CN106475121A - A kind of new catalyst Er: Y3Al5O12/BiPO4And its preparation method and application - Google Patents
A kind of new catalyst Er: Y3Al5O12/BiPO4And its preparation method and application Download PDFInfo
- Publication number
- CN106475121A CN106475121A CN201610896753.4A CN201610896753A CN106475121A CN 106475121 A CN106475121 A CN 106475121A CN 201610896753 A CN201610896753 A CN 201610896753A CN 106475121 A CN106475121 A CN 106475121A
- Authority
- CN
- China
- Prior art keywords
- bipo
- preparation
- new catalyst
- catalyst
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000006260 foam Substances 0.000 claims description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 8
- -1 rare-earth ion Chemical class 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229950000845 politef Drugs 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 3
- 238000005187 foaming Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 235000005979 Citrus limon Nutrition 0.000 claims 2
- 244000248349 Citrus limon Species 0.000 claims 1
- 244000131522 Citrus pyriformis Species 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 238000004821 distillation Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 12
- 239000003795 chemical substances by application Substances 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000009835 boiling Methods 0.000 abstract 1
- 239000006227 byproduct Substances 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 238000005755 formation reaction Methods 0.000 abstract 1
- 239000012153 distilled water Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 229940124899 Biothrax Drugs 0.000 description 3
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 3
- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 description 3
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 229910052590 monazite Inorganic materials 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 238000011426 transformation method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- VVSWDMJYIDBTMV-ORWNZLQRSA-N (2s,4ar,6s,7s,8s,8ar)-6-methoxy-2-phenyl-4,4a,6,7,8,8a-hexahydropyrano[3,2-d][1,3]dioxine-7,8-diol Chemical compound C1([C@H]2OC[C@H]3O[C@@H]([C@H]([C@H](O)[C@H]3O2)O)OC)=CC=CC=C1 VVSWDMJYIDBTMV-ORWNZLQRSA-N 0.000 description 1
- 101000978544 Homo sapiens MAP3K12-binding inhibitory protein 1 Proteins 0.000 description 1
- 102100023728 MAP3K12-binding inhibitory protein 1 Human genes 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1815—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with arsenic, antimony or bismuth
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/166—Nitrites
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of new catalyst Er:Y3Al5O12/BiPO4And its preparation method and application.Employed technical scheme comprise that：The BiPO of three kinds of crystal formations is first synthesized with hydro-thermal method4, afterwards with the upper light conversion agent Er of sol-gal process synthesis:Y3Al5O12, finally by the BiPO of preparation4Powder and upper light conversion agent Er:Y3Al5O12Synthesize Er with the method for ultrasonic disperse and liquid boiling:Y3Al5O12/BiPO4.Under simulated solar light irradiation, use Er:Y3Al5O12/BiPO4Make catalyst, photocatalytic conversion nitrite.The inventive method is simply novel, low cost, and does not have by-product generation can't cause environmental pollution.
Description
Technical field
The invention belongs to chemical catalysis field, more particularly, to new E r:Y3Al5O12/BiPO4The synthesis of catalyst and utilization
Its method that Nitrite is converted.
Background technology
With modern industry and agriculture developing rapidly, the concentration of Nitrite is due to the excessive row of trade effluent
Put, nitrogenous fertilizer excessive using and incomplete abiotic denitrification process and significantly rise.Nitrite is a kind of strong to human body
Health has the inorganic environment pollutant of very big toxicity.World Health Organization (WHO) proposes, and the nitrite concentration peak in drinking water is
3mg/L.Photocatalysis technology receives because it directly can remove pollutant and easily separated reuse in water body using the light absorbing
Widely pay close attention to.This characteristic mainly appears in metal-oxide and combined metal oxide semiconductor, such as TiO2Because it is urged
Change active of a relatively high, physicochemical properties are stable, and are widely used.However, for the sodium nitrite removing in water body, needing
Select a quasiconductor having compared with Strong oxdiative ability and reducing power, Nitrite transformation is acid group and ammonia, therefore
Select a broadband semiconductor with of a relatively high conduction band and relatively low valence band.
Bismugel (Biothrax)., as a kind of novel metalloid oxygen-containing acid group quasiconductor, has three kinds of principal crystalline phase structures：Monoclinic phase, monocline
Phase monazite and hexagonal phase.But as a broadband semiconductor, Bismugel (Biothrax). absorbs the poor ability of sunlight, can only be using purple
Outer light is obtaining the photon energy, and ultraviolet light only accounts for the 4% of solar spectrum.Therefore, how sufficiently effective utilization sunlight, be
Problem demanding prompt solution.
Content of the invention
It is an object of the invention to design synthesis is a kind of can be used for converting the new catalyst Er of aqueous solution nitrite3 +:Y3Al5O12/BiPO4.Compound involved in the present invention belongs to new rare metal catalyst, is applied to nitrite and turns
Change, method is simple, pollution-free, catalyst stabilization and being easily isolated.
The technical solution used in the present invention is：A kind of new catalyst Er:Y3Al5O12/BiPO4, preparation method is as follows：Will
Er3+:Y3Al5O12And BiPO4After mixing, plus deionized water, ultrasonic disperse 15-30min, under stirring, heat 30- in 50-60 DEG C
40min, filters, and cleaning is placed in Muffle furnace, in 280-320 DEG C of roasting 2-3h, obtains target product.
Preferably, above-mentioned a kind of new catalyst Er:Y3Al5O12/BiPO4, Er3+:Y3Al5O12And BiPO4Weight ratio
For 0.25-0.35:1.
Preferably, above-mentioned a kind of new catalyst Er:Y3Al5O12/BiPO4, described BiPO4Preparation method be：Will
H3PO4With Bi (NO3)3·6H2O mixes, and magnetic agitation 1-2h at room temperature obtains suspension, suspension is put into politef
In stainless steel cauldron, hydro-thermal reaction 70-75h at 20-200 DEG C, reactant filters, cleaning, is dried, obtains target product.
Preferably, above-mentioned a kind of new catalyst Er:Y3Al5O12/BiPO4, described Er3+:Y3Al5O12Preparation side
Method is：In nitric acid, by Er:Y3Al5O12In ratio add Er2O3And Y2O3, simultaneously heated and stirred, to water white transparency, obtains dilute for dissolving
Native solion；By Er:Y3Al5O12In ratio weigh Al (NO3)3·9H2O is dissolved in distilled water, then at room temperature,
It is slowly added in rare-earth ion solution, after mix homogeneously, adds citric acid, in 50-60 DEG C of heated and stirred, when solution is in sticky
Stop during shape, obtain the glutinous colloidal solution that foams, glutinous for foaming colloidal solution is put into baking oven, heats 23-25h in 95-105 DEG C, obtain
To foam sol, the foam sol obtaining is heated 40-60min at 500 DEG C, then calcine 100-150min at 1100 DEG C, cold
But, obtain Er:Y3Al5O12Powder.
Preferably, above-mentioned a kind of new catalyst Er:Y3Al5O12/BiPO4, in molar ratio, citric acid：Rare earth ion=
3-4：1.
A kind of above-mentioned new catalyst Er:Y3Al5O12/BiPO4Application in conversion Nitrite.Method
As follows：In the aqueous solution containing nitrite, add the catalyst Er described in claim 1 or 2:Y3Al5O12/BiPO4, can
See reaction 0.5-6h under light.
The invention has the beneficial effects as follows：The present invention, on the basis of multiple photocatalysis technologies, have studied for nitrite
It is combined with Bismugel (Biothrax). and turn the technology carrying out Nitrite transformation based on light luminescent material.By the method for the present invention, can be by Asia
Nitrate concentration is down to below 3ppm, and does not affect other quality index.Compared with other photocatalysis technologies, process of the present invention letter
Single, normal temperature and pressure is carried out, mild condition, and solar energy can be utilized, and Nitrite transformation rate reaches more than 85%.
Brief description
Fig. 1 a is the Er preparing3+:Y3Al5O12XRD figure.
Fig. 1 b is the Er preparing3+:Y3Al5O12SEM figure.
Fig. 2 a is the XRD figure of the HBIP of embodiment 1 preparation.
Fig. 2 b is the Er of embodiment 1 preparation3+:Y3Al5O12The XRD figure of/HBIP.
Fig. 2 c is HBIP and Er of embodiment 1 preparation3+:Y3Al5O12The SEM figure of/HBIP.
Fig. 3 a is the XRD figure of the nMBIP of embodiment 2 preparation.
Fig. 3 b is the Er of embodiment 2 preparation3+:Y3Al5O12The XRD figure of/nMBIP.
Fig. 3 c is nMBIP and Er of embodiment 2 preparation3+:Y3Al5O12The SEM figure of/nMBIP.
Fig. 4 a is the XRD figure of the mMBIP of embodiment 3 preparation.
Fig. 4 b is the Er of embodiment 3 preparation3+:Y3Al5O12The XRD figure of/mMBIP.
Fig. 4 c is mMBIP and Er of embodiment 3 preparation3+:Y3Al5O12The SEM figure of/mMBIP.
Specific embodiment
A kind of new catalyst Er of embodiment 13+:Y3Al5O12/HBIP
(1) Er3+:Y3Al5O12The preparation of/HBIP
The preparation of 1.HBIP：By 100mL H3PO4(12M) pour beaker into, the Bi (NO with 10mmol3)3·6H2O mixes,
Magnetic agitation 1h under room temperature, obtains suspension, the suspension obtaining is put in politef stainless steel cauldron, at 20 DEG C
Hydro-thermal reaction 72h.Reactant is naturally cooled to room temperature, filters, distilled water cleans, dry 24h in 80 DEG C, obtain white powder
End, as has the BiPO of monoclinic phase crystal formation4(being designated as HBIP).
2.Er3+:Y3Al5O12Preparation：Take the salpeter solution that 100ml concentration is 65% (v/v), add 0.013g Er2O3
With 2.271g Y2O3, dissolving, and at 60 DEG C, magnetic force heated and stirred, until water white transparency, obtain rare-earth ion solution.Weigh
12.621g Al(NO3)3·9H2O is dissolved in distilled water, is stirred with Glass rod at room temperature and is slowly added to rare earth ion
In solution.Then, according to mol ratio, citric acid：Rare earth ion=3：1, add 33.935g citric acid, with magneton at 50-60 DEG C
Heated and stirred, stops when solution is in thick, obtains the glutinous colloidal solution that foams.Glutinous for foaming colloidal solution is put into baking oven, permanent
Heat 24h at 100 DEG C of temperature, finally give foam sol.The foam sol obtaining is heated 50min at 500 DEG C, then 1100
DEG C calcining 120min.Take out sinter, be cooled to room temperature in atmosphere, obtain Er:Y3Al5O12Powder.
3. by 0.3g Er3+:Y3Al5O12BiPO with 1.0g monoclinic phase crystal formation4It is placed in beaker, add 50mL deionization
Water, carries out ultrasonic disperse 15min-20min.At 60 DEG C, under magnetic agitation, heat 30min, filter, distilled water cleans, filtrate
Put crucible into, be placed in Muffle furnace, in 300 DEG C of roasting 2h, 2 DEG C/min of heat rate, obtain target product Er3+:Y3Al5O12/
HBIP.
(2) characterize data：
The Er of preparation3+:Y3Al5O12XRD as shown in Figure 1a, found out by Fig. 1 a, the diffraction peak of sample and JCPDS standard
It is fairly good that the data result of card 33-0040 meets, and is indicated above the sample after heat treatment and is single body-centered cubic structure,
Other dephasigns all do not occur.This illustrates Er3+The doping of ion does not produce obvious impact to crystal structure.
The Er of preparation3+:Y3Al5O12SEM as shown in Figure 1 b, found out by Fig. 1 b, the particle diameter of gained crystal is 40-50nm,
It is shaped as spherical or spherical, size distribution ratio is more uniform, and dispersibility is also preferable.Sample preparation success is described.
HBIP and Er of preparation3+:Y3Al5O12The XRD of/HBIP as shown in Figure 2 a and 2 b, is found out by Fig. 2 a, HBIP feature
Peak 2 θ=19.1 °, 2 θ=21.5 °, 2 θ=29.5 °, meet with standard card JCPDS 45-1370 data result, be indicated above
Sample after heat treatment is single cube structure, other dephasigns.Er is found out by Fig. 2 b3+:Y3Al5O12/HBIP
Complex has HBIP and Er simultaneously3+:Y3Al5O12Characteristic peak, have no other dephasigns occur, this illustrate Er3+:Y3Al5O12With
HBIP is combined and crystal structure is not produced with obvious impact.
HBIP and Er of preparation3+:Y3Al5O12The SEM of/HBIP as shown in Figure 2 c, finds out, HBIP assumes 1.0- by Fig. 2 c
1.5 μm long, and 100-200nm width and 30-50nm are high, and light conversion agent is dispersed in its surface in spherical, and composite catalyst system is described
Standby success.
(3) Nitrite transformation method
In the test tube of light-catalyzed reaction instrument, add the catalyst Er of 50mL nitrite solution (10ppm) and 50mg3+:
Y3Al5O12/ HBIP, under room temperature, simulated solar illumination, opens magnetic agitation, reacts 0.5～6 hour, reaction finishes, and will urge
Agent and solution carry out separating.
With liquid chromatogram measuring aqueous solution nitrite concentration, aqueous solution nitrite concentration is 1.47ppm, conversion
Rate is 85.3%.
A kind of new catalyst Er of embodiment 23+:Y3Al5O12/nMBIP
(1) Er3+:Y3Al5O12The preparation of/nMBIP
The preparation of 1.nMBIP：By 100mL H3PO4(12M) pour beaker into, the Bi (NO with 10mmol3)3·6H2O mixes,
Magnetic agitation 1h at room temperature, obtains suspension, the suspension obtaining is put in politef stainless steel cauldron, in 100
Hydro-thermal reaction 72h at DEG C.Reactant is naturally cooled to room temperature, filters, distilled water cleans, dry 24h in 80 DEG C, obtain white
Powder, as has the BiPO of monoclinic phase monazite crystal formation4(being designated as nMBIP).
2.Er3+:Y3Al5O12Preparation：With embodiment 1.
3. by 0.3g Er3+:Y3Al5O12BiPO with 1.0g monoclinic phase monazite crystal formation4It is placed in beaker, add 50mL
Deionized water, carries out ultrasonic disperse 15min-20min.At 60 DEG C, under magnetic agitation, heat 30min, filter, distilled water cleans,
Filtrate puts crucible into, is placed in Muffle furnace, with 300 DEG C of roasting 2h, 2 DEG C/min of heat rate, obtains target product Er3+:
Y3Al5O12/nMBIP.
(2) characterize data
NMBIP and Er of preparation3+:Y3Al5O12The XRD of/nMBIP as shown in Figure 3 a and Figure 3 b shows, is found out by Fig. 3 a, nMBIP
Characteristic peak 2 θ=17.0 °, 21.4 °, 34.5 ° are met with standard card JCPDS 80-0209, are indicated above the sample after heat treatment
For single cube structure, other dephasigns do not occur.Er be can be seen that by Fig. 3 b3+:Y3Al5O12/ HBIP complex is simultaneously
There is nMBIP and Er3+:Y3Al5O12Characteristic peak, have no other dephasigns occur, this illustrate Er3+:Y3Al5O12It is combined with nMBIP
Crystal structure is not produced with obvious impact.
NMBIP and Er of preparation3+:Y3Al5O12The SEM of/nMBIP as shown in Figure 3 c, finds out, nMBIP assumes 50- by Fig. 3 c
The nanocube of the routine of 100nm, light conversion agent is dispersed in its surface in spherical, illustrates that composite catalyst is successfully prepared.
(3) Nitrite transformation method
In the test tube of light-catalyzed reaction instrument, add 50mL nitrite solution (10ppm) and 50mg catalyst Er3+:
Y3Al5O12/ nMBIP, under room temperature simulated solar illumination, opens magnetic agitation, reacts 0.5～6 hour, reaction finishes, and will urge
Agent and solution carry out separating.
Aqueous solution nitrite concentration is measured with liquid chromatograph, aqueous solution nitrite concentration is 1.38ppm, turns
Rate is 86.2%.
A kind of new catalyst Er of embodiment 33+:Y3Al5O12/mMBIP
(1) Er3+:Y3Al5O12The preparation of/mMBIP
The preparation of 1.mMBIP：By 100mL H3PO4(12M) pour beaker into, the Bi (NO with 10mmol3)3·6H2O mixes,
Magnetic agitation 1h at room temperature, obtains suspension, the suspension obtaining is put in politef stainless steel cauldron, in 200
Hydro-thermal reaction 72h at DEG C.Reactant is naturally cooled to room temperature, filters, distilled water cleans, dry 24h in 80 DEG C, obtain white
Powder, as has the BiPO of hexagonal phase crystal formation4(being designated as mMBIP).
2.Er3+:Y3Al5O12Preparation：With embodiment 1.
3. by 0.3g Er3+:Y3Al5O12BiPO with 1.0g hexagonal phase crystal formation4It is placed in beaker, add 50mL deionization
Water, carries out ultrasonic disperse 15min-20min.At 60 DEG C, under magnetic agitation, heat 30min, filter, distilled water cleans, filtrate
Put crucible into, be placed in Muffle furnace, with 300 DEG C of roasting 2h, 2 DEG C/min of heat rate, obtain target product Er3+:Y3Al5O12/
mMBIP.
(2) characterize data
MMBIP and Er of preparation3+:Y3Al5O12The XRD of/mMBIP as shown in figures 4 a and 4b, is found out by Fig. 4 a, mMBIP
Characteristic peak 2 θ=18.5 °, 22.8 °, 37.0 ° are met with standard card JCPDS 43-0637, are indicated above the sample after heat treatment
For single cube structure, other dephasigns do not occur.Er be can be seen that by Fig. 4 b3+:Y3Al5O12/ mMBIP complex is same
When there is mMBIP and Er3+:Y3Al5O12Characteristic peak, have no other dephasigns occur, this illustrate Er3+:Y3Al5O12Multiple with mMBIP
Close and crystal structure is not produced with obvious impact.
MMBIP and Er of preparation3+:Y3Al5O12The SEM of/mMBIP as illustrated in fig. 4 c, is found out by Fig. 4 c, and MBIP cuboid is tied
Long 1.0-1.5 μm wide 50-100nm is high for 1.5-2.0 μm of structure, and light conversion agent is evenly distributed on its surface in spherical, and composite catalyzing is described
Agent is successfully prepared.
(3) Nitrite transformation method
In the test tube of light-catalyzed reaction instrument, add 50mL nitrite solution (10ppm) and 50mg catalyst Er3+:
Y3Al5O12/ mMBIP, under room temperature simulated solar illumination, opens magnetic agitation, reacts 0.5～6 hour, reaction finishes, and will urge
Agent and solution carry out separating.
Aqueous solution nitrite concentration is measured with liquid chromatograph, aqueous solution nitrite concentration is 1.55ppm, turns
Rate is 84.5%.
Claims (7)
1. a kind of new catalyst Er:Y3Al5O12/BiPO4It is characterised in that preparation method is as follows：By Er3+:Y3Al5O12With
BiPO4After mixing, add deionized water, ultrasonic disperse 15-30min, under stirring, heat 30-40min in 50-60 DEG C, filter,
Cleaning, is placed in Muffle furnace, in 280-320 DEG C of roasting 2-3h, obtains target product.
2. a kind of new catalyst Er according to claim 1:Y3Al5O12/BiPO4It is characterised in that Er3+:Y3Al5O12
And BiPO4Weight than for 0.25-0.35:1.
3. a kind of new catalyst Er according to claim 1 and 2:Y3Al5O12/BiPO4It is characterised in that it is described
BiPO4Preparation method be：By H3PO4With Bi (NO3)3·6H2O mixes, and magnetic agitation 1-2h at room temperature obtains suspension, will
Suspension is put in politef stainless steel cauldron, hydro-thermal reaction 70-75h at 20-200 DEG C, and reactant filters, clearly
Wash, be dried, obtain target product.
4. a kind of new catalyst Er according to claim 1 and 2:Y3Al5O12/BiPO4It is characterised in that it is described
Er3+:Y3Al5O12Preparation method be：In nitric acid, by Er:Y3Al5O12In ratio add Er2O3And Y2O3, dissolve and heat
Stir to water white transparency, obtain rare-earth ion solution；By Er:Y3Al5O12In ratio weigh Al (NO3)3·9H2O is dissolved in distillation
In water, then at room temperature, it is slowly added in rare-earth ion solution, after mix homogeneously, add citric acid, add at 50-60 DEG C
Thermal agitation, stops when solution is in thick, obtains the glutinous colloidal solution that foams, and glutinous for foaming colloidal solution is put into baking oven, in 95-
105 DEG C of heating 23-25h, obtain foam sol, the foam sol obtaining are heated 40-60min at 500 DEG C, then at 1100 DEG C
Calcining 100-150min, cooling, obtain Er:Y3Al5O12Powder.
5. a kind of new catalyst Er according to claim 4:Y3Al5O12/BiPO4It is characterised in that in molar ratio, lemon
Lemon acid:Rare earth ion=3-4:1.
6. a kind of new catalyst Er described in claim 1 or 2:Y3Al5O12/BiPO4In conversion Nitrite
Application.
7. application according to claim 6 is it is characterised in that method is as follows：In the aqueous solution containing nitrite, plus
Enter the catalyst Er described in claim 1 or 2:Y3Al5O12/BiPO4It is seen that reacting 0.5-6h under light.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610896753.4A CN106475121A (en) | 2016-10-13 | 2016-10-13 | A kind of new catalyst Er: Y3Al5O12/BiPO4And its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610896753.4A CN106475121A (en) | 2016-10-13 | 2016-10-13 | A kind of new catalyst Er: Y3Al5O12/BiPO4And its preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106475121A true CN106475121A (en) | 2017-03-08 |
Family
ID=58269360
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610896753.4A Pending CN106475121A (en) | 2016-10-13 | 2016-10-13 | A kind of new catalyst Er: Y3Al5O12/BiPO4And its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106475121A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109078645A (en) * | 2018-09-04 | 2018-12-25 | 辽宁大学 | A kind of photochemical catalyst and its preparation method and application of novel cladding Z-type structure |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101502795A (en) * | 2009-03-17 | 2009-08-12 | 江苏工业学院 | Photocatalysis nano material with energy conversion and preparation method thereof |
| CN102078807A (en) * | 2011-01-05 | 2011-06-01 | 吉林大学 | Er<3+>:YAlO3/TiO2-loaded photocatalyst and preparation method thereof |
| CN102311734A (en) * | 2011-09-23 | 2012-01-11 | 辽宁大学 | Upconversion UV (ultraviolet) luminescent material of broadband spectral adsorption and application thereof |
| CN102895965A (en) * | 2012-10-31 | 2013-01-30 | 辽宁大学 | Er<3+>: Y3Al5O12/TiO2 composite membrane and application thereof in catalytic degradation of organic dye |
| CN104399461A (en) * | 2014-11-25 | 2015-03-11 | 赤峰学院 | Upconversion luminescence nanometer photocatalyst and application of nanometer photocatalyst in hydrogen generation by hydrolysis |
-
2016
- 2016-10-13 CN CN201610896753.4A patent/CN106475121A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101502795A (en) * | 2009-03-17 | 2009-08-12 | 江苏工业学院 | Photocatalysis nano material with energy conversion and preparation method thereof |
| CN102078807A (en) * | 2011-01-05 | 2011-06-01 | 吉林大学 | Er<3+>:YAlO3/TiO2-loaded photocatalyst and preparation method thereof |
| CN102311734A (en) * | 2011-09-23 | 2012-01-11 | 辽宁大学 | Upconversion UV (ultraviolet) luminescent material of broadband spectral adsorption and application thereof |
| CN102895965A (en) * | 2012-10-31 | 2013-01-30 | 辽宁大学 | Er<3+>: Y3Al5O12/TiO2 composite membrane and application thereof in catalytic degradation of organic dye |
| CN104399461A (en) * | 2014-11-25 | 2015-03-11 | 赤峰学院 | Upconversion luminescence nanometer photocatalyst and application of nanometer photocatalyst in hydrogen generation by hydrolysis |
Non-Patent Citations (4)
| Title |
|---|
| YUNFAN ZHANG ET AL: ""Enhanced solar photocatalytic activity of Er3+:YAlO3-loaded BiPO4 composite"", 《JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY》 * |
| 何燧源等: "《环境化学 第4版》", 28 February 2005, 华东理工大学出版社 * |
| 董丽红等: "《两亲分子在纳米技术领域中的应用》", 31 October 2013, 吉林大学出版社 * |
| 贾瑛等: "《推进剂污染与治理》", 31 January 2016, 北京航空航天大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109078645A (en) * | 2018-09-04 | 2018-12-25 | 辽宁大学 | A kind of photochemical catalyst and its preparation method and application of novel cladding Z-type structure |
| CN109078645B (en) * | 2018-09-04 | 2021-04-30 | 辽宁大学 | Photocatalyst coated with Z-shaped structure and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101890354B (en) | Method for preparing bismuth ferrite photocatalyst | |
| CN105642299B (en) | A kind of cadmium ferrite/clay nano structural composite material and its preparation method and application of nickel doping | |
| Wang et al. | Chemical co-precipitation synthesis and properties of pure-phase BiFeO3 | |
| CN102489324B (en) | F and N co-doped visible-light response bismuth vanadate photocatalyst and preparation method thereof | |
| CN105964250B (en) | It is a kind of with visible light-responded Ag10Si4O13Photochemical catalyst and its preparation method and application | |
| CN105195198B (en) | A kind of mpg-C3N4/Bi0.9Nd0.1VO4Composite photo-catalyst and its preparation method and application | |
| CN105668632A (en) | Variable valency metal catalyzed and doped tungsten bronze nano-short rod particle and preparation method thereof | |
| CN107159223B (en) | A kind of cobalt acid lanthanum/attapulgite/redox graphene nanostructure composite material and its preparation method and application | |
| CN102553565A (en) | Preparation of bismuth vanadate visible light photocatalysis material with cotton fiber as template | |
| CN107185547A (en) | A kind of C/Fe FeVO4Composite photo-catalyst and its preparation method and application | |
| CN113083277B (en) | Preparation method and application of nano ZnO rich in oxygen vacancy for photocatalytic reduction of hexavalent uranium | |
| CN106111108A (en) | The preparation method of a kind of nanometer doped zinc oxide and the application in photocatalysis direction thereof | |
| CN110605128A (en) | CoTiO (cobalt-titanium oxide)3/Bi4NbO8Preparation method of Cl composite photocatalyst material | |
| CN106732588B (en) | The catalyst and its preparation method and application of Cr (VI) in a kind of conversion aqueous solution | |
| CN106475121A (en) | A kind of new catalyst Er: Y3Al5O12/BiPO4And its preparation method and application | |
| WO2021136228A1 (en) | Method for preparing copper ferrite/zeolite spinel composite material and use thereof | |
| CN111013565B (en) | Ytterbium and erbium doped titanium dioxide/attapulgite nano composite material and preparation method and application thereof | |
| CN101219375A (en) | Process for producing composite photocatalysis material containing rare earth element | |
| CN105148899B (en) | A kind of rare earth codope BiVO with upper transfer characteristic4Photochemical catalyst and its preparation method and application | |
| CN107159280A (en) | A kind of catalyst for converting aqueous solution nitrite and its preparation method and application | |
| CN108273522B (en) | A kind of Z-type semiconductor light-catalyst and its preparation method and application with trapezium structure | |
| CN110171811A (en) | A kind of preparation method of heat-staple cupric phosphate crystalline nanometric materials | |
| CN104328479B (en) | The method that the water-heat process utilizing glycerol to modulate synthesizes (010) preferred orientation bismuth vanadate powder | |
| CN113101932B (en) | Preparation method and application of microwave-ultraviolet light catalyst | |
| CN109384262A (en) | A kind of sheet Li4Mn5O12The preparation method of ion sieve presoma and ion sieve |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170308 |