CN110102281A - A kind of preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth - Google Patents
A kind of preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth Download PDFInfo
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- CN110102281A CN110102281A CN201910400137.9A CN201910400137A CN110102281A CN 110102281 A CN110102281 A CN 110102281A CN 201910400137 A CN201910400137 A CN 201910400137A CN 110102281 A CN110102281 A CN 110102281A
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- rare earth
- doped porous
- erbium ion
- strontium titanates
- isometric particle
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- 229910052691 Erbium Inorganic materials 0.000 title claims abstract description 32
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 30
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 30
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 30
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000002245 particle Substances 0.000 title claims abstract description 28
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 13
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- -1 erbium ion Chemical class 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- YBYGDBANBWOYIF-UHFFFAOYSA-N erbium(3+);trinitrate Chemical compound [Er+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YBYGDBANBWOYIF-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 239000000356 contaminant Substances 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 description 6
- 230000004044 response Effects 0.000 description 4
- 229910002370 SrTiO3 Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910002367 SrTiO Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of the erbium ion-doped porous strontium titanates isometric particle of rare earth, the following steps are included: first titanium sulfate and potassium hydroxide are dissolved in deionized water respectively, appropriate potassium hydroxide solution is taken to instill in titanium sulfate solution, form precipitating, repeatedly mixed nitrate strontium, erbium nitrate and potassium hydroxide after washing, hydro-thermal reaction is then carried out, the erbium ion-doped porous strontium titanates isometric particle of rare earth is obtained after being washed, being dried.Erbium ion-doped porous strontium titanates isometric particle prepared by the present invention has large specific surface area, forbidden bandwidth is adjustable, and redox catalysis activity performance it is excellent the features such as, have a wide range of applications in fields such as photocatalytic hydrogen production by water decomposition, photocatalysis degradation organic contaminant and photochemical cells.
Description
Technical field
The present invention relates to a kind of preparation method of the erbium ion-doped porous strontium titanates isometric particle of perovskite structure rare earth,
Belong to material science and technology field.
Background technique
Inorganic perovskite structure oxide, general molecular formula ABO3, it is ceramic that this type oxide can be used for making middle high-pressure
Capacitor, the precise electronics component such as PTC thermistor.Wherein, strontium titanates (SrTiO3) it is a kind of typical perovskite structure
Oxide has high dielectric constant, low-dielectric loss and excellent thermal stability, is widely used in electronic component neck
Domain.Meanwhile SrTiO3Have the characteristics that photocatalytic activity is excellent, in photocatalysis degradation organic contaminant, photochemical catalyzing system
The photocatalysis fields such as hydrogen and photochemical cell are also widely used.However, SrTiO3Forbidden bandwidth is higher (3.2eV),
It is lower to the producing level of sunlight, currently, mostly use it is heterogeneous be combined into, the form of ion doping urges its forbidden bandwidth and light
Change efficiency to be improved.Rare earth ion has energy level abundant, and the transition number between rare earth ion energy level is more, contains from purple
Outside, the light of visible infrared each wave band.Therefore, the present invention is quasi- by rare earth doped erbium ion, and controllability adjusts SrTiO3's
Forbidden bandwidth improves SrTiO3Sunlight photocatalysis is realized to improve its effective use to sunlight to the absorption of light
Effect.
The erbium ion-doped SrTiO of rare earth of the invention3Simply, conveniently, synthesis material is cheap and is easy to get for preparation method,
The SrTiO prepared3It is porous cubic.Product prepared by the present invention has large specific surface area, and forbidden bandwidth is adjustable, and aoxidizes
The features such as reduction catalysts activity performance is excellent, in photocatalytic hydrogen production by water decomposition, photocatalysis degradation organic contaminant and photochemistry electricity
The photocatalysis fields such as pond have a wide range of applications.
Summary of the invention
The purpose of the present invention is to provide a kind of simple process, the erbium ion-doped POROUS TITANIUM of the easily controllable rare earth of process
The preparation method of sour strontium isometric particle.
The preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth proposed by the present invention, including following step
It is rapid:
(1) titanium sulfate is dissolved in deionized water, is stirred, obtain solution A；
(2) potassium hydroxide solution is added dropwise in Xiang Shangshu solution A, stirs, form precipitate B；
(3) precipitate B is cleaned with deionized water, then sequentially adds strontium nitrate solution, Nitrate Solution and potassium hydroxide
Solution, stirring obtain mixture C to abundant dissolution；
(4) said mixture C is transferred in reaction kettle, at 180-200 DEG C, carries out hydro-thermal reaction, the reaction time is
4-15h obtains reaction product；
(5) finally, reaction product is taken out, filtering is cleaned with deionized water and ethyl alcohol, is dried, is transferred to forced air drying
Drying and processing, the i.e. erbium ion-doped porous strontium titanates isometric particle of acquisition rare earth are carried out in case.
Further, in the erbium ion-doped porous strontium titanates isometric particle of the rare earth Sr:Ti atomic ratio be 1~
1.2:1.
Further, the doping concentration of erbium ion is in the erbium ion-doped porous strontium titanates isometric particle of the rare earth
The ratio that 0.1-10mol%, i.e. Er ion doping enter strontium titanates intracell is the molar ratio of Er ion and strontium titanates.
Further, potassium hydroxide solution concentration described in step (3) is 6-10mol/L, changes the adjustable production of its concentration
The size of hole in object.
Further, drying and processing described in step (5) is 60-80 DEG C, 5-10 hours.
A kind of erbium ion-doped porous strontium titanates isometric particle of rare earth, is prepared using the above method.
Erbium ion-doped porous strontium titanates isometric particle prepared by the present invention has the advantage that
For porous structure, with large specific surface area, forbidden bandwidth is adjustable, and the excellent equal spies of redox catalysis activity performance
Point, before the fields such as photocatalytic hydrogen production by water decomposition, photocatalysis degradation organic contaminant and photochemical cell have a wide range of applications
Scape.In method of the invention in reaction time and reactant concentration especially step (3) potassium hydroxide concentrations on product pattern
It has an important influence, when KOH concentration exceeds a certain range, it may be difficult to obtain porous structure.
Detailed description of the invention
Fig. 1 is the SEM figure of the erbium ion-doped porous strontium titanates isometric particle of the rare earth of the preparation of embodiment 1；
Fig. 2 is the XRD diagram of the erbium ion-doped porous strontium titanates isometric particle of the rare earth of the preparation of embodiment 2；
Specific embodiment
Below with reference to example, the invention will be further described.
Embodiment 1:
It weighs a certain amount of titanium sulfate to be dissolved in deionized water, stir, obtaining concentration is 0.005mol/L's
Solution A；Suitable potassium hydroxide solution is added dropwise into above-mentioned solution A, stirs, forms precipitate B；It is with deionized water that precipitate B is clear
After washing for several times, the strontium nitrate of the 1mol/L dissolved is sequentially added, the erbium nitrate that doping content is 1mol% and concentration are
The potassium hydroxide solution of 6mol/L, stirring to abundant dissolution；Said mixture is transferred in reaction kettle, water is carried out at 180 DEG C
Thermal response, reaction time 15h.Finally, reaction product is taken out, filter, cleaned with deionized water and ethyl alcohol, dries, transfer
80 DEG C are carried out into air dry oven, the drying and processing of 5h, the i.e. erbium ion-doped porous strontium titanates isometric particle of acquisition rare earth.
Embodiment 2:
It weighs a certain amount of titanium sulfate to be dissolved in deionized water, stir, obtaining concentration is 0.005mol/L's
Solution A；Suitable potassium hydroxide solution is added dropwise into above-mentioned solution A, stirs, forms precipitate B；It is with deionized water that precipitate B is clear
After washing for several times, the strontium nitrate of the 1.2mol/L dissolved is sequentially added, the erbium nitrate that doping content is 10mol% and concentration are
The potassium hydroxide solution of 10mol/L, stirring to abundant dissolution；Said mixture is transferred in reaction kettle, water is carried out at 200 DEG C
Thermal response, reaction time 4h.Finally, reaction product is taken out, filter, cleaned with deionized water and ethyl alcohol, dries, be transferred to
60 DEG C are carried out in air dry oven, the drying and processing of 10h, the i.e. erbium ion-doped porous strontium titanates isometric particle of acquisition rare earth.
Embodiment 3:
It weighs a certain amount of titanium sulfate to be dissolved in deionized water, stir, obtaining concentration is 0.005mol/L's
Solution A；Suitable potassium hydroxide solution is added dropwise into above-mentioned solution A, stirs, forms precipitate B；It is with deionized water that precipitate B is clear
After washing for several times, the strontium nitrate of the 1.1mol/L dissolved is sequentially added, the erbium nitrate that doping content is 5mol% and concentration are
The potassium hydroxide solution of 8mol/L, stirring to abundant dissolution；Said mixture is transferred in reaction kettle, water is carried out at 190 DEG C
Thermal response, reaction time 10h.Finally, reaction product is taken out, filter, cleaned with deionized water and ethyl alcohol, dries, transfer
70 DEG C are carried out into air dry oven, the drying and processing of 8h, the i.e. erbium ion-doped porous strontium titanates isometric particle of acquisition rare earth.
Embodiment 4:
It weighs a certain amount of titanium sulfate to be dissolved in deionized water, stir, obtaining concentration is 0.005mol/L's
Solution A；Suitable potassium hydroxide solution is added dropwise into above-mentioned solution A, stirs, forms precipitate B；It is with deionized water that precipitate B is clear
After washing for several times, the strontium nitrate of the 1.1mol/L dissolved is sequentially added, the erbium nitrate that doping content is 5mol% and concentration are
The potassium hydroxide solution of 12mol/L, stirring to abundant dissolution；Said mixture is transferred in reaction kettle, water is carried out at 200 DEG C
Thermal response, reaction time 4h.Finally, reaction product is taken out, filter, cleaned with deionized water and ethyl alcohol, dries, be transferred to
In air dry oven carry out 60 DEG C, the drying and processing of 10h, obtain product be the isometric particle shape rare earth erbium without porous structure from
Sub- strontium titanate doping.
Claims (6)
1. a kind of preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth, it is characterised in that including following step
It is rapid:
(1) titanium sulfate is dissolved in deionized water, is stirred evenly, obtain solution A；
(2) potassium hydroxide solution is added dropwise in Xiang Shangshu solution A, stirs, form precipitate B；
(3) precipitate B is cleaned with deionized water, then sequentially adds strontium nitrate solution, Nitrate Solution and potassium hydroxide solution,
Stirring obtains mixture C to abundant dissolution；
(4) said mixture C is transferred in reaction kettle, at 180-200 DEG C, carries out hydro-thermal reaction 4-15h, obtained reaction and produce
Object；
(5) finally, reaction product is taken out, filtering is cleaned with deionized water and ethyl alcohol, is dried, is transferred in air dry oven
Carry out drying and processing, the i.e. erbium ion-doped porous strontium titanates isometric particle of acquisition rare earth.
2. the preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth according to claim 1, feature
It is, Sr:Ti atomic ratio is 1~1.2:1 in the erbium ion-doped porous strontium titanates isometric particle of the rare earth.
3. the preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth according to claim 1, feature
It is, the doping concentration of erbium ion is 0.1-10mol% in the erbium ion-doped porous strontium titanates isometric particle of the rare earth.
4. the preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth according to claim 1, feature
It is, the concentration of potassium hydroxide solution described in step (3) is 6-10mol/L.
5. the preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth according to claim 1, feature
It is, drying and processing described in step (5) is 60-80 DEG C, 5-10 hours.
6. a kind of erbium ion-doped porous strontium titanates isometric particle of rare earth, is prepared using method as claimed in claim 1.
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| CN201910400137.9A CN110102281A (en) | 2019-05-14 | 2019-05-14 | A kind of preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth |
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| CN201910400137.9A CN110102281A (en) | 2019-05-14 | 2019-05-14 | A kind of preparation method of the erbium ion-doped porous strontium titanates isometric particle of rare earth |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111495352A (en) * | 2020-04-27 | 2020-08-07 | 昆明理工大学 | Method for efficiently carrying out photocatalytic oxidation on elemental mercury through metal doping modification of strontium titanate |
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2019
- 2019-05-14 CN CN201910400137.9A patent/CN110102281A/en active Pending
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| JPH07220902A (en) * | 1994-02-07 | 1995-08-18 | Murata Mfg Co Ltd | Barium titanate semiconductor ceramic |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111495352A (en) * | 2020-04-27 | 2020-08-07 | 昆明理工大学 | Method for efficiently carrying out photocatalytic oxidation on elemental mercury through metal doping modification of strontium titanate |
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Application publication date: 20190809 |