CN104907036A - Graded dandelion-flower-shaped ZnO-Al2O3 compound and preparation method therefor - Google Patents
Graded dandelion-flower-shaped ZnO-Al2O3 compound and preparation method therefor Download PDFInfo
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Abstract
The invention provides a graded dandelion-flower-shaped ZnO-Al2O3 compound and a preparation method therefor. The preparation method is mainly as follows: aluminum nitrate, aluminum potassium sulfate and urea are mixed and dissolved in deionized water, AlOOH is prepared through a hydrothermal reaction, and Al2O3 is obtained through calcination; Al2O3 is employed as a matrix and is mixed with zinc nitrate and urea, the mixture is placed in a baking oven, a reaction is carried out, natural cooling after the reaction is carried out, washing is carried out, drying is carried out, calcination is carried out and therefore a ZnO-Al2O3 compound is obtained. Characterization of XRD, SEM and TEM and the like of the structure and the morphology of the compound is carried out, and the graded dandelion-like structure of the compound can be observed through the TEM and the SEM. The performance of the compound is raised obviously compared with the performance, adsorbing methyl blue dyes, of single alumina and zinc oxide and the maximum adsorption quantity reaches 228.3mg/g.
Description
Technical field the present invention relates to a kind of burning compound and preparation method thereof.
Background technology zinc oxide is a kind of polyfunctional new inorganic material.Due to the granular of zinc oxide size, its specific area is sharply increased, thus produce a series of special physical effect.Meanwhile, zinc oxide shows tempting potential application foreground in problem such as the solution energy, environment etc., and the research of current zinc oxide and compound thereof has become the focus of research both at home and abroad.At present, the preparation of different shape zinc oxide material, zinc oxide and the preparation of composite thereof and the performance study of Zinc oxide-base composite and application is mainly concentrated on for the research of zinc oxide.For functional research of composite, especially about the compound of zinc oxide and zinc oxide thereof for the fresh understatement road of research of adsorptivity.
Along with the aggravation of environmental pollution, people more and more pay attention to the reparation problem of environment.Be generally by Dye Adsorption material as active carbon, biomaterial etc. carry out adsorption treatment for dyestuff waste liquid, but adsorption effect is remarkable, and with high costs.Therefore, seek to have efficient adsorption effect, the compound of cheap zinc oxide and zinc oxide thereof has huge potential using value for the protection of the research of Environmental security aspect.
Summary of the invention the object of the present invention is to provide a kind of flower-shaped ZnO-Al of classification dandelion with efficient adsorption effect, cheapness
2o
3compound and preparation method thereof.Aluminum nitrate, alum and urea proportioning are mainly produced Al by the present invention
2o
3, then Al
2o
3znO-Al is obtained after reacting in proportion with zinc nitrate, urea
2o
3compound.Obtained ZnO-Al
2o
3compound has higher degree of crystallinity and lamella hollow ball pattern, is similar to dandelion flower shape, for the research and development of New function material provide technical support.
The flower-shaped ZnO-Al of classification dandelion of the present invention
2o
3compound preparation method is as follows:
1. raw material:
Aluminum nitrate, alum, urea, deionized water, absolute ethyl alcohol and zinc nitrate (wherein the purity of aluminum nitrate, alum, urea, absolute ethyl alcohol and zinc nitrate is more than 99%).2. preparation method:
(1) Al
2o
3synthesis
By aluminum nitrate at 35 DEG C, alum and urea are by each material mol ratio, i.e. aluminum nitrate: alum: urea=2:1:3 ~ 2:1:5, be dissolved in deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is again in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, take out to be cooled to room temperature place 6h at 180 DEG C after, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, finally the reactant after washing is dried 12h at 80 DEG C, obtain AlOOH solid, AlOOH solid roasting 3h at 600 DEG C is obtained Al
2o
3,
(2) ZnO-Al is synthesized
2o
3compound
By the Al that step (1) obtains
2o
3each material mol ratio is pressed respectively, i.e. Al with zinc nitrate and urea
2o
3: zinc nitrate: urea=1:1:9 ~ 1:3:9 mixing, wherein Al
2o
3as reactive matrix, at 35 DEG C, add deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 100 ~ 140 DEG C, place 12 ~ 24h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, finally roasting 4h at 500 DEG C, obtains ZnO-Al
2o
3compound.
The present invention compared with prior art tool has the following advantages:
(1) by the flower-shaped ZnO-Al of classification dandelion synthesized by growth in situ method
2o
3compound, has higher degree of crystallinity and lamella hollow ball pattern, has enriched the research that metal composite pattern controls greatly.
(2) this synthetic method has feature simple and convenient, with low cost.
(3) to the ZnO-Al of preparation
2o
3compound carries out the Study on adsorption properties of methyl blue dye waste water, and this result of study shows that its adsorbance is up to 228.3mg/g, ZnO and Al
2o
3carry out separately its adsorbance of adsorption test and be respectively 59.12mg/g and 107.3mg/g, this further illustrates this compound and has good effectiveness to absorption methyl blue dye.Therefore, the present invention expands ZnO-Al
2o
3the range of application of compound, extends the functional research of burning compound.
Accompanying drawing explanation
Fig. 1 is the flower-shaped ZnO-Al of classification dandelion in the embodiment of the present invention 1
2o
3the x-ray diffractogram of powder of compound
Fig. 2 is Al in the embodiment of the present invention 1
2o
3transmission electron microscope photo figure.
Fig. 3 is the flower-shaped ZnO-Al of the embodiment of the present invention 1 classification dandelion
2o
3the transmission electron microscope photo figure of compound.
Fig. 4 is the flower-shaped ZnO-Al of the embodiment of the present invention 1 classification dandelion
2o
3the stereoscan photograph figure of compound.
Detailed description of the invention
Embodiment 1:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:4 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.42042g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
35.9498g zinc nitrate, 1.02gAl is taken with the ratio of urea 2:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 120 DEG C, place 18h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.Accompanying drawing 1 is ZnO-Al
2o
3the XRD spectra of compound, this compound meets the standard card (PDF#36-1451) of ZnO substantially, and 2 θ are at 45 ° simultaneously, and about 66 ° is Al
2o
3diffraction maximum.Accompanying drawing 2 ~ 4 illustrates that the pattern of this compound is dandelion flower-like structure.
The research of adsorbing methyl blue dye is carried out to this compound, by 0.04gZnO-Al
2o
3compound absorption 50mL variable concentrations (100,120,140,160,180,200mg/L) methyl blue solution, Static Adsorption 24h under room temperature, after reaching balance, under the rotating speed of 1000r/min, centrifugal 15min, gets supernatant, then measures its absorbance with visible spectrophotometer, be balanced concentration according to calibration curve, result shows that its adsorbance is 228.3mg/g.Under equal experiment condition, the adsorbance of ZnO is 59.12mg/g, Al
2o
3adsorbance be 107.3mg/g.
Embodiment 2:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:4 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.42042g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
32.9749g zinc nitrate, 1.02gAl is taken with the ratio of urea 1:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 120 DEG C, place 18h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.
Carry out the research of adsorbing methyl blue dye to this compound, result shows that its adsorbance is 178.2mg/g.
Embodiment 3:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:4 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.42042g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
38.9247g zinc nitrate, 1.02gAl is taken with the ratio of urea 3:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 120 DEG C, place 18h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.
Carry out the research of adsorbing methyl blue dye to this compound, result shows that its adsorbance is 189.6mg/g.
Embodiment 4:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:4 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.42042g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
35.9498g zinc nitrate, 1.02gAl is taken with the ratio of urea 2:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 100 DEG C, place 24h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.Carry out the research of adsorbing methyl blue dye to this compound, result shows that its adsorbance is 120.2mg/g.
Embodiment 5:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:4 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.42042g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
35.9498g zinc nitrate, 1.02gAl is taken with the ratio of urea 2:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 140 DEG C, place 12h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.Carry out the research of adsorbing methyl blue dye to this compound, result shows that its adsorbance is 147.7mg/g.
Embodiment 6:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:5 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.52552g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
32.9749g zinc nitrate, 1.02gAl is taken with the ratio of urea 1:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 100 DEG C, place 24h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.
Carry out the research of adsorbing methyl blue dye to this compound, result shows that its adsorbance is 96.48mg/g.
Embodiment 7:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:5 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.52552g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
38.9247g zinc nitrate, 1.02gAl is taken with the ratio of urea 3:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 140 DEG C, place 12h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.Carry out the research of adsorbing methyl blue dye to this compound, result shows that its adsorbance is 105.2mg/g.
Embodiment 8:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:3 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.31532g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
38.9247g zinc nitrate, 1.02gAl is taken with the ratio of urea 3:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 140 DEG C, place 12h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.Carry out the research of adsorbing methyl blue dye to this compound, result shows that its adsorbance is 74.52mg/g.
Embodiment 9:
By aluminum nitrate at 35 DEG C, alum and urea in molar ratio 2:1:3 take 1.1817g aluminum nitrate, 0.71157g and alum, 0.31532g urea is dissolved in 100mL deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, 6h is placed at 180 DEG C, be cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and removes impurity more than 3 times, 12h is dried at 80 DEG C, obtain AlOOH solid, AlOOH is obtained Al at 600 DEG C of roasting 3h
2o
3.
Get the Al that previous step is obtained
2o
3, by zinc nitrate, Al
2o
32.9749g zinc nitrate, 1.02gAl is taken with the ratio of urea 1:1:9 in molar ratio
2o
3with 5.4054g urea, wherein Al
2o
3as reactive matrix, at 35 DEG C, add 100mL deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 100 DEG C, place 24h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are replaced washing and remove impurity more than 3 times, at 80 DEG C, dry 12h, last at 500 DEG C of roasting 4h, obtain ZnO-Al
2o
3compound.Carry out the research of adsorbing methyl blue dye to this compound, result shows that its adsorbance is 109.5mg/g.
Claims (3)
1. the flower-shaped ZnO-Al of classification dandelion
2o
3compound, is characterized in that: it is the Al synthesized by aluminum nitrate, alum and urea
2o
3what obtain after reacting in proportion with zinc nitrate and urea has the ZnO-Al that higher degree of crystallinity and lamella hollow ball pattern are similar to dandelion flower shape
2o
3compound.
2. the flower-shaped ZnO-Al of classification dandelion of claim 1
2o
3the preparation method of compound, is characterized in that:
1) Al
2o
3synthesis
At 35 DEG C by aluminum nitrate, alum and urea in molar ratio 2:1:3 ~ 2:1:5 mix, be dissolved in deionized water for stirring, ultrasonic disperse 15min, proceeding to liner is again in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, take out to be cooled to room temperature place 6h at 180 DEG C after, the white solid deionized water of generation and absolute ethyl alcohol are alternately washed minimum 3 times and removes impurity, finally the reactant after washing is dried 12h at 80 DEG C, obtain AlOOH solid, AlOOH solid roasting 3h at 600 DEG C is obtained Al
2o
3;
2) ZnO-Al is synthesized
2o
3compound
By the Al that step (1) obtains
2o
3distinguish 1:1:9 ~ 1:3:9 in molar ratio with zinc nitrate and urea to mix, wherein Al
2o
3as reactive matrix, at 35 DEG C, add deionized water and stirring 30min form uniform white suspension, then proceeding to liner is in the stainless steel cauldron of polytetrafluoroethylene (PTFE), the reactor of good seal is put into baking oven, at 100 ~ 140 DEG C, place 12 ~ 24h, after being cooled to room temperature, the white solid deionized water of generation and absolute ethyl alcohol are alternately washed minimum 3 times and remove impurity, at 80 DEG C, dry 12h, finally roasting 4h at 500 DEG C, obtains ZnO-Al
2o
3compound.
3. aluminum nitrate according to claim 2, alum, urea, absolute ethyl alcohol, its purity of zinc nitrate are more than 99%.
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| CN105540641A (en) * | 2016-01-30 | 2016-05-04 | 湘潭大学 | Method for preparing flower-like microspheric magnesium doped zinc oxide material |
| CN107020055A (en) * | 2017-06-10 | 2017-08-08 | 安徽工程大学 | A kind of SiO2The preparation method and applications of@ZnO core shell structure polypody bead nano composite materials |
| CN108735517A (en) * | 2018-05-30 | 2018-11-02 | 大连交通大学 | A kind of basic zinc carbonate electrode material for super capacitor and preparation method thereof |
| CN116351407A (en) * | 2023-03-23 | 2023-06-30 | 天津科技大学 | Petal-shaped alpha-Al 2 O 3 Preparation method and application of carrier and silver-loaded catalyst |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105540641A (en) * | 2016-01-30 | 2016-05-04 | 湘潭大学 | Method for preparing flower-like microspheric magnesium doped zinc oxide material |
| CN107020055A (en) * | 2017-06-10 | 2017-08-08 | 安徽工程大学 | A kind of SiO2The preparation method and applications of@ZnO core shell structure polypody bead nano composite materials |
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| CN116351407A (en) * | 2023-03-23 | 2023-06-30 | 天津科技大学 | Petal-shaped alpha-Al 2 O 3 Preparation method and application of carrier and silver-loaded catalyst |
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