thermal analysis of the feedstock by us, showed that this was mainly due to the following reasons: ni (NO)3)2，Al(NO3)3Different from the decomposition temperature of urea, wherein Ni (NO)3)2Decomposition starts at around 275 deg.C, and Al (NO)3)3And urea starts to decompose at about 150 ℃; the temperature at which the decomposition products of the raw material start to burn is about 300 c, and if the preheating temperature of the furnace is low and the rate of temperature rise of the raw material is slow, a long time is required to elapse between the decomposition of the raw material and the combustion of the gaseous phase, which also results in a large amount of gaseous decomposition products from the vesselMiddle overflow results in reduced heat released by combustion and no synthesis of NiAl2O4。
When the preheating temperature is 370 ℃, a small amount of amorphous NiAl can be synthesized2O4. When the preheating temperature is 400 ℃, the amorphous NiAl2O4The amount of (A) is remarkably increased, and the specific surface area is 140m2(ii) in terms of/g. Along with the increase of the preheating temperature of the heating furnace, the crystallization degree of the product is improved, the purity is correspondingly improved, but the specific surface area of the powder is reduced, when the preheating temperature reaches 500 ℃, the powder with higher crystallization degree can be obtained, and NiAl in the product2O4Has a purity of 97% or more and a specific surface area of 27m2(ii) in terms of/g. After the preheating temperature is higher than 600 ℃, the crystallization degree of the product is further improved, but the specific surface area of the product is further reduced, and the powder is coarsened. When the preheating temperature is 800 ℃, NiAl in the product2O4Has a purity of 98% and a specific surface area reduced to 10g/m2Left and right. The purity and crystallization degree of the product are not obviously changed when the preheating temperature is further increased, but the specific surface area is further reduced, and the sintering activity is obviously deteriorated. Suitable preheating temperatures are therefore from 500 ℃ to 800 ℃.
As described above, it is considered that urea is used as a raw material, and NiAl is caused by an excessively high combustion temperature of urea2O4Decomposition and no synthesis of NiAl2O4. However, previous studies by the inventors have shown that NiAl2O4Even at a high temperature of 2000 ℃ is very stable and does not have the phenomenon of pyrolysis, so the inventor thinks that the NiAl can not be synthesized by taking urea as fuel2O4And cannot be attributed to excessive combustion temperatures. By the reaction of NiAl2O4The inventor finally succeeded in preparing NiAl from urea as a fuel by intensive research on a urea liquid-phase combustion synthesis method2O4And a powder, thereby completing the present invention.
The variation of both the urea content and the furnace preheating temperature can affect the heat released by combustion, and thus the performance of the synthesized powder. If the furnace temperature is low, the product purity can be improved by increasing the urea content; if the urea content is low, the product purity can be increased by increasing the furnace temperature. Meanwhile, the purity and the specific surface area of the product are a pair of contradictory performance parameters, and the powder with the required performance can be obtained according to the specific requirements during application.
NiAl is mentioned below2O4The XRD pattern of a portion of the product is shown in FIG. 1, and the properties are shown in Table 1 (where the phase composition and single crystal size of the product are measured using an X-ray diffractometer (D/max-RB X-ray diffactometer Rigku, Japan, scanning speed 4 °/min, step width 0.02 °). CuK α (wavelength 0.15418nm) radiation, Ni filters are used, the phase content is calculated using the k-value method, two diffraction peaks are used for each phase, and the single crystal size is calculated using Scherrer's officialFormula (i) is calculated as Dhkl＝0.89λ/(βhklcos θ) of the crystal plane, the corresponding derivative of the (440) crystal plane being selected for use in the calculationAnd (4) peak shooting. The specific surface area of the powder was measured by a NOVA model 4000 high-speed specific surface area and porosity analyzer manufactured by KANGTAO, USA.
Example 1
By using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As a raw material, N2+∶Al3+∶NH2CONH2Preparing a solution according to the mol ratio of 1: 2: 6.67, and putting the solution into a furnace with the temperature of 700 ℃ for combustion synthesis. The purity of the obtained product is 98 percent, and the specific surface area is about 12m by using an X-ray diffractometer2In terms of a single crystal size of 41 nm.
Example 2
By using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As a raw material, N2+∶Al3+∶NH2CONH2Preparing a solution according to the mol ratio of 1: 2: 6.67, and putting the solution into a furnace with the temperature of 800 ℃ for combustion synthesis. The purity of the obtained product is 98 percent, and the specific surface area is about 9m by using an X-ray diffractometer2In terms of a/g, the single crystal size is 47 nm.
Example 3
By using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As a raw material, N2+∶Al3+∶NH2CONH2Preparing a solution according to the mol ratio of 1: 2: 6.67, and putting the solution into a furnace with the temperature of 600 ℃ for combustion synthesis. The purity of the obtained product is 98 percent, and the specific surface area is about 10m by using an X-ray diffractometer2In terms of a single crystal size of 41 nm.
Example 4
By using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As a raw material, N2+∶Al3+∶NH2CONH2Preparing a solution according to the mol ratio of 1: 2: 6.67, and putting the solution into a furnace with the temperature of 500 ℃ for combustion synthesis. The purity of the obtained product is 97 percent, and the specific surface area is about 27m by using an X-ray diffractometer2Single crystal rulerInch, 25 nm.
Example 5
By using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As a raw material, N2+∶Al3+∶NH2CONH2Preparing a solution according to the mol ratio of 1: 2: 6.67, and putting the solution into a furnace with the temperature of 400 ℃ for combustion synthesis. The purity of the obtained product is 96 percent, and the specific surface area is about 140m2G, single crystal size 11 nm.
Example 6
By using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As a raw material, N2+∶Al3∶NH2CONH2Preparing solution at molar ratio of 1: 2: 5, placing in a furnace at 800 deg.C to obtain product with purity of 97%, and adding XThe specific surface area measured by a ray diffractometer is about 10m2G, single crystal size 40 nm.
Example 7
By using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As raw materials,according to molar ratio N2+∶Al3∶NH2CONH2Preparing a solution at a ratio of 1: 2: 8, placing the solution in an oven at 370 deg.C to obtain a product with a purity of 96%, and measuring the specific surface area of about 100m with an X-ray diffractometer2G, single crystal size 20 nm.
Example 8 use of Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As raw materials, according to molar ratio N2+∶Al3∶NH2CONH2Preparing a solution at a ratio of 1: 2: 8, placing the solution in an oven at a temperature of 800 ℃ to obtain a product with a purity of 98.2%, and measuring the specific surface area of about 10m by an X-ray diffractometer2In terms of a single crystal size of 50 nm/g.
Comparative example 1 Using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As raw materials, according to molar ratio N2+∶Al3∶NH2CONH2Preparing solution at the ratio of 1: 2: 8, putting the solution into a furnace at the temperature of 350 ℃ to obtain amorphous NiO and Al serving as products2O3。
Comparative example 2 Using Ni (NO)3·6H2O，Al(NO3)3·9H2O and NH2CONH2As raw materials, according to molar ratio N2+∶Al3∶NH2CONH2Preparing a solution according to the ratio of 1: 2: 5, putting the solution into a furnace at the temperature of 350 ℃ to obtain NiO and Al with amorphous products2O3。
TABLE 1 partial NiAl2O4Purity, specific surface area and single crystal size of the product
Purity specific surface area product single crystal size
Preheating temperature
(％) (m2/g) (nm)
400 95.6 139.52 11.3
500 97.1 27.11 24.8
600 97.6 9.6 40.8
700 97.8 11.82 40.8
800 98.1 8.51 47.2
In the embodiments of the invention, the mixed liquid is heated by using the heating furnace to initiate spontaneous combustion, but the heating ignition method is not limited to the heating furnace, and various rapid heating methods such as input electric heater heating, various flame heating, microwave heating, electromagnetic heating, laser heating, infrared heating and the like can also achieve the same purpose.
Claims (3)
1. NiAl2O4Combustion synthesis of spinel powderThe method is characterized in that: the NiAl is synthesized by adopting a liquid-phase combustion synthesis method and urea as a fuel2O4The spinel powder is prepared by the following steps:
1) mixing nitrate containing Ni and Al and urea with Ni2+∶Al3+∶NH2CONH21: 2: 3-10 mol ratio;
2) dissolving the raw materials into distilled water, and uniformly stirring to prepare a saturated solution;
3) the crucible containing the mixed solution is placed into a heating furnace preheated to the temperature of 370-2O4A product;
4) rolling crushed the foam-like combustion synthetic product and sieving to obtain the final product NiAl2O4And (3) powder.
2. The NiAl of claim 12O4The combustion synthesis method of the spinel powder is characterized by comprising the following steps: the nitrate containing Ni and the nitrate containing Al respectively adopt Ni (NO)3·6H2O and Al (NO)3)3·9H2The molar ratio of O, nitrate and urea is Ni2+∶Al3+∶NH2CONH2＝1∶2∶5～8。
3. The NiAl of claim 12O4The combustion synthesis method of the spinel powder is characterized by comprising the following steps: the preheating temperature range of the heating furnace is 500-800 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427380C (en) * | 2005-06-08 | 2008-10-22 | 北京化工大学 | Process for preparing high radio surface area nano spinel by lamellar precursor body method |
| CN102161001A (en) * | 2011-03-14 | 2011-08-24 | 上海大学 | Preparation method of mesoporous NiAl10O16 material with regular pore diameter distribution |
| CN101580279B (en) * | 2009-06-24 | 2011-09-21 | 中国铝业股份有限公司 | Preparation method of NiAl2O4 nano-powder |
| CN102649590A (en) * | 2012-05-04 | 2012-08-29 | 上海大学 | Method for preparing mesoporous material NiAl2O4 without specific surface active agent |
| EP3067323A1 (en) * | 2015-03-10 | 2016-09-14 | Tallinn University of Technology | Method for producing nanofibers composed of nio and nial2o4 as well as product comprising said nanofibers |
| CN108636413A (en) * | 2018-05-02 | 2018-10-12 | 太原理工大学 | Nickel aluminate catalyst and preparation method thereof |
-
2004
- 2004-01-06 CN CN 200410000054 patent/CN1238244C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427380C (en) * | 2005-06-08 | 2008-10-22 | 北京化工大学 | Process for preparing high radio surface area nano spinel by lamellar precursor body method |
| CN101580279B (en) * | 2009-06-24 | 2011-09-21 | 中国铝业股份有限公司 | Preparation method of NiAl2O4 nano-powder |
| CN102161001A (en) * | 2011-03-14 | 2011-08-24 | 上海大学 | Preparation method of mesoporous NiAl10O16 material with regular pore diameter distribution |
| CN102161001B (en) * | 2011-03-14 | 2012-08-08 | 上海大学 | Preparation method of mesoporous NiAl10O16 material with regular pore diameter distribution |
| CN102649590A (en) * | 2012-05-04 | 2012-08-29 | 上海大学 | Method for preparing mesoporous material NiAl2O4 without specific surface active agent |
| CN102649590B (en) * | 2012-05-04 | 2014-07-30 | 上海大学 | Method for preparing mesoporous material NiAl2O4 without specific surface active agent |
| EP3067323A1 (en) * | 2015-03-10 | 2016-09-14 | Tallinn University of Technology | Method for producing nanofibers composed of nio and nial2o4 as well as product comprising said nanofibers |
| CN108636413A (en) * | 2018-05-02 | 2018-10-12 | 太原理工大学 | Nickel aluminate catalyst and preparation method thereof |
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