CN107335442B - Composite photocatalyst material and its preparation method and application is converted on a kind of Er ions yttrium aluminate/concave convex rod - Google Patents
Composite photocatalyst material and its preparation method and application is converted on a kind of Er ions yttrium aluminate/concave convex rod Download PDFInfo
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- CN107335442B CN107335442B CN201710484851.1A CN201710484851A CN107335442B CN 107335442 B CN107335442 B CN 107335442B CN 201710484851 A CN201710484851 A CN 201710484851A CN 107335442 B CN107335442 B CN 107335442B
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- convex rod
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- -1 ions yttrium aluminate Chemical class 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 32
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 5
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 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 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 2
- 229910052727 yttrium Inorganic materials 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000006477 desulfuration reaction Methods 0.000 description 7
- 230000023556 desulfurization Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 229910052691 Erbium Inorganic materials 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- IYYZUPMFVPLQIF-UHFFFAOYSA-N dibenzothiophene Chemical class C1=CC=C2C3=CC=CC=C3SC2=C1 IYYZUPMFVPLQIF-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G29/00—Refining of hydrocarbon oils, in the absence of hydrogen, with other chemicals
- C10G29/06—Metal salts, or metal salts deposited on a carrier
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
Abstract
The invention belongs to new chemical materials field, in particular to composite photocatalyst material and its preparation method and application is converted on a kind of Er ions yttrium aluminate/concave convex rod.Yttrium nitrate, erbium nitrate, aluminum nitrate and citric acid are add to deionized water stirring, water-bath is then carried out to vitreosol, is dried to xerogel, finally calcines, grinding obtains Er ions yttrium aluminate composite material；It is distributed in deionized water with concave convex rod again, regulation system pH promotes Er ions yttrium aluminate composite material and concave convex rod compound, is evaporated using water-bath to moisture, and grinding obtains Er ions yttrium aluminate/concave convex rod composite photocatalyst material after calcining.
Description
Technical field
The invention belongs to new chemical materials field, in particular to complex light is converted on a kind of Er ions yttrium aluminate/concave convex rod
Catalysis material and its preparation method and application.
Background technique
Up-conversion luminescence is the photon that a high-energy is converted out on the photon for absorb two or more low energy.
Rare earth element has unique electron structure, so that near-infrared, visible and ultraviolet etc. various can be absorbed in rare earth luminescent material
The radiation of wavelength.Due to its internal energy level transition having between 4f abundant, shine so that rare earth up-conversion luminescent material becomes
The mainstream of material.It therefore, can be by the near-infrared in sunlight by the semiconductors coupling of rare earth up-conversion and ultraviolet light response
Ultraviolet light is converted on light and visible light, greatly improves the utilization rate of sunlight, to improve the photocatalytic activity of semiconductor.
Summary of the invention
In order to solve the problems, such as the utilization rate of sunlight, the present invention provides turn on a kind of Er ions yttrium aluminate/concave convex rod
Composite photocatalyst material is changed, forms general formula are as follows: Er3+YAlO3/ ATP,
Wherein, Er/ (Er+Y)=0.01~0.02, Er3+YAlO3Account for the 20%~60% of ATP mass.
The present invention also provides the preparation sides that composite photocatalyst material is converted on a kind of above-mentioned Er ions yttrium aluminate/concave convex rod
Method:
(1) yttrium nitrate, erbium nitrate, aluminum nitrate and citric acid are add to deionized water stirring, it is anti-then carries out water-bath
It should be dried to vitreosol to xerogel, finally calcining, grinding obtain Er ions yttrium aluminate composite material,
Wherein, the molar ratio of citric acid and metal ion (the sum of yttrium, erbium, aluminium three) is 1:1~5:1,
Bath temperature is 50~80 DEG C；
(2) Er ions yttrium aluminate composite material obtained in step (1) and concave convex rod are distributed in deionized water, are adjusted
System pH promotes Er ions yttrium aluminate composite material and concave convex rod compound, is evaporated using water-bath to moisture, grinds after calcining
Mill obtains Er ions yttrium aluminate/concave convex rod composite photocatalyst material,
Regulation system pH is 2~5, so that Er3+YAlO3Different charges, i.e. concave convex rod surface are had from concave convex rod surface
With negative electrical charge, Er ions yttrium aluminate surface has positive charge, so that generating electrostatic attraction promotes Er ions yttrium aluminate and bumps
Stick it is compound.
The present invention also provides on a kind of above-mentioned Er ions yttrium aluminate/concave convex rod convert composite photocatalyst material application,
Photocatalysis desulfurization is carried out using the composite photocatalyst material.
The beneficial effects of the present invention are:
It is found by the applicant that: concave convex rod due to inside it containing the iron oxide of semiconductor property so that concave convex rod also has half
Conductor nature, however due to its greater band gap, it only can be to ultraviolet light response, so under very low to the utilization rate of sunlight；Cause
This present invention is made on the nonabsorbable near infrared light of concave convex rod and visible light by the way that rare earth up-conversion is compound with concave convex rod
Ultraviolet light is converted to, has widened the optical response range of concave convex rod indirectly, improves the utilization rate of sunlight；
The method that the present invention uses electrostatic attraction, under certain pH conditions, concave convex rod surface has negative electricity, converts on rare earth
Material surface has positive electricity, enhances the combination between conversion and semiconductor, avoids rare earth up-conversion and semiconductor
Simple mechanical mixture is easy to the problem of being detached from during photocatalysis desulfurization；
Concave convex rod in the present invention is excited as semiconductor generates light induced electron and hole with sulfur-containing compound of degrading
Meanwhile the peculiar absorption property that other semiconductors do not have has been played, because itself has biggish specific surface area and unique
Cellular structure, the meeting absorbed portion sulfur-containing compound in photocatalysis sweetening process, to improve desulfurization degree.
Detailed description of the invention
Fig. 1 is Y prepared by the embodiment of the present invention 10.98Er0.02AlO3, 40%Y0.98Er0.02AlO3/ ATP's and raw material A TP
XRD diagram；
Fig. 2 is Y prepared by the embodiment of the present invention 10.98Er0.02AlO3SEM figure；
Fig. 3 is 40%Y prepared by the embodiment of the present invention 10.98Er0.02AlO3The SEM of/ATP schemes.
Specific embodiment
Embodiment 1
(1) by 3.01g yttrium nitrate, 0.07g erbium nitrate, 3.00g aluminum nitrate and 10.09g citric acid be added to 100ml go from
It is stirred in sub- water, then 60 DEG C of water-baths to vitreosol, by its 80 DEG C dryings to xerogel, last 1100 DEG C of calcinings 2h,
Grinding obtains Er ions yttrium aluminate composite material Y0.98Er0.02AlO3；
(2) by Er ions yttrium aluminate composite material Y obtained in 0.4g step (1)0.98Er0.02AlO3With 1.0g concave convex rod
It is distributed in 100ml deionized water, regulation system pH is 4.5, is evaporated using 60 DEG C of water-bath to moisture, 400 DEG C of calcinings
Grinding obtains Er ions yttrium aluminate/concave convex rod composite photocatalyst material 40%Y after 2h0.98Er0.02AlO3/ATP。
X-ray powder diffraction is carried out to gained sample and characterizes its structure and composition, and is seen using scanning electron microscope
The pattern for examining sample, the 40%Y prepared according to the technique of embodiment 10.98Er0.02AlO3The XRD diagram of/ATP is as shown in Figure 1, compound
Occurs Er in material respectively3+YAlO3With the characteristic peak of ATP, illustrate Er3+YAlO3Success is compound with ATP, has prepared Er3+
YAlO3Composite photocatalyst material is converted on/ATP；
The present embodiment step (1) obtained Y0.98Er0.02AlO3SEM it is as shown in Figure 2: show particle shape；This reality
Apply a step (2) obtained 40%Y0.98Er0.02AlO3The SEM of/ATP is as shown in Figure 3: 40%Y0.98Er0.02AlO3It is tight with ATP
Close combination, it is consistent with XRD result；
Composite photocatalyst material 40%Y manufactured in the present embodiment is utilized the present invention also provides a kind of0.98Er0.02AlO3/
The method of ATP progress photocatalysis desulfurization: it weighs 0.4031g dibenzothiophenes and is dissolved in 500ml normal octane to prepare 200ppm
Simulation oil, 40%Y is added in photocatalytic reaction device0.98Er0.02AlO3/ ATP and simulation oil (mass ratio 1:1000), secretly
Absorption 30min after introduce simulated solar irradiation, every half an hour collect a sample, be added N-N, dimethylformamide extraction on
Layer clear liquid measures sulfur content with UV suLfur anaLyzer, and desulfurization degree (%) is calculated according to following equation:
D=(1-Ct/C0) * 100%
Wherein: C0For the sulfur content of initial soln, CtSulfur content when to react the t time in solution system, in 3h illumination
Under, 40%Y0.98Er0.02AlO3The desulfurization degree of/ATP has reached 94%.
Embodiment 2
(1) with embodiment 1；
(2) by Er ions yttrium aluminate composite material Y obtained in 0.2g step (1)0.98Er0.02AlO3With 1.0g concave convex rod
It is distributed in 100ml deionized water, regulation system pH is 4.5, is evaporated using 60 DEG C of water-bath to moisture, 400 DEG C of calcinings
Grinding obtains Er ions yttrium aluminate/concave convex rod composite photocatalyst material 20%Y after 2h0.98Er0.02AlO3/ATP。
Subsequent detection such as embodiment 1.
Embodiment 3
(1) with embodiment 1；
(2) by Er ions yttrium aluminate composite material Y obtained in 0.6g step (1)0.98Er0.02AlO3With 1.0g concave convex rod
It is distributed in 100ml deionized water, regulation system pH is 4.5, is evaporated using 60 DEG C of water-bath to moisture, 400 DEG C of calcinings
Grinding obtains Er ions yttrium aluminate/concave convex rod composite photocatalyst material 60%Y after 2h0.98Er0.02AlO3/ATP。
Subsequent detection such as embodiment 1.
Embodiment 4
(1) by 3.03g yttrium nitrate, 0.04g erbium nitrate, 3.00g aluminum nitrate and 10.09g citric acid be added to 100ml go from
It is stirred in sub- water, then 60 DEG C of water-baths to vitreosol, by its 80 DEG C dryings to xerogel, last 1100 DEG C of calcinings 2h,
Grinding obtains Er ions yttrium aluminate composite material Y0.99Er0.01AlO3；
(2) by Er ions yttrium aluminate composite material Y obtained in 0.2g step (1)0.99Er0.01AlO3With 1.0g concave convex rod
It is distributed in 100ml deionized water, regulation system pH is 4.5, is evaporated using 60 DEG C of water-bath to moisture, 400 DEG C of calcinings
Grinding obtains Er ions yttrium aluminate/concave convex rod composite photocatalyst material 20%Y after 2h0.99Er0.01AlO3/ATP。
Subsequent detection such as embodiment 1.
Embodiment 5
(1) with embodiment 4；
(2) by Er ions yttrium aluminate composite material Y obtained in 0.6g step (1)0.99Er0.01AlO3With 1.0g concave convex rod
It is distributed in 100ml deionized water, regulation system pH is 4.5, is evaporated using 60 DEG C of water-bath to moisture, 400 DEG C of calcinings
Grinding obtains Er ions yttrium aluminate/concave convex rod composite photocatalyst material 60%Y after 2h0.99Er0.01AlO3/ATP。
Subsequent detection such as embodiment 1.
Comparative example 1
Step is not adjusted pH value in (2), remaining operation is with embodiment 1:
(1) with embodiment 1；
(2) by Er ions yttrium aluminate composite material Y obtained in 0.4g step (1)0.98Er0.02AlO3With 1.0g concave convex rod
It is distributed in 100ml deionized water, is evaporated by 60 DEG C of water-bath to moisture, grinding is to obtain erbium to mix after 400 DEG C of calcining 2h
Miscellaneous yttrium aluminate/concave convex rod composite photocatalyst material 40%Y0.98Er0.02AlO3/ATP。
Subsequent detection such as embodiment 1.Under 3h illumination, the 40%Y of this comparative example preparation0.98Er0.02AlO3/ ATP's
Desulfurization degree is only 72%, this is because the molding binding force in this comparative example between concave convex rod and up-conversion is undesirable
Caused by.
Claims (3)
1. converting composite photocatalyst material on a kind of Er ions yttrium aluminate/concave convex rod, it is characterised in that: the composite photocatalyst material
The composition general formula of material is Er3+YAlO3/ATP；For calculation in the molar ratio, Er/ (Er+Y)=0.01~0.02；Er3+YAlO3Account for ATP matter
The 20%~60% of amount；
The Er3+YAlO3/ ATP composite photocatalyst material the preparation method comprises the following steps:
(1) yttrium nitrate, erbium nitrate, aluminum nitrate and citric acid are add to deionized water stirring, then carry out water-bath extremely
Vitreosol is dried to xerogel, is finally calcined, grinding obtains Er ions yttrium aluminate composite material；
(2) Er ions yttrium aluminate composite material obtained in step (1) and concave convex rod are distributed in deionized water, regulation system
PH, regulation system pH are 2~5, are evaporated using water-bath to moisture, and grinding obtains Er ions yttrium aluminate/recessed after calcining
Convex stick composite photocatalyst material.
2. converting composite photocatalyst material on Er ions yttrium aluminate/concave convex rod as described in claim 1, it is characterised in that: step
Suddenly in (1), the molar ratio of citric acid and metal ion is 1:1~5:1.
3. converting composite photocatalyst material on Er ions yttrium aluminate/concave convex rod as described in claim 1, it is characterised in that: step
Suddenly in (1), bath temperature is 50~80 DEG C.
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| CN109621940B (en) * | 2018-12-12 | 2020-05-26 | 常州大学 | Rare earth doped lithium niobate/attapulgite composite photocatalytic material and preparation method and application thereof |
| CN109999838B (en) * | 2019-05-09 | 2022-07-12 | 江苏纳欧新材料有限公司 | Preparation method and application of vanadium sulfide/attapulgite nanocomposite with wide spectral response |
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| CN102078807B (en) * | 2011-01-05 | 2013-01-16 | 吉林大学 | Er<3+>:YAlO3/TiO2-loaded photocatalyst and preparation method thereof |
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