CN105233787A - Preparation method and applications of Al2O3/TiO2 core-shell nano material - Google Patents
Preparation method and applications of Al2O3/TiO2 core-shell nano material Download PDFInfo
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- CN105233787A CN105233787A CN201510628017.6A CN201510628017A CN105233787A CN 105233787 A CN105233787 A CN 105233787A CN 201510628017 A CN201510628017 A CN 201510628017A CN 105233787 A CN105233787 A CN 105233787A
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- core
- nano material
- tio
- shell nano
- precipitate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention relates to a preparation method and applications of an Al2O3/TiO2 core-shell nano material. The preparation method comprises the following steps: synthesizing nano Al cores through a hydrolysis-precipitation method or a hydrothermal method; grinding the Al cores, dissolving Al cores into anhydrous ethanol, evenly stirring by a magnetic stirrer, at the same time, dropwise adding ammonia liquor and butyl titanate, stirring for 2 to 4 hours, then carrying out centrifugal separation, washing the obtained precipitate by deionized water until the precipitate becomes neutral, drying the precipitate at a temperature of 55 to 80 DEG C; grinding the dried precipitate, burning the precipitate in a muffle furnace for 2 to 3 hours at a temperature of 450 to 600 DEG C, and cooling to obtain the Al2O3/TiO2 core-shell nano material. The provided preparation method is simple, the conditions are mild, and the complicated technology of conventional preparation method is avoided. Al and Ti are successfully combined together to form core-shell nano particles with a better performance, and the decoloring efficiency of nano particles on dye wastewater is improved.
Description
Technical field
The invention belongs to technical field of material and water-treatment technology field, be specifically related to a kind of Al
2o
3/ TiO
2the method of its dye wastewater treatment of preparations and applicatio of core-shell nano material.
Background technology
Nuclear shell type nano meter particle be with a size at the spheric granules of micron to nano grade for core, at a kind of composite construction of its surface parcel several layers of even film, be interconnected by physics or chemical action between its center and shell.Hud typed composite nano materials integrates the character of core and shell, and can realize the regulation and control of composite performance by controlling its composition, thickness etc.The nano composite material of nucleocapsid structure has a lot of excellent character, has often both possessed the performance of stratum nucleare and Shell Materials, and has been different from again homogenous material wherein, and become the focus of people's research in recent years.According to TiO
2good optics, electric property and light transfer characteristic, hud typed TiO
2material can be used as the performance that the important source material such as high transparency toughness film, photoelectricity equipment, solar cell also improve them greatly.The TiO of nucleocapsid structure
2material, as sensitising agent, coating, ink addition agent, catalyst, magnetic material etc., has important application and wide prospect in fields such as electronics, chemical industry, environmental protection, food, medical science.
Due to TiO
2stability is high, acid-alkali-corrosive-resisting and have good catalytic activity, and Chang Zuowei shell is wrapped in other semiconductor material surface, prepares multi-functional composite.The preparation method of core-shell material is varied, mainly contains sedimentation, polymerization, in-situ reaction and self-assembling technique etc.In most cases, nucleocapsid structure can be obtained on the surface of core by the material of the Direct precipitation shells such as hydrolysis or redox reaction.But this method needs to consider the relevant nature between core and shell matter, such as the problems such as Lattice Matching.When can not directly wrap up, by the effect of coupling agent, core and shell can be coupled together, or adopt LBL self-assembling technique, the material alternating packets of different electric charge is wrapped on core.
Summary of the invention
The object of this invention is to provide a kind of Al
2o
3/ TiO
2core-shell nano material and preparation method thereof.
Another object of the present invention is to provide Al
2o
3/ TiO
2the application of core-shell nano material organic dyestuff in degrading waste water.
The technical solution used in the present invention is: a kind of Al
2o
3/ TiO
2core-shell nano material, its preparation method comprises the steps:
1) hydrolysis methods or hydrothermal synthesis method prepare nanometer Al core;
2) nanometer Al core is ground, be dissolved in absolute ethyl alcohol, uniform stirring on magnetic stirring apparatus, dropwise add ammoniacal liquor and butyl titanate simultaneously, stir after 2-4 hour, centrifugation, the deposit obtained is spent deionized water to neutral, dry at 55-80 DEG C;
3) ground by dried deposit, 450-600 DEG C of calcining 2-3h in Muffle furnace, cooling, obtains Al
2o
3/ TiO
2core-shell nano material.
Above-mentioned Al
2o
3/ TiO
2core-shell nano material, described hydrolysis methods prepares nanometer Al core: get alchlor, is dissolved in the water, and magnetic stirring apparatus fully stirs, dropwise add ammoniacal liquor, observe precipitation to produce, continued to add ammoniacal liquor and stop after fully producing precipitation, then in 25-65 DEG C of reaction 24h, centrifugal, get precipitation, by precipitate with deionized water washing to neutral, dry at 55-80 DEG C.
Above-mentioned Al
2o
3/ TiO
2core-shell nano material, described hydrothermal synthesis method prepares nanometer Al core: get alchlor, be dissolved in the water, after dropwise adding ammoniacal liquor, be placed in the hydrothermal reaction kettle of polytetrafluoroethylliner liner, 4-6 hour is reacted at 120-160 DEG C, cooling, centrifugal, get precipitation, by precipitate with deionized water washing to neutral, dry at 55-80 DEG C.
Above-mentioned Al
2o
3/ TiO
2the application of core-shell nano material organic dyestuff in degrading waste water.Method is as follows: the initial concentration regulating organic dyestuff in wastewater is 10-500mg/L, and pH value is 2-9, adds above-mentioned Al
2o
3/ TiO
2core-shell nano material.
The invention has the beneficial effects as follows: the inventive method is simple, and mild condition, avoids the complicated technology of customary preparation methods.This bi-material of Al and Ti successfully combines by the present invention, forms the core-shell structure nanometer particle stronger compared with homogenous material character, enhances the decolorizing efficiency of nano particle to waste water from dyestuff.
Accompanying drawing explanation
Fig. 1 is the Al that embodiment 1 utilizes hydrolysis methods to prepare
2o
3/ TiO
2the infrared spectrogram of core-shell nano material.
Fig. 2 is the Al that embodiment 1 utilizes hydrolysis methods to prepare
2o
3/ TiO
2titanium dioxide prepared by core-shell nano material and butyl titanate removes the Contrast on effect of pacifying the dark blue L-3G of promise element.
Fig. 3 is the Al that embodiment 2 utilizes hydro-thermal method to prepare
2o
3/ TiO
2titanium dioxide prepared by core-shell nano material and butyl titanate removes the Contrast on effect of reactive brilliant red x-3b.
Fig. 4 is the Al that embodiment 1 utilizes hydrolysis methods to prepare
2o
3/ TiO
2core-shell nano material is for the clearance of pacifying the dark blue L-3G of promise element under different pH condition.
Detailed description of the invention
Embodiment 1 one kinds of Al
2o
3/ TiO
2core-shell nano material
(1) preparation method is as follows:
1) hydrolysis methods prepares nanometer Al core: the alchlor taking 31.4g, is dissolved in 30ml water, magnetic stirring apparatus fully stirs, dropwise add ammoniacal liquor, has observed precipitation and has produced, and continues to add ammoniacal liquor until stop after fully producing precipitation.By above-mentioned precipitation and liquid as after 45 DEG C of reaction 24h in thermostat water bath, centrifugation, by centrifugal obtained precipitation, spends deionized water to neutral, dry in 70 DEG C of drying boxes, obtains nanometer Al core.
2) 0.75g nanometer Al core is ground, be dissolved in 100ml absolute ethyl alcohol, uniform stirring on magnetic stirring apparatus, dropwise add 4ml ammoniacal liquor and 4ml butyl titanate simultaneously, stir after 2 hours, centrifugation, spends deionized water to neutral by the deposit obtained, dry in 55 DEG C of drying boxes.
3), after being ground by dried deposit, calcine 2 hours for 550 DEG C in Muffle furnace, cooling, obtains Al
2o
3/ TiO
2core-shell nano material.
Al
2o
3/ TiO
2the infrared spectrum of core-shell nano material as shown in Figure 1, as seen from Figure 1,3444.7cm
-1and 1641.79cm
-1for in Ti-OH and Al-OH and the stretching vibration of material surface physical bond water-OH.Under normal circumstances, the symmetrical peak peak position of the bending vibrations of Al-O-Al appears at 1073cm
-1, the antisymmetry acromion of bending vibrations appears at 1163cm
-1, the stretching vibration of Al-O appears at 500-750cm
-1.Al-O-Al appears at 563cm
-1, Ti-O-Ti appears at 615cm
-1, Ti-O-Al appears at 583cm
-1and 439cm
-1.And 406-1366cm in Fig. 1
-1between region but there is a roomy peak, be the result because the coated process of shell core causes the characteristic peak of above-mentioned various Typical groups mutually to cover.
(2) apply
Method: be respectively in the dark blue L-3G solution of peace promise element of 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L in 100ml concentration, add 0.1gAl
2o
3/ TiO
2core-shell nano material, regulates its pH value to be 6.0 with HCl and NaOH, and take out after shaking 24 hours in oscillator, centrifugation, gets supernatant liquor, adopts UV-VIS spectrophotometry to measure remaining dye strength, calculates clearance.Result is as shown in table 1 and Fig. 2.
Table 1
| Concentration mg/L | 10 | 20 | 30 | 40 | 50 |
| Clearance (Al 2O 3/TiO 2)％ | 99.5 | 97.3 | 99.8 | 99.5 | 98 |
| Clearance (TiO 2)％ | 35 | 14 | 15 | 18 | 12 |
From table 1 and Fig. 2, compared with the titanium dioxide of tetrbuty titanate synthesis, Al
2o
3/ TiO
2core-shell material is for pacifying the clearance of the dark blue L-3G of promise element far away higher than titanium dioxide.
Embodiment 2 one kinds of Al
2o
3/ TiO
2core-shell nano material
1) hydrothermal synthesis method prepares nanometer Al core: take 31.4g alchlor, be dissolved in 40ml water, dropwise adding 5ml ammoniacal liquor is placed in the hydrothermal reaction kettle of polytetrafluoroethylliner liner, in 160 DEG C of reactions 6 hours, cooling, centrifugation, by the washing of centrifugal obtained precipitate with deionized water to neutral, in 75 DEG C of drying boxes, dry.
2) 0.75g nanometer Al core is ground, be dissolved in 100ml absolute ethyl alcohol, uniform stirring on magnetic stirring apparatus, dropwise add 4ml ammoniacal liquor and 4ml butyl titanate simultaneously, stir after 2 hours, centrifugation, spends deionized water to neutral by the deposit obtained, dry in 55 DEG C of drying boxes.
3) ground by dried deposit, calcine 2 hours for 550 DEG C in Muffle furnace, cooling, obtains Al
2o
3/ TiO
2core-shell nano material.
(2) apply
Method: be respectively in the reactive brilliant red x-3b solution of 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L in 100ml concentration, add 0.1gAl
2o
3/ TiO
2core-shell nano material, regulates its pH value to be 5.0 with HCl and NaOH, and take out after shaking 24 hours in oscillator, centrifugation, gets supernatant liquor, adopts UV-VIS spectrophotometry to measure remaining dye strength, calculates clearance.Result as shown in Table 2 and Figure 3.
Table 2
| Concentration mg/L | 10 | 20 | 30 | 40 | 50 |
| Clearance (Al 2O 3/TiO 2)％ | 99.59 | 94 | 97 | 96 | 97.81 |
| Clearance (TiO 2)％ | 54 | 35 | 29 | 23 | 10 |
From table 2 and Fig. 3, compared with the titanium dioxide of tetrbuty titanate synthesis, Al
2o
3/ TiO
2core-shell material for the clearance of reactive brilliant red x-3b far away higher than titanium dioxide.
Embodiment 3:pH value is for Al
2o
3/ TiO
2core-shell nano material is for pacifying the removal impact of the dark blue L-3G of promise element
Method: be in the dark blue L-3G solution of peace promise element of 350mg/L in 100ml concentration, add 0.1gAl
2o
3/ TiO
2core-shell nano material is 2-12 by HCl and NaOH adjust ph, and be placed in oscillator concussion and take out after 24 hours, centrifugation, gets supernatant liquor, adopts UV-VIS spectrophotometry to measure remaining dye strength, calculates clearance.Result as shown in table 3 and fig. 4.
Table 3
From table 3 and Fig. 4, Al of the present invention
2o
3/ TiO
2core-shell nano material (pH2-9) in pH value range more widely all has good adsorption effect.
Embodiment 4: initial concentration is for Al
2o
3/ TiO
2core-shell nano material affects for the removal of reactive brilliant red x-3b
Method: be in the reactive brilliant red x-3b solution of 10-500mg/L in 100ml concentration, add 0.1gAl
2o
3/ TiO
2core-shell nano material, be placed in oscillator concussion and take out after 24 hours, centrifugation, gets supernatant liquor, adopts UV-VIS spectrophotometry to measure remaining dye strength, calculates clearance.Result is as shown in table 4.
Table 4
From table 4, Al of the present invention
2o
3/ TiO
2core-shell nano material (10-500mg/L) within the scope of dye strength more widely all has good adsorption effect.
Claims (6)
1. an Al
2o
3/ TiO
2core-shell nano material, is characterized in that preparation method comprises the steps:
1) hydrolysis methods or hydrothermal synthesis method prepare nanometer Al core;
2) nanometer Al core is ground, be dissolved in absolute ethyl alcohol, uniform stirring on magnetic stirring apparatus, dropwise add ammoniacal liquor and butyl titanate simultaneously, stir after 2-4 hour, centrifugation, the deposit obtained is spent deionized water to neutral, dry at 55-80 DEG C;
3) ground by dried deposit, 450-600 DEG C of calcining 2-3h in Muffle furnace, cooling, obtains Al
2o
3/ TiO
2core-shell nano material.
2. Al according to claim 1
2o
3/ TiO
2core-shell nano material, it is characterized in that: described hydrolysis methods is prepared nanometer Al core and is: get alchlor, be dissolved in the water, magnetic stirring apparatus fully stirs, dropwise add ammoniacal liquor, observe precipitation to produce, continued to add ammoniacal liquor and stop after fully producing precipitation, then in 25-65 DEG C of reaction 24h, centrifugal, get precipitation, by precipitate with deionized water washing to neutral, dry at 55-80 DEG C.
3. Al according to claim 1
2o
3/ TiO
2core-shell nano material, it is characterized in that: described hydrothermal synthesis method is prepared nanometer Al core and is: get alchlor, be dissolved in the water, after dropwise adding ammoniacal liquor, be placed in the hydrothermal reaction kettle of polytetrafluoroethylliner liner, 4-6 hour is reacted at 120-160 DEG C, cooling, centrifugal, get precipitation, by precipitate with deionized water washing to neutral, dry at 55-80 DEG C.
4. Al according to claim 1
2o
3/ TiO
2the application of core-shell nano material organic dyestuff in degrading waste water.
5. application according to claim 4, is characterized in that method is as follows: the initial concentration regulating organic dyestuff in wastewater is 10-500mg/L, and pH value is 2-9, adds the arbitrary described Al of claim 1-3
2o
3/ TiO
2core-shell nano material.
6. the application according to claim 4 or 5, is characterized in that: described organic dyestuff is the dark blue or reactive brilliant red of peace promise element.
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|---|---|---|---|
| CN201510628017.6A CN105233787A (en) | 2015-09-28 | 2015-09-28 | Preparation method and applications of Al2O3/TiO2 core-shell nano material |
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| CN201510628017.6A CN105233787A (en) | 2015-09-28 | 2015-09-28 | Preparation method and applications of Al2O3/TiO2 core-shell nano material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107254242A (en) * | 2017-07-12 | 2017-10-17 | 东莞市联洲知识产权运营管理有限公司 | A kind of Water-borne Alkyd Coatings core-shell structure nanometer particle-modified based on titanium oxide/aluminum oxide |
| CN112062979A (en) * | 2020-09-07 | 2020-12-11 | 清华大学 | Organic-inorganic core-shell structure self-lubricating composite material and preparation method thereof |
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2015
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107254242A (en) * | 2017-07-12 | 2017-10-17 | 东莞市联洲知识产权运营管理有限公司 | A kind of Water-borne Alkyd Coatings core-shell structure nanometer particle-modified based on titanium oxide/aluminum oxide |
| CN112062979A (en) * | 2020-09-07 | 2020-12-11 | 清华大学 | Organic-inorganic core-shell structure self-lubricating composite material and preparation method thereof |
| CN112062979B (en) * | 2020-09-07 | 2022-04-19 | 清华大学 | Organic-inorganic core-shell structure self-lubricating composite material and preparation method thereof |
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Application publication date: 20160113 |