CN105417570A - Method for preparing spinel-type complex oxide through co-precipitation, homogenization and spray drying - Google Patents
Method for preparing spinel-type complex oxide through co-precipitation, homogenization and spray drying Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000000975 co-precipitation Methods 0.000 title claims abstract description 13
- 238000001694 spray drying Methods 0.000 title abstract description 4
- 238000000265 homogenisation Methods 0.000 title abstract 2
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000010009 beating Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims description 25
- 238000005507 spraying Methods 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 9
- 239000003637 basic solution Substances 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 230000029087 digestion Effects 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical group CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052596 spinel Inorganic materials 0.000 abstract description 9
- 239000011029 spinel Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract 2
- 239000012670 alkaline solution Substances 0.000 abstract 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 150000002823 nitrates Chemical class 0.000 abstract 1
- 239000000047 product Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 229910015645 LiMn Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000035800 maturation Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 235000014653 Carica parviflora Nutrition 0.000 description 1
- 241000243321 Cnidaria Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910003266 NiCo Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004033 diameter control Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 238000005839 oxidative dehydrogenation reaction Methods 0.000 description 1
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005287 template synthesis Methods 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention belongs to the field of chemical engineering and relates to a preparation method of a spinel type material, in particular to a method for preparing a spinel-type complex oxide through co-precipitation, homogenization and spray drying. According to the method, a mixed solution of two metallic nitrates and an alkaline solution are combined and added to a precipitation tank for a reaction, an obtained material is washed by deionized water, filtered, subjected to beating and refined by a homogenizer and then is sent to a spray drying machine, the dried material is subjected to calcination, and the spinel-type complex oxide powder is obtained. The method has the advantages of low calcination temperature, short time and low energy consumption, and a product has low loss, high purity and small particle size.
Description
Technical field
The invention belongs to chemical field, relate to a kind of preparation method of spinel type materials, be specially the method that co-precipitation-homogeneous-spraying dry prepares spinelle type composite oxides.
Background technology
The chemical general formula of spinelle type composite oxides is AB
2o
4, in formula, A is mostly divalent cation, and B is mostly Tricationic, and A, B can be identical.Spinelle type composite oxides is widely used as catalysis, fire-resistant and Conversion of energy and storage medium due to the high-temperature stability of its excellence and physical strength, the traditional method preparing this kind of material mainly contains: (1) mechanical mixing, such as: South China Science & Engineering University is disclosed a kind of for the preparation of lithium ion battery negative material LiMn
2o
4high temperature solid-state method (CN103904321A), need by lithium source and manganese source through twice continuous ball milling (6h-12h), calcine (500 DEG C-1000 DEG C), the LiMn that the method is obtained
2o
4there is excellent lithium ion battery negative material performance; (2) coprecipitation method, such as M.M.Rashad etc. are at " AnovelapproachforsynthesisofnanocrystallineMgAl
2o
4powdersbyco-precipitationmethod " (JournalofMaterialScience; 2009; Vol.44, pp.2992-2998) report respectively with organic bases tetraethyl ammonium and oxine be precipitation agent, adopt coprecipitation method, prepare nanometer MgAl at 600 DEG C-1000 DEG C roasting 2h
2o
4the research of spinel powder; (3) sol-gel method, such as: WuYQ etc. are at " Sol-gelapproachforcontrollablesynthesisandelectrochemica lpropertiesofNiCo
2o
4crystalsaselectrodematerialsforapplicationincapacitors " (ElectrochimicaActa, 2011, Vol.56 (21), pp.7517-7522) report the NiCo prepared by sol-gel method
2o
4class coral submicron particles shows excellent electrochemical capacitor performance; (4) hydrothermal synthesis method, such as: PengC etc. are at " OpticalandphotocatalyticpropertiesofspinelZnCr
2o
4nanoparticlessynthesizedbyahydrothermalroute " (JournalofAmericanCeramicSociety; 2008; Vol.91 (7), pp.2388-2399) report and prepared ZnCr through hydrothermal crystallizing 48h in enclosed high pressure reactor
2o
4nano-powder, this material exhibits goes out good photocatalysis performance; (5) vapour deposition process, such as: Gao Bo etc. are at " Si base AAO template synthesis spinel type ZnAl
2o
4nanostructure " (luminous journal, 2011, Vol.32 (12), pp.1243-1246) report and prepared ZnAl with vapour deposition process at 800 DEG C
2o
4nanotube, this material can increase substantially photocatalysis efficiency.
In the above-mentioned methods, when mechanical mixing prepares spinel, because raw material is difficult to mix, can not fully contact solid solution reaction occurs between thing phase, therefore product component heterogeneity, purity be not high, granularity is comparatively large, and maturing temperature is high simultaneously; In coprecipitation method easily there is solute segregation phenomenon in material when conventional oven dry, and product component heterogeneity, purity can be caused equally not high, and the method also exists the high problem of maturing temperature; Sol-gel method forms uniform and stable gel needs the long period, and the colloid of formation is not easy to washing, and maturing temperature is also higher; Hydrothermal Synthesis spinel needs the crystallization long period in the reactor of certain pressure, and preparation cycle is long, is not suitable for large-scale industrial production; Vapour deposition process needs to add heat-flash to material, and energy consumption is higher, and there is the deficiency that loss of material is serious, product yield is low.
Southwest Research & Design Institute of Chemical Industry Co., Ltd. patent CN102755897A discloses a kind of method that multiple step coprecipitation-spraying dry prepares copper-based methanol Oxidative Dehydrogenation methyl-formiate catalyzer, but there is not yet up to now about the report adopting co-precipitation, homogeneous, spraying dry recombining process prepare spinelle type composite oxides.
Summary of the invention
The object of the invention is to the deficiency avoiding conventional preparation techniques, a kind of co-precipitation-homogeneous-spraying dry is provided to prepare the method for spinelle type composite oxides, the method energy consumption is low, the cycle is short, product yield is high, each segment process technology maturation, is applicable to continuous, large-scale industrial production.
The object of the invention is realized by following technical proposals:
Co-precipitation-homogeneous-spraying dry prepares the method for spinelle type composite oxides, specifically comprise the following steps: first the salts solution of metal A, B and basic solution are carried out coprecipitation reaction under certain condition, gained material uses the deionized water wash of certain temperature, making beating, filtration again, clarifixator is utilized to carry out thinning processing to slurry after foreign matter content is up to standard, then carry out spraying dry to it under appropriate conditions, the roasting finally by certain condition obtains spinelle type composite oxides.
Described metal A is Mg, Mn, Fe, Co, Ni, Zn, Cu, Cd or Li, metal B is Al, Cr, Fe, Co, Mn, In or Ga, the salts solution of metal A and metal B is nitrate or acetate solution, and in raw material, metal A is 1:2 with the ratio of the amount of substance of metal B, and basic solution is Na
2cO
3or NaHCO
3solution.
The condition of described coprecipitation reaction is: temperature 55 DEG C-90 DEG C, pH value 6.0-8.5, stirring velocity 100r/min-1000r/min, digestion time 30min-60min.
The deionized water wash of described use certain temperature, making beating, filtration, its temperature is 60 DEG C-100 DEG C, and single wash amount of deionized water used is 2 times-8 times of filter cake volume, and washing times is 2 times-5 times.
Described foreign matter content is up to standard refers to Na in filtrate
+massfraction be 10ppm-110ppm.
The gap of described clarifixator is 100 μm-800 μm, and the number of times of homogeneous is 1 time-3 times, and amount of deionized water needed for single is 2 times-5 times of filter cake volume.
Described spray-dired inlet temperature is 200 DEG C-280 DEG C, and nozzle diameter is 150 μm-900 μm.
The condition of described roasting is: temperature 600 DEG C-900 DEG C, roasting time 1.0h-5.0h.
Compared with prior art, beneficial effect of the present invention is:
(1), meticulous, sufficient coprecipitation technology can realize raw material in the contact of molecule level, collision, not easily unevenly producing heterogeneous presoma because mixing, ensure that homogeneous, high-purity spinel products.
(2), the high speed rotating of clarifixator rotor produces Strong shear power, between stator and rotor, reciprocal aquashear, friction, centrifugal extruding, liquid stream collision effect are amplified by narrow gap further simultaneously, add the repeatedly homogenizing process that material participates in, these all make the abundant refinement of product granular precursor, high dispersing.
(3), thermo-sensitivity liquid, suspension and viscous liquid can be atomized and in very short time, make it complete dehydration, granulation process simultaneously by spraying dry, because drying process completes instantaneously, not only greatly shorten the production cycle, the more important thing is that presoma component can not segregation, further ensure the homogeneity of product and high-purity property.In addition, spraying dry coordinates the atomizer of certain diameter can prepare particle in regular spherical, ultra-fine, high-ratio surface, can also by the particle diameter of adjustment atomizer diameter control spinel precursor powder.Further, dried material no longer needs fragmentation, screening, simplifies production process, shortens the production cycle.
(4), in conjunction with co-precipitation, homogeneous, spraying dry technical superiority separately reduce presoma-spinel crystal conversion temperature, shorten roasting time, reduce production energy consumption, ensure that product yield.
(5), co-precipitation-homogeneous-spray-drying process prepares spinelle type composite oxides each segment process technology maturation, energy consumption is low, the cycle is short, product is homogeneous, purity and yield high, to be applicable to continuously, large-scale industrial production.
Accompanying drawing explanation
(1), (3), (10) in Fig. 1, (13) are expressed as the X ray diffracting spectrum (XRD) of the spinelle type composite oxides prepared in embodiment 1,3,10,13.
The crystal phase structure of spinelle type composite oxides prepared by the present invention utilizes BruckerD8 type X-ray diffractometer to record, the spectrogram of the spinelle type composite oxides in Fig. 1 is identical with PowderDiffractionFile database, known accordingly, spinelle type composite oxides prepared by the present invention is pure pressed powder
Embodiment
All features disclosed in this specification sheets, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
Arbitrary feature disclosed in this specification sheets (comprising any accessory claim, summary), unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object.That is, unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.
Embodiment:
When preparing spinelle type composite oxides with co-precipitation-homogeneous-spraying dry, be that the metal A of 2:1 and the salts solution of metal B and basic solution are at certain precipitation temperature by the ratio of amount of substance, pH value, stirring velocity, coprecipitation reaction is carried out under digestion time, gained material uses certain temperature again, appropriate deionized water wash, making beating, filter several times, being added by slurry after foreign matter content is up to standard is provided with in the clarifixator of certain interval, to the certain number of times of slurry thinning processing, then leave in suitable inlet temperature and nozzle chi and spraying dry is carried out to it, finally obtain spinelle type composite oxides in suitable atmosphere and roasting temperature for some time.
The preparation technology of embodiment of the present invention 1-17 is the same, and the concrete technology condition of 17 kinds of spinelle type composite oxides of preparation is listed in table 1.
The preparation process condition of table 1 embodiment 1-17
The present invention is not limited to aforesaid embodiment.The present invention expands to any new feature of disclosing in this manual or any combination newly, and the step of the arbitrary new method disclosed or process or any combination newly.
Claims (8)
1. co-precipitation-homogeneous-spraying dry prepares the method for spinelle type composite oxides, it is characterized in that comprising the following steps: first the salts solution of metal A, B and basic solution are carried out coprecipitation reaction under certain condition, gained material uses the deionized water wash of certain temperature, making beating, filtration again, clarifixator is utilized to carry out thinning processing to slurry after foreign matter content is up to standard, then carry out spraying dry to it under appropriate conditions, the roasting finally by certain condition obtains spinelle type composite oxides.
2. co-precipitation-homogeneous-spraying dry according to claim 1 prepares the method for spinelle type composite oxides, it is characterized in that: described metal A is Mg, Mn, Fe, Co, Ni, Zn, Cu, Cd or Li, metal B is Al, Cr, Fe, Co, Mn, In or Ga, the salts solution of metal A and metal B is nitrate or acetate solution, in raw material, metal A is 1:2 with the ratio of the amount of substance of metal B, and basic solution is Na
2cO
3or NaHCO
3solution.
3. co-precipitation-homogeneous-spraying dry prepares the method for spinelle type composite oxides according to claim 1, it is characterized in that the condition of described coprecipitation reaction is: temperature 55 DEG C-90 DEG C, pH value 6.0-8.5, stirring velocity 100r/min-1000r/min, digestion time 30min-60min.
4. co-precipitation-homogeneous-spraying dry prepares the method for spinelle type composite oxides according to claim 1, it is characterized in that: the deionized water wash of described use certain temperature, making beating, filtration, its temperature is 60 DEG C-100 DEG C, single wash amount of deionized water used is 2 times-8 times of filter cake volume, and washing times is 2 times-5 times.
5. co-precipitation-homogeneous-spraying dry prepares the method for spinelle type composite oxides according to claim 1, it is characterized in that: described foreign matter content is up to standard refers to Na in filtrate
+massfraction be 10ppm-110ppm.
6. co-precipitation-homogeneous-spraying dry prepares the method for spinelle type composite oxides according to claim 1, it is characterized in that: the gap of described clarifixator is 100 μm-800 μm, the number of times of homogeneous is 1 time-3 times, and amount of deionized water needed for single is 2 times-5 times of filter cake volume.
7. co-precipitation-homogeneous-spraying dry prepares the method for spinelle type composite oxides according to claim 1, it is characterized in that: described spray-dired inlet temperature is 200 DEG C-280 DEG C, and nozzle diameter is 150 μm-900 μm.
8. co-precipitation-homogeneous-spraying dry prepares the method for spinelle type composite oxides according to claim 1, it is characterized in that the condition of described roasting is: temperature 600 DEG C-900 DEG C, roasting time 1.0h-5.0h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105854892A (en) * | 2016-04-13 | 2016-08-17 | 沈阳大学 | Preparation method of porous rod-shaped spinel structured catalyst |
| CN105949709A (en) * | 2016-06-22 | 2016-09-21 | 金华知产婺源信息技术有限公司 | Preparation method of pleonaste-containing artificial stone |
| CN106007480A (en) * | 2016-06-22 | 2016-10-12 | 金华知产婺源信息技术有限公司 | Preparation method of flame-retardant artificial stone containing pleonaste |
| CN106446356A (en) * | 2016-09-05 | 2017-02-22 | 广东工业大学 | Detection method and system of improvement point in spray drying technology |
| CN106732616A (en) * | 2016-11-29 | 2017-05-31 | 西南化工研究设计院有限公司 | A kind of catalyst for being suitable to extensive methanol synthesizer and preparation method thereof |
| CN107930644A (en) * | 2017-11-28 | 2018-04-20 | 西南化工研究设计院有限公司 | A kind of high-performance methanol synthesis catalyst and preparation method thereof |
| CN108057448A (en) * | 2016-11-07 | 2018-05-22 | 中国科学院大连化学物理研究所 | A kind of cinnamic acid selective hydrogenation prepares cinnamyl alcohol catalyst and its application |
| CN108264081A (en) * | 2016-12-30 | 2018-07-10 | 海门市源美美术图案设计有限公司 | A kind of aluminium oxide and oxidation carbon/carbon-copper composite material and preparation method thereof |
| CN108777302A (en) * | 2018-04-27 | 2018-11-09 | 中南大学 | NiCo2O4And preparation method and application |
| WO2020020039A1 (en) * | 2018-07-23 | 2020-01-30 | The University Of Hong Kong | Methods for manufacturing spinel-type ternary metal oxides as hole transport materials |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105854892B (en) * | 2016-04-13 | 2018-05-22 | 沈阳大学 | The preparation method of porous rodlike spinel structure catalyst |
| CN105854892A (en) * | 2016-04-13 | 2016-08-17 | 沈阳大学 | Preparation method of porous rod-shaped spinel structured catalyst |
| CN106007480B (en) * | 2016-06-22 | 2018-08-07 | 金华知产婺源信息技术有限公司 | A kind of preparation method of the fire retardant man-made stone containing magnesium aluminate spinel |
| CN109133722B (en) * | 2016-06-22 | 2021-07-20 | 杭州百维艾特卫浴有限公司 | Preparation method of artificial stone containing magnesium aluminate spinel |
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| CN105949709B (en) * | 2016-06-22 | 2018-11-13 | 金华知产婺源信息技术有限公司 | A kind of preparation method of the artificial stone containing magnesium aluminate spinel |
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| CN108057448B (en) * | 2016-11-07 | 2020-12-01 | 中国科学院大连化学物理研究所 | Catalyst for preparing cinnamyl alcohol by selective hydrogenation of cinnamyl aldehyde and application thereof |
| CN108057448A (en) * | 2016-11-07 | 2018-05-22 | 中国科学院大连化学物理研究所 | A kind of cinnamic acid selective hydrogenation prepares cinnamyl alcohol catalyst and its application |
| CN106732616B (en) * | 2016-11-29 | 2019-07-30 | 西南化工研究设计院有限公司 | A kind of catalyst and preparation method thereof suitable for extensive methanol synthesizer |
| CN106732616A (en) * | 2016-11-29 | 2017-05-31 | 西南化工研究设计院有限公司 | A kind of catalyst for being suitable to extensive methanol synthesizer and preparation method thereof |
| CN108264081A (en) * | 2016-12-30 | 2018-07-10 | 海门市源美美术图案设计有限公司 | A kind of aluminium oxide and oxidation carbon/carbon-copper composite material and preparation method thereof |
| CN107930644A (en) * | 2017-11-28 | 2018-04-20 | 西南化工研究设计院有限公司 | A kind of high-performance methanol synthesis catalyst and preparation method thereof |
| CN108777302A (en) * | 2018-04-27 | 2018-11-09 | 中南大学 | NiCo2O4And preparation method and application |
| CN108777302B (en) * | 2018-04-27 | 2019-08-30 | 中南大学 | NiCo2O4And preparation method and application |
| WO2020020039A1 (en) * | 2018-07-23 | 2020-01-30 | The University Of Hong Kong | Methods for manufacturing spinel-type ternary metal oxides as hole transport materials |
| CN112368430A (en) * | 2018-07-23 | 2021-02-12 | 香港大学 | Method for producing spinel-type ternary metal oxide as hole transport material |
| CN112368430B (en) * | 2018-07-23 | 2023-09-22 | 香港大学 | Method for producing spinel-type ternary metal oxide as hole transport material |
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