CN106513025A - Method for preparing yttrium phosphate/silver phosphate composite catalyst - Google Patents
Method for preparing yttrium phosphate/silver phosphate composite catalyst Download PDFInfo
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- CN106513025A CN106513025A CN201610912917.8A CN201610912917A CN106513025A CN 106513025 A CN106513025 A CN 106513025A CN 201610912917 A CN201610912917 A CN 201610912917A CN 106513025 A CN106513025 A CN 106513025A
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- Prior art keywords
- phosphate
- yttrium
- concentration
- silver
- 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.)
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- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 24
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- UXBZSSBXGPYSIL-UHFFFAOYSA-K yttrium(iii) phosphate Chemical compound [Y+3].[O-]P([O-])([O-])=O UXBZSSBXGPYSIL-UHFFFAOYSA-K 0.000 title claims abstract description 20
- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 title claims abstract description 17
- 229940019931 silver phosphate Drugs 0.000 title abstract 5
- 229910000161 silver phosphate Inorganic materials 0.000 title abstract 5
- 238000000034 method Methods 0.000 title abstract 3
- 238000003756 stirring Methods 0.000 claims abstract description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 8
- DEXZEPDUSNRVTN-UHFFFAOYSA-K yttrium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Y+3] DEXZEPDUSNRVTN-UHFFFAOYSA-K 0.000 claims abstract description 8
- 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 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims abstract description 6
- 235000019799 monosodium phosphate Nutrition 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 6
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract 2
- 229910021641 deionized water Inorganic materials 0.000 claims abstract 2
- 239000007787 solid Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 claims description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 2
- 235000019800 disodium phosphate Nutrition 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 238000001782 photodegradation Methods 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- YYYARFHFWYKNLF-UHFFFAOYSA-N 4-[(2,4-dimethylphenyl)diazenyl]-3-hydroxynaphthalene-2,7-disulfonic acid Chemical compound CC1=CC(C)=CC=C1N=NC1=C(O)C(S(O)(=O)=O)=CC2=CC(S(O)(=O)=O)=CC=C12 YYYARFHFWYKNLF-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 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 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 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
- 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
- B01J27/1817—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 copper, silver or gold
-
- 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
Landscapes
- 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 method for preparing a yttrium phosphate/silver phosphate composite catalyst. The method for preparing the yttrium phosphate/silver phosphate composite catalyst comprises the following steps sequentially: dropwise adding 3mL to 6mL of ammonia water with the mass percent of 15% to 25% into 5mL of yttrium nitrate solution with the concentration of 0.2mol/L to 0.3mol/L, so as to obtain a yttrium hydroxide black colloidal solution; measuring off 1mL of 20mmol/L silver nitrate solution and 1mL to 10mL of 20mmol/L disodium hydrogen phosphate solution, carrying out mixing at the revolution rate of 350rpm to 400rpm, and carrying out continuous stirring for 3 to 4 hours, so as to produce silver phosphate and form a green-yellow colloidal solution; and mixing the obtained green-yellow colloidal solution and the black colloidal solution with continuous stirring, then, adding 5mL to 8mL of sodium dihydrogen phosphate solution with the concentration of 0.2mol/L to 0.3mol/L into the mixture, continuing to carry out stirring for 3 hours, carrying out precipitating, carrying out solid-liquid separation, carrying out washing for 3 to 5 times with deionized water, and carrying out baking at the temperature of 100 DEG C to 105 DEG C, thereby obtaining the yttrium phosphate/silver phosphate composite catalyst. The prepared catalyst has a relatively good crystal structure, is stable and is high in photodegradation treatment efficiency.
Description
Technical field
A kind of the present invention relates to novel environmental pollution control material field, more particularly to yttrium phosphate/silver orthophosphate composite catalyst
Preparation method.
Background technology
With the development of science and technology, the murder by poisoning organic pollution produced in industrial and agricultural production seriously threatens environment and people
The health of class, seeks a kind of new and effective environmental improvement technology and has great importance.Photocatalysis technology is because of its energy-conservation, height
Effect, contaminant degradation are thorough, non-secondary pollution advantage, have become a kind of emerging environmental improvement with important application prospect at present
Technology.In recent years, the development of new and effective visible-light photocatalyst becomes an important research content in photocatalysis technology,
The wherein catalysis material with surface plasma resonance effect, because of its unique Surface Physical Chemistry property and efficient visible
Light photocatalysis performance, becomes one of focus of research.
However, the visible-light photocatalysis material reported at present is most with higher photo-generated carrier recombination rate and poor
Visible absorption, cause its quantum efficiency relatively low.Therefore, new and effective visible-light photocatalysis material is developed, expands semiconductor
Material spectrum response range and promotion light induced electron and hole are efficiently separated, and are become current catalysis material research field and are badly in need of
The problem in science of solution.
The content of the invention
The purpose of the present invention is for overcoming the shortcomings of in prior art during photocatalytic pollutant degradation, there is provided a kind of phosphorus
The preparation method of sour yttrium/silver orthophosphate composite catalyst.
For this purpose, the invention provides technical scheme below, a kind of preparation method of yttrium phosphate/silver orthophosphate composite catalyst,
In turn include the following steps：
1) it is 15%～25% 3～6mL mass fractions to be added dropwise in the yttrium nitrate solution that 5mL concentration is 0.2～0.3mol/L
Ammoniacal liquor, obtain yttrium hydroxide black colloidal solution；
2) the silver nitrate solution 1mL that concentration is 20mmol/L and the disodium phosphate soln 1 that concentration is 20mmol/L are measured
～10mL, mixes under 350～400 revs/min of rotating speed, persistently stirs 3～4h, generates silver orthophosphate formation yellow green colloid molten
Liquid；
3) the yellow green colloidal solution for obtaining and black colloidal solution are mixed into 20～30min under continuous stirring, then plus
Enter the sodium dihydrogen phosphate that 5-8mL concentration is 0.2～0.3mol/L, continue stirring 3h, precipitation, separation of solid and liquid use deionization
Water washing 3～5 times, dries at 100～105 DEG C, obtains yttrium phosphate/silver orthophosphate composite catalyst.
Compared with traditional catalyst, the present invention has following superiority：Yttrium hydroxide black colloidal solution (band during being somebody's turn to do
Positive electricity) and (negatively charged) institute of yellow green phosphoric acid silver colloidal solution it is electrically charged conversely, colloidal solid be combined with each other under electrostatic interaction,
It is dispersed.Yttrium hydroxide generates yttrium phosphate under conditions of with the presence of hydrogen phosphate.Obtained catalyst has preferable crystalline substance
Body structure, stable, light degradation treatment effeciency is high.
Specific embodiment
Describe the present invention with reference to embodiment in detail, but the present invention is not limited to this.
Embodiment 1
The ammoniacal liquor that 6mL mass fractions are 25% is added dropwise in 5mL concentration for the yttrium nitrate solution of 0.3mol/L, obtain hydroxide
Yttrium black colloidal solution；Measure the silver nitrate solution 1mL that concentration is 20mmol/L and the disodium hydrogen phosphate that concentration is 20mmol/L
Solution 10mL, mixes under 400 revs/min of rotating speed, persistently stirs 4h, generates silver orthophosphate and forms yellow green colloidal solution；Will
The yellow green colloidal solution and black colloidal solution for obtaining mixes 30min under continuous stirring, adds 8mL concentration and is
The sodium dihydrogen phosphate of 0.3mol/L, continues stirring 3h, and precipitation, separation of solid and liquid are washed with deionized 5 times, at 105 DEG C
Drying, obtains yttrium phosphate/silver orthophosphate composite catalyst.
Obtained yttrium phosphate/silver orthophosphate composite catalyst is used for processing waste water containing acid scarlet：0.5g yttrium phosphates/phosphoric acid
Silver-colored composite catalyst is added in the acid scarlet waste water that 100mL concentration is 20mg/L, under the irradiation of 300w Metal halogen lamps, reaction
0.5h, percent of decolourization are 97.8%.
Embodiment 2
The ammoniacal liquor that 3mL mass fractions are 15% is added dropwise in 5mL concentration for the yttrium nitrate solution of 0.2mol/L, obtain hydroxide
Yttrium black colloidal solution；Measure the silver nitrate solution 1mL that concentration is 20mmol/L and the disodium hydrogen phosphate that concentration is 20mmol/L
Solution 1mL, mixes under 350 revs/min of rotating speed, persistently stirs 3h, generates silver orthophosphate and forms yellow green colloidal solution；Will
To yellow green colloidal solution and black colloidal solution mix 20min under continuous stirring, add 5mL concentration for 0.2mol/L
Sodium dihydrogen phosphate, continue stirring 3h, precipitation, separation of solid and liquid is washed with deionized 3 times, dries, obtain at 100 DEG C
To yttrium phosphate/silver orthophosphate composite catalyst.
Obtained yttrium phosphate/silver orthophosphate composite catalyst is used for processing wastewater containing methylene blue：0.5g yttrium phosphates/phosphoric acid
Silver-colored composite catalyst is added in the methylene blue waste water that 100mL concentration is 20mg/L, under the irradiation of 300w Metal halogen lamps, reaction
0.5h, percent of decolourization are 99.0%.
Embodiment 3
The ammoniacal liquor that 6mL mass fractions are 25% is added dropwise in 5mL concentration for the yttrium nitrate solution of 0.3mol/L, obtain hydroxide
Yttrium black colloidal solution；Measure the silver nitrate solution 1mL that concentration is 20mmol/L and the disodium hydrogen phosphate that concentration is 20mmol/L
Solution 8mL, mixes under 400 revs/min of rotating speed, persistently stirs 4h, generates silver orthophosphate and forms yellow green colloidal solution；Will
To yellow green colloidal solution and black colloidal solution mix 30min under continuous stirring, add 8mL concentration for 0.3mol/L
Sodium dihydrogen phosphate, continue stirring 3h, precipitation, separation of solid and liquid is washed with deionized 5 times, dries, obtain at 105 DEG C
To yttrium phosphate/silver orthophosphate composite catalyst.
Obtained yttrium phosphate/silver orthophosphate composite catalyst is used for processing the waste water of II containing gold orange：0.5g yttrium phosphates/silver orthophosphate
Composite catalyst is added in the gold orange II waste water that 100mL concentration is 20mg/L, under the irradiation of 300w Metal halogen lamps, reacts 0.5h,
Percent of decolourization is 99.1%.
Claims (1)
1. the preparation method of a kind of yttrium phosphate/silver orthophosphate composite catalyst, it is characterised in that：In turn include the following steps：
1) ammonia that 3～6mL mass fractions are 15%～25% is added dropwise in the yttrium nitrate solution that 5mL concentration is 0.2～0.3mol/L
Water, obtains yttrium hydroxide black colloidal solution；
2) silver nitrate solution 1mL that concentration is 20mmol/L and concentration are measured for 20mmol/L disodium phosphate soln 1～
10mL, mixes under 350～400 revs/min of rotating speed, persistently stirs 3～4h, generates silver orthophosphate formation yellow green colloid molten
Liquid；
3) the yellow green colloidal solution for obtaining and black colloidal solution are mixed into 20～30min under continuous stirring, adds 5-
8mL concentration is the sodium dihydrogen phosphate of 0.2～0.3mol/L, continues stirring 3h, and precipitation, separation of solid and liquid are washed with deionized water
Wash 3～5 times, dry at 100～105 DEG C, obtain yttrium phosphate/silver orthophosphate composite catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610912917.8A CN106513025B (en) | 2016-10-19 | 2016-10-19 | A kind of preparation method of yttrium phosphate/silver orthophosphate composite catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610912917.8A CN106513025B (en) | 2016-10-19 | 2016-10-19 | A kind of preparation method of yttrium phosphate/silver orthophosphate composite catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106513025A true CN106513025A (en) | 2017-03-22 |
| CN106513025B CN106513025B (en) | 2018-10-19 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013185328A1 (en) * | 2012-06-14 | 2013-12-19 | East China University Of Science And Technology | Photocatalytic compositions and methods for their preparation and use |
| CN105233823A (en) * | 2015-10-19 | 2016-01-13 | 桂林理工大学 | Visible light responsive photocatalyst AgYW2O8 and preparation method thereof |
-
2016
- 2016-10-19 CN CN201610912917.8A patent/CN106513025B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013185328A1 (en) * | 2012-06-14 | 2013-12-19 | East China University Of Science And Technology | Photocatalytic compositions and methods for their preparation and use |
| CN105233823A (en) * | 2015-10-19 | 2016-01-13 | 桂林理工大学 | Visible light responsive photocatalyst AgYW2O8 and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| LIN LUO等: "Visible photocatalysis and photostability of Ag3PO4 photocatalyst", 《APPLIED SURFACE SCIENCE》 * |
| 刘健梅等: "Ｙ－ＴｉＯ２光催化剂的制备与性能研究", 《功能材料》 * |
| 马世昌: "《化学物质辞典》", 30 April 1999 * |
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