CN107308963A - A kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst - Google Patents
A kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst Download PDFInfo
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- CN107308963A CN107308963A CN201710561911.5A CN201710561911A CN107308963A CN 107308963 A CN107308963 A CN 107308963A CN 201710561911 A CN201710561911 A CN 201710561911A CN 107308963 A CN107308963 A CN 107308963A
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- phosphate
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- basic zirconium
- catalyst
- indium
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- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- UJXZVRRCKFUQKG-UHFFFAOYSA-K indium(3+);phosphate Chemical compound [In+3].[O-]P([O-])([O-])=O UJXZVRRCKFUQKG-UHFFFAOYSA-K 0.000 title claims abstract description 25
- 229910000166 zirconium phosphate Inorganic materials 0.000 title claims abstract description 24
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 12
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008346 aqueous phase Substances 0.000 claims abstract description 12
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims abstract description 6
- 235000019832 sodium triphosphate Nutrition 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000005829 trimerization reaction Methods 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- QAKNNONVLHYVFR-UHFFFAOYSA-N [In].OP(O)(O)=O Chemical compound [In].OP(O)(O)=O QAKNNONVLHYVFR-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910001449 indium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-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
- 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
- B01J27/1811—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 gallium, indium or thallium
-
- B01J35/39—
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The present invention discloses the preparation method that a kind of tabular basic zirconium phosphate loads indium phosphate catalyst, comprises the following steps：Zirconium chloride is dissolved in water and is configured to concentration for 0.1 0.5mol/L chlorination zirconium solutions, using the solution as aqueous phase, according to TrionX 100: n-butanol: hexamethylene: aqueous phase mass ratio is stirred preparation microemulsion for 1: 2~20: 2~40: 0.2~0.4, indiumchloride solution is added dropwise when stirring microemulsion, after being added dropwise to complete, sodium tripolyphosphate solution is instilled again, continue to stir after being added dropwise to complete, finally centrifuge, solid is washed with ethanol, vacuum drying, that is, be made tabular basic zirconium phosphate load indium phosphate catalyst.
Description
Technical field
The present invention relates to technical field of sewage in environmental protection, and in particular to a kind of tabular basic zirconium phosphate loads indium phosphate
The preparation method of catalyst.
Background technology
Traditional method for treating water efficiency is low, cost is high, there are secondary pollution problems, and waste water control always cannot be well
Solution.The development and application of nanometer technology are likely to thoroughly solve this problem.Start within 1972 to find TiO2Oxidation activity
Higher, chemical stability is good, harmless to the human body, and cost is low, pollution-free, has a wide range of application, thus is most paid attention to, but TiO2
Larger (such as anatase TiO of energy gap2Energy gap Eg=3.2eV), be only capable of absorb ultraviolet region (wavelength is less than
Light 387nm), the utilization ratio to solar energy is relatively low.
In contaminant degradation and production of energy field, conductor photocatalysis is one of most promising method.Work as energy
Amount will produce point of electron-hole pair when being more than or equal to the photon irradiation of semiconductor energy gap in photocatalyst surface
From this is the initial basic step of light-catalyzed reaction.In order to find efficient photochemical catalyst, numerous studies work is all concentrated on
In the influence factor for studying photocatalytic activity.And it is an endless job to improve photocatalysis effect.Further, since nanometer
Grain is difficult to be separated from waste water after processing waste water, it is therefore desirable to which nano particle is supported on some carriers.Basic zirconium phosphate is one
Kind common support materials, can as catalyst carrier, but its general Composite mechanism be by directly being covered in carrier surface,
And this contact is physical contact, it is easy to which coming off causes catalyst loss.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to propose a kind of tabular basic zirconium phosphate load indium phosphate catalyst
Preparation method, this method be carrier surface formation catalyst, catalyst and carrier are combined closely.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst, comprises the following steps:
(1) weigh a certain amount of zirconium chloride and be dissolved in water, be configured to the chlorination zirconium solution that concentration is 0.1-0.5mol/L；
(2) by the chlorination zirconium solution of step (1) as aqueous phase, according to TrionX-100: n-butanol: hexamethylene: aqueous phase matter
Amount for 1: 2~20: 2~40: 0.2~0.4 progress preparation than stirring into microemulsion；
(3) 10~15mL of microemulsion obtained by step (2) is taken, 5~15mL concentration is instilled into microemulsion while stirring is
0.1~0.5mol/L inidum chloride, after being added dropwise to complete, then instills the sodium tripolyphosphate that 5~15mL concentration is 0.5~0.8mol/L
Solution, continues to stir 50~70min with identical rotating speed after being added dropwise to complete；
(4) centrifuge, solid is washed with ethanol 3~4 times, vacuum drying is made tabular basic zirconium phosphate load indium phosphate
Catalyst.
Preferably, the rotating speed in step (3) is 200-400r/s.
Preferably, vacuum drying temperature is 82-86 DEG C in step (4).
Preferably, concentration of alcohol is 95-97% in step (4).
The beneficial effects of the invention are as follows：(1) sodium tripolyphosphate combines nucleation with zirconium part first, recycles sodium tripolyphosphate
Aggregation features, obtain the indium phosphate catalyst using basic zirconium phosphate as carrier.(2) the not common ground and mixed of load of the invention,
Nor simple surface deposition, but the phosphate radical and indium ion in carrier body are combined, and indium phosphate crystal is formed on surface,
It is this to be firmly combined with, make indium phosphate difficult for drop-off, and specific surface area increases, and can obtain good catalytic effect.
Embodiment
Embodiment 1
A kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst, comprises the following steps:
Weigh 11.65g zirconium chlorides to be dissolved in 100mL water, be configured to the chlorination zirconium solution that concentration is 0.5mol/L；By chlorination
Zirconium solution is as aqueous phase, according to TrionX-100: n-butanol: hexamethylene: aqueous phase mass ratio is 1: 2: 2: 0.2 progress preparation stirring
Into microemulsion；15mL microemulsions are taken, in the case where rotating speed is 400-r/s, are stirred while instillation concentration is into microemulsion
0.5mol/L, volume 5mL indiumchloride solution after being added dropwise to complete, then instills concentration for 0.8mol/L, volume 15mL trimerization phosphorus
Acid sodium solution, continues to stir 70min in 400r/s rotating speed after being added dropwise to complete；Finally centrifuge, wash solid with 97% ethanol
Body 3 times, the vacuum drying at 86 DEG C is made tabular basic zirconium phosphate load indium phosphate catalyst.
Application test 1
Weigh obtained 1g tabulars basic zirconium phosphate load indium phosphate catalyst and be added to the acid red that 300mL concentration is 40mg/L
In waste water, under 120W LED irradiation, 30min is reacted, percent of decolourization is 96.6%, after catalyst is separated from waste water also
It can reuse.
Embodiment 2
A kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst, comprises the following steps:
Weigh 2.33g zirconium chlorides to be dissolved in 100mL water, be configured to the chlorination zirconium solution that concentration is 0.1mol/L；By chlorination
Zirconium solution is as aqueous phase, according to TrionX-100: n-butanol: hexamethylene: aqueous phase mass ratio is that 1: 20: 40: 0.4 progress preparation is stirred
Mix microemulsion；10mL microemulsions are taken, in the case where rotating speed is 200r/s, are stirred while instillation concentration is into microemulsion
0.1mol/L, volume 5mL indiumchloride solution after being added dropwise to complete, then instills concentration for 0.5mol/L, volume 5mL trimerization phosphorus
Acid sodium solution, continues to stir 50min in 200r/s rotating speed after being added dropwise to complete；Finally centrifuge, wash solid with 95% ethanol
Body 4 times, the vacuum drying at 82 DEG C is made tabular basic zirconium phosphate load indium phosphate catalyst.
Application test 2
Weigh obtained 1g tabulars basic zirconium phosphate load indium phosphate catalyst and be added to the gold orange 7 that 300mL concentration is 40mg/L
In waste water, under 120W LED irradiation, 30min is reacted, percent of decolourization is 97.2%, can be reused after catalyst separation.
For identical waste water under the same conditions, the degradation efficiency of pure phosphoric acid indium is 89.1%, but due to being pure phosphoric acid indium, is urged
The consumption of indium is very big in agent, is economically difficult to bear.
Embodiment 3
A kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst, comprises the following steps:
Weigh 6.99g zirconium chlorides to be dissolved in 100mL water, be configured to the chlorination zirconium solution that concentration is 0.3mol/L；By chlorination
Zirconium solution is as aqueous phase, according to TrionX-100: n-butanol: hexamethylene: aqueous phase mass ratio is that 1: 10: 20: 0.3 progress preparation is stirred
Mix microemulsion；12mL microemulsions are taken, in the case where rotating speed is 300r/s, are stirred while instillation concentration is into microemulsion
0.3mol/L, volume 10mL indiumchloride solution after being added dropwise to complete, then instills concentration for 0.6mol/L, volume 10mL trimerization
Sodium radio-phosphate,P-32 solution, continues to stir 70min in 400r/s rotating speed after being added dropwise to complete；Finally centrifuge, washed with 97% ethanol
Solid 3 times, the vacuum drying at 84 DEG C is made tabular basic zirconium phosphate load indium phosphate catalyst.
Application test 3
Weigh obtained 1g tabulars basic zirconium phosphate load indium phosphate catalyst and be added to the rhodamine that 300mL concentration is 40mg/L
In B waste water, under 120W LED irradiation, 30min is reacted, percent of decolourization is 95.9%, after catalyst is separated from waste water also
It can reuse.
Claims (4)
1. a kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst, it is characterised in that comprise the following steps:
(1) weigh a certain amount of zirconium chloride and be dissolved in water, be configured to the chlorination zirconium solution that concentration is 0.1-0.5mol/L；
(2) by the chlorination zirconium solution of step (1) as aqueous phase, according to TrionX-100: n-butanol: hexamethylene: aqueous phase mass ratio
Microemulsion is stirred into for 1: 2~20: 2~40: 0.2~0.4 progress preparation；
(3) take 10~15mL of microemulsion obtained by step (2), instilled while stirring into microemulsion 5~15mL concentration be 0.1~
0.5mol/L inidum chloride, after being added dropwise to complete, then instill 5~15mL concentration be 0.5~0.8mol/L sodium tripolyphosphate solution,
Continue to stir 50~70min with identical rotating speed after being added dropwise to complete；
(4) centrifuge, solid is washed with ethanol 3~4 times, vacuum drying is made the load indium phosphate catalysis of tabular basic zirconium phosphate
Agent.
2. tabular basic zirconium phosphate according to claim 1 loads the preparation method of indium phosphate catalyst, it is characterised in that step
(3) rotating speed in is 200-400r/s.
3. tabular basic zirconium phosphate according to claim 1 loads the preparation method of indium phosphate catalyst, it is characterised in that step
(4) vacuum drying temperature is 82-86 DEG C in.
4. tabular basic zirconium phosphate according to claim 1 loads the preparation method of indium phosphate catalyst, it is characterised in that step
(4) concentration of alcohol is 95-97% in.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710561911.5A CN107308963A (en) | 2017-07-11 | 2017-07-11 | A kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710561911.5A CN107308963A (en) | 2017-07-11 | 2017-07-11 | A kind of tabular basic zirconium phosphate loads the preparation method of indium phosphate catalyst |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040203A (en) * | 2010-11-19 | 2011-05-04 | 安徽师范大学 | Preparation method and application of nano nickel phosphide |
| CN103464186A (en) * | 2013-09-29 | 2013-12-25 | 天津工业大学 | Lead phosphate and silver phosphate composite photocatalyst and preparation method thereof |
| CN105018089A (en) * | 2015-07-06 | 2015-11-04 | 河北大学 | Phosphate or metaphosphate based visible-ultraviolet up-conversion luminescence material doped with rare earth ions, and preparation method and application thereof |
| CN105645371A (en) * | 2016-01-08 | 2016-06-08 | 西南大学 | One-step preparation method and application of nano transition metal phosphates |
| CN106540722A (en) * | 2016-10-19 | 2017-03-29 | 常州大学 | A kind of preparation method of hollow structure yttrium phosphate catalyst |
-
2017
- 2017-07-11 CN CN201710561911.5A patent/CN107308963A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040203A (en) * | 2010-11-19 | 2011-05-04 | 安徽师范大学 | Preparation method and application of nano nickel phosphide |
| CN103464186A (en) * | 2013-09-29 | 2013-12-25 | 天津工业大学 | Lead phosphate and silver phosphate composite photocatalyst and preparation method thereof |
| CN105018089A (en) * | 2015-07-06 | 2015-11-04 | 河北大学 | Phosphate or metaphosphate based visible-ultraviolet up-conversion luminescence material doped with rare earth ions, and preparation method and application thereof |
| CN105645371A (en) * | 2016-01-08 | 2016-06-08 | 西南大学 | One-step preparation method and application of nano transition metal phosphates |
| CN106540722A (en) * | 2016-10-19 | 2017-03-29 | 常州大学 | A kind of preparation method of hollow structure yttrium phosphate catalyst |
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Application publication date: 20171103 |
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