CN102500298A - Preparation method of metal oxides and composite microspheres of metal oxides - Google Patents

Preparation method of metal oxides and composite microspheres of metal oxides Download PDF

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CN102500298A
CN102500298A CN2011103766856A CN201110376685A CN102500298A CN 102500298 A CN102500298 A CN 102500298A CN 2011103766856 A CN2011103766856 A CN 2011103766856A CN 201110376685 A CN201110376685 A CN 201110376685A CN 102500298 A CN102500298 A CN 102500298A
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microballoon
metal oxide
preparation
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metal oxides
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黄驰
张依福
刘兴海
樊美娟
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Wuhan University WHU
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Abstract

The invention discloses a preparation method of metal oxides and composite microspheres of the metal oxides, which comprises the following steps of: taking any one or more of metal oxides or metal hydroxides or salt containing metal elements as an initial raw material; after the initial raw material is mixed with oxalic acid and water, placing into a high-pressure kettle reactor for reaction; after the end of reaction, naturally cooling and discharging; and after washing and vacuum drying, obtaining the different metal oxides and the composite microsphere of the metal oxides. The invention has the beneficial effects that the preparation method is simple in process, is easy in control, is good in process repeatability and is suitable for large-scale industrial production; a series of metal oxides and the composite microspheres of the metal oxides can be prepared by the method; and the obtained products have uniform appearance, respectively have a grain size of 1-5 micrometres, are rough in surface, respectively have a specific surface area of 89-125 m<2>/g, are larger in specific surface area and can be applied to the fields of catalysis, optics and the like.

Description

The preparation method of a kind of metal oxide and compound microballoon thereof
Technical field
The invention belongs to field of inorganic chemical engineering, relate in particular to the preparation method of a kind of metal oxide and compound microballoon thereof.
Background technology
In the periodic table of elements, metallic element approximately occupies 4/5.In daily life, metal oxide is widely used.For example: quick lime (CaO) is a kind of drier commonly used, also can be used for sterilization; Iron oxide (Fe 2O 3) be commonly called as iron oxide red, can make red pigment; Catalyst for application also is a metal oxide in some industrial process; The selective oxidation catalyst that uses in the industry mostly is made up of multiple metal oxide, and these oxides can be solid solution or composite oxides.
Along with the development of science and technology with information technology, also just more and more to the functional requirement of material, and a lot of metal oxide just has some special function.Like TiO 2Have functions such as unique photo catalysis, excellent colour effect and ultraviolet screener, have broad application prospects at aspects such as photochemical catalyst, cosmetics, ultraviolet-resistant absorbent, function ceramics, gas-sensitive sensor devices.V 2O 3And VO 2Material has excellent optics, electricity, magnetic property, thereby they are with a wide range of applications in fields such as thermistor material, photoelectric switch material, smart window material, intelligent temperature control material, infrared acquisition material, nonlinear resistance material, gas sensor, anti-laser material, optical memory materials.Therefore, metal oxide materials is by scientific research personnel's extensive studies, and some metal oxide special nature also it is found that gradually and are applied.
For same material, if make up different patterns, this material can show different chemistry and physical property, some novel characteristics also might occur.Along with raising, the people of the development of society, industrial level increase what the material specific function required, make the scientific research personnel to the in addition detailed research of having to of composition, structure and the pattern etc. of material.Also emerge in an endless stream for preparation methods at present, but these methods generally all are a kind of material of preparation or different materials, and the method for preparing a series of same type of material is not simultaneously also arranged.
Summary of the invention
The object of the present invention is to provide that a kind of process is simple, with low cost, the preparation method of the metal oxide and the compound microballoon thereof that are easy to control, be suitable for large-scale industrial production; Adopt the inventive method can prepare a series of metal oxides and compound microballoon thereof; Adopt the prepared microballoon of the inventive method to be of a size of the 1-5 micron; Rough surface has bigger specific area.
The inventive method is an initial feed with any or several kinds in the salt of metal oxide or metal hydroxides or containing metal element; Above-mentioned initial feed, oxalic acid and water mixed to be placed in the autoclave reactor react; After question response finishes; The nature cooling discharge after washing, vacuum drying, can obtain different metal oxides and compound microballoon thereof; Product after the vacuum drying, some crystal formation is bad or contain the crystallization water, can adopt the means of calcining to be optimized, and crystal formation is improved or loses the crystallization water, thereby obtain well-crystallized's metal oxide and compound microballoon thereof.The preparation method of a kind of metal oxide provided by the invention and compound microballoon thereof may further comprise the steps:
Step 1, the preparation oxalic acid aqueous solution;
Step 2 adds any or several kinds in the salt of metal oxide, metal hydroxides or containing metal element in the oxalic acid aqueous solution that step 1 prepares, and obtains reaction system through fully mixing;
Step 3; Step 2 gained reaction system is placed autoclave; React 0.5～96 h down for 150～300 ℃ in temperature, after question response is accomplished, after centrifugal, washing, vacuum drying; Can directly obtain metal oxide or its compound microballoon, or the product after the vacuum drying is obtained metal oxide or its compound microballoon through calcining.
The preferable range of the oxalic acid aqueous solution concentration in the step 1 is 0.01 mol/L～5.0 mol/L.
The total valent numerical value of reaction system medium-height grass acid group in the step 2 is not less than the total valent numerical value of metal cation.
Metal oxide in the step 2 is MgO, Al 2O 3, the oxide of the period 4 metallic element except that potassium, the oxide of the period 5 metallic element except that rubidium, technetium, ruthenium, the oxide of the lanthanide series except that promethium, BaO, HfO 2, WO 3, ReO 2, PtO 2, Tl 2O 3, PbO, Bi 2O 3In the mixture of any or several kinds.
Metal hydroxides in the step 2 is Mg (OH) 2, Al (OH) 3, Ca (OH) 2, VO (OH) 2, Cr (OH) 3, Mn (OH) 2, Fe (OH) 3, Co (OH) 3, Ni (OH) 2, Cu (OH) 2, Zn (OH) 2, Ga (OH) 3, Ge (OH) 2, Sr (OH) 2, Mo (OH) 4, Cd (OH) 2, Ba (OH) 2, the lanthanide series except that promethium hydroxide in the mixture of any or several kinds.
The salt of the containing metal element in the step 2 is MgCl 2, CaCO 3, CaC 2O 4, VO (Ac) 2, VOCl 2, VOCl 3, VOSO 4, CrCl 3, FeSO 4H 2O, Co (Ac) 2, CuSO 45H 2O, Zn (Ac) 2, ZnC 2O 4, Na 2MoO 4, (NH 4) 2MoO 4, (NH 4) 2WO 4, Na 2WO 4, BaC 2O 4In the mixture of any or several kinds.
Adopting the inventive method products therefrom is MgO, Al 2O 3, the oxide (except that potassium) of period 4 metallic element, the oxide (except that rubidium, technetium, ruthenium) of period 5 metallic element, BaO, HfO 2, WO 3, ReO 2, PtO 2, Tl 2O 3, PbO, Bi 2O 3Any or several kinds compound, and products therefrom all has unified microballoon pattern, particle diameter is the 1-5 micron.
 
The reaction mechanism of the inventive method is following:
Metal oxide and metal hydroxides can react with oxalic acid, produce corresponding oxalates, for example, and Fe 2O 3And Fe (OH) 3Can following reaction take place with oxalic acid:
Fe 2O 3?+?3H 2C 2O 4?→?Fe 2(C 2O 4) 3?+?3H 2O
2Fe(OH) 3?+?3H 2C 2O 4?→?Fe 2(C 2O 4) 3?+?6H 2O
The reaction of other metal oxide and metal hydroxides and oxalic acid and Fe 2O 3And Fe (OH) 3Similar.
For the salt of containing metal element, itself and oxalic acid do not react.Under 150～300 ℃ reaction temperature, oxalates in the reaction system or oxalic acid can decompose generation CO 2And CO, the gas of generation will be regulated the pattern of product, thereby can prepare metal oxide and compound microballoon thereof.
Compared with prior art, the inventive method has the following advantages and beneficial effect:
1, the raw material of the inventive method employing is simple, and solvent for use is a water, and environmental protection is cheap;
2, the inventive method technology simple, be easy to control, good process repeatability, be suitable for large-scale industrial production;
3, adopt the inventive method can prepare a series of metal oxides and compound microballoon thereof, products therefrom all has unified pattern, and particle diameter is the 1-5 micron, and rough surface, and specific area is 89-125m 2/ g has bigger specific area, can be used for fields such as catalysis, optics.
Description of drawings
Fig. 1 is embodiment 1 gained Fe 3O 4The SEM of microballoon (SEM) photo;
Fig. 2 is embodiment 2 gained Co 3O 4The SEM of microballoon (SEM) photo;
Fig. 3 is embodiment 3 gained VO 2The SEM of microballoon (SEM) photo;
Fig. 4 is embodiment 3 gained V 2O 3The SEM of microballoon (SEM) photo;
Fig. 5 is embodiment 4 gained CaC 2O 4The SEM of micro-sphere material (SEM) photo;
Fig. 6 is SEM (SEM) photo of embodiment 5 gained metal Cu microballoons;
Fig. 7 is embodiment 6 gained Al 2O 3The SEM of microballoon (SEM) photo;
Fig. 8 is embodiment 7 gained VO 2The SEM of micro-sphere material (SEM) photo;
Fig. 9 is embodiment 8 gained WO 3The SEM of microballoon (SEM) photo;
Figure 10 is embodiment 9 gained MoO 2The SEM of microballoon (SEM) photo;
Figure 11 is SEM (SEM) photo of embodiment 10 gained vanadium and chromium composite oxides microballoon;
Figure 12 is SEM (SEM) photo of embodiment 11 gained vanadium and tungsten composite oxides microballoon;
Figure 13 is embodiment 12 gained La 2O 3The SEM of microballoon (SEM) photo.
The specific embodiment
Below through specific embodiment technical scheme of the present invention is described further.
Embodiment 1
Compound concentration is the oxalic acid aqueous solution of 0.2 mol/L, with 0.48g block Fe 2O 3Join in the 40mL oxalic acid aqueous solution, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 24 h down in 260 ℃; Behind the nature cooling place material, after centrifugal, deionized water washing, vacuum drying, can obtain Fe 3O 4The microballoon product.Product is characterized by Fe through X-ray diffraction analysis (XRD) 3O 4Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 1 is present embodiment gained Fe 3O 4The SEM photo of microballoon; Product detects through specific area tester (BET), shows present embodiment gained Fe 3O 4Microballoon has bigger specific area, is 111 m 2/ g.With gained Fe 3O 4Microballoon in 300 ℃ of calcining 6 h, can obtain Fe in air 2O 3Microballoon.
Embodiment 2
Compound concentration is the oxalic acid aqueous solution of 0.2 mol/L, with 0.40g block Co 2O 3Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 12 h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain Co 3O 4The microballoon product.Product is characterized by Co through X-ray diffraction analysis (XRD) 3O 4Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 2 is present embodiment gained Co 3O 4The SEM photo of microballoon; Product detects through specific area tester (BET), shows present embodiment gained Co 3O 4Microballoon has bigger specific area, is 89 m 2/ g.With gained Co 3O 4Microballoon in 700 ℃ of calcining 2 h, can obtain Co in air 2O 3Microballoon.
Embodiment 3
Compound concentration is the oxalic acid aqueous solution of 0.2 mol/L, with 0.91 g block V 2O 5Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 0.5 h down in 300 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain VO 2The microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 3 is present embodiment gained VO 2The SEM photo of microballoon; Product detects through specific area tester (BET), shows present embodiment gained VO 2Microballoon has bigger specific area, is 95 m 2/ g.With gained VO 2Microballoon in 700 ℃ of calcining 2 h, can obtain V in inert atmosphere 2O 3Microballoon, Fig. 4 are gained V 2O 3The SEM of microballoon (SEM) photo.
Embodiment 4
Compound concentration is the oxalic acid aqueous solution of 0.2 mol/L, and 0.35 g block CaO is joined in the 40 mL oxalic acid aqueous solutions, obtains reaction system after the employing magnetic stirring apparatus fully stirs, and reaction system is transferred in the autoclave, and reacted 24 h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain CaC 2O 4The microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 5 is present embodiment gained CaC 2O 4The SEM photo of microballoon.With gained CaC 2O 4Microballoon in 1000 ℃ of calcining 2 h, can obtain the CaO microballoon in air atmosphere.
Embodiment 5
Compound concentration is the oxalic acid aqueous solution of 5mol/L, and 0.40 g block CuO is joined in the 40 mL oxalic acid aqueous solutions, obtains reaction system after the employing magnetic stirring apparatus fully stirs, and reaction system is transferred in the autoclave, and reacted 24 h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain metal Cu microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 6 is the SEM photo of present embodiment gained metal Cu microballoon.With gained metal Cu microballoon in air atmosphere in 500 ℃ the calcining 6 h, can obtain the CuO microballoon.
Embodiment 6
Compound concentration is the oxalic acid aqueous solution of 0.2mol/L, with 0.50 g block Al 2O 3Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 96 h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain AlO (OH) microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 7 is the SEM photo of present embodiment gained AlO (OH) microballoon.With gained AlO (OH) microballoon in air atmosphere in 400 ℃ the calcining 6 h, can obtain Al 2O 3Microballoon.
Embodiment 7
Compound concentration is the oxalic acid aqueous solution of 0.01mol/L, with 0.36 g block VO (Ac) 2Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 24 h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain VO 2The microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 8 is present embodiment gained VO 2The SEM photo of microballoon.
Embodiment 8
Compound concentration is the oxalic acid aqueous solution of 0.2mol/L, with 1.0 g block Na 2WO 4Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 12 h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain WO 3The microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 9 is present embodiment gained WO 3The SEM photo of microballoon.
Embodiment 9
Compound concentration is the oxalic acid aqueous solution of 0.2mol/L, with 1.5 g block (NH 4) 2MoO 4Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 24 h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain MoO 2The microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 10 is present embodiment gained MoO 2The SEM photo of microballoon.
Embodiment 10
Compound concentration is the oxalic acid aqueous solution of 0.2mol/L, with 0.38 g block Cr 2O 3With 0.45 g block V 2O 5Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 24 h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain VCrO 2The microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 11 is present embodiment gained VCrO 2The SEM photo of microballoon.
Embodiment 11
Compound concentration is the oxalic acid aqueous solution of 0.2mol/L, with 0.0464 g block WO 3With 0.8918 g block V 2O 5Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 36h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain V 0.98W 0.02O 2The microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 12 is present embodiment gained V 0.98W 0.02O 2The SEM photo of microballoon.
Embodiment 12
Compound concentration is the oxalic acid aqueous solution of 0.2mol/L, with 0.50 g block La 2O 3Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 24h down in 260 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain La 2O 3The microballoon product.Product is accredited as microspheroidal through SEM (SEM), and particle diameter is the 1-5 micron, and rough surface, and shown in Figure 13 is present embodiment gained La 2O 3The SEM photo of microballoon; Product detects through specific area tester (BET), shows present embodiment gained La 2O 3Microballoon has bigger specific area, is 125 m 2/ g.
Embodiment 13
Compound concentration is the oxalic acid aqueous solution of 0.2mol/L, with 0.91 g block V 2O 5Join in the 40 mL oxalic acid aqueous solutions, obtain reaction system after the employing magnetic stirring apparatus fully stirs, reaction system is transferred in the autoclave, and reacted 72h down in 150 ℃; Behind the nature cooling discharge, after centrifugal, deionized water washing, vacuum drying, can obtain VO 2The microballoon product.

Claims (6)

1. the preparation method of metal oxide and compound microballoon thereof is characterized in that, may further comprise the steps:
Step 1, the preparation oxalic acid aqueous solution;
Step 2 adds any or several kinds in the salt of metal oxide, metal hydroxides or containing metal element in the oxalic acid aqueous solution that step 1 prepares, and obtains reaction system through fully mixing;
Step 3; Step 2 gained reaction system is placed autoclave; React 0.5～96 h down for 150～300 ℃ in temperature, after question response is accomplished, after centrifugal, washing, vacuum drying; Can directly obtain metal oxide or its compound microballoon, or the product after the vacuum drying is obtained metal oxide or its compound microballoon through calcining.
2. the preparation method of metal oxide according to claim 1 and compound microballoon thereof is characterized in that:
Described oxalic acid aqueous solution concentration is 0.01 mol/L～5.0 mol/L.
3. the preparation method of metal oxide according to claim 1 and compound microballoon thereof is characterized in that:
The total valent numerical value of described reaction system medium-height grass acid group is not less than total valent numerical value of metal cation.
4. the preparation method of metal oxide according to claim 1 and compound microballoon thereof is characterized in that:
Described metal oxide is MgO, Al 2O 3, the oxide of the period 4 metallic element except that potassium, the oxide of the period 5 metallic element except that rubidium, technetium, ruthenium, the oxide of the lanthanide series except that promethium, BaO, HfO 2, WO 3, ReO 2, PtO 2, Tl 2O 3, PbO, Bi 2O 3In the mixture of any or several kinds.
5. the preparation method of metal oxide according to claim 1 and compound microballoon thereof is characterized in that:
Described metal hydroxides is Mg (OH) 2, Al (OH) 3, Ca (OH) 2, VO (OH) 2, Cr (OH) 3, Mn (OH) 2, Fe (OH) 3, Co (OH) 3, Ni (OH) 2, Cu (OH) 2, Zn (OH) 2, Ga (OH) 3, Ge (OH) 2, Sr (OH) 2, Mo (OH) 4, Cd (OH) 2, Ba (OH) 2, the lanthanide series except that promethium hydroxide in the mixture of any or several kinds.
6. the preparation method of metal oxide according to claim 1 and compound microballoon thereof is characterized in that:
The salt of described containing metal element is MgCl 2, CaCO 3, CaC 2O 4, VO (Ac) 2, VOCl 2, VOCl 3, VOSO 4, CrCl 3, FeSO 4H 2O, Co (Ac) 2, CuSO 45H 2O, Zn (Ac) 2, ZnC 2O 4, Na 2MoO 4, (NH 4) 2MoO 4, (NH 4) 2WO 4, Na 2WO 4, BaC 2O 4In the mixture of any or several kinds.
CN2011103766856A 2011-11-24 2011-11-24 Preparation method of metal oxides and composite microspheres of metal oxides Pending CN102500298A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838165A (en) * 2012-09-29 2012-12-26 黑龙江大学 Method for preparing WO3 multiporous micro beads
CN107519891A (en) * 2017-09-19 2017-12-29 常州大学 A kind of preparation method of ternary metal oxide catalyst
CN107930614A (en) * 2017-12-14 2018-04-20 聊城大学 A kind of Cd2Nb2O7/Cd(OH)2The preparation method of catalysis material
CN112397707A (en) * 2020-11-13 2021-02-23 何叶红 Porous VO for lithium ion battery2Microspheres and method for preparing same

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101428348A (en) * 2008-07-29 2009-05-13 张建玲 Process for producing spherical submicron metal with hydro-thermal treatment

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101428348A (en) * 2008-07-29 2009-05-13 张建玲 Process for producing spherical submicron metal with hydro-thermal treatment

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838165A (en) * 2012-09-29 2012-12-26 黑龙江大学 Method for preparing WO3 multiporous micro beads
CN107519891A (en) * 2017-09-19 2017-12-29 常州大学 A kind of preparation method of ternary metal oxide catalyst
CN107930614A (en) * 2017-12-14 2018-04-20 聊城大学 A kind of Cd2Nb2O7/Cd(OH)2The preparation method of catalysis material
CN107930614B (en) * 2017-12-14 2020-06-05 聊城大学 Cd (cadmium)2Nb2O7/Cd(OH)2Preparation method of photocatalytic material
CN112397707A (en) * 2020-11-13 2021-02-23 何叶红 Porous VO for lithium ion battery2Microspheres and method for preparing same

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Application publication date: 20120620