CN104495777B - Polyhedral silver phosphate nano material and preparation method thereof - Google Patents
Polyhedral silver phosphate nano material and preparation method thereof Download PDFInfo
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- CN104495777B CN104495777B CN201410827832.0A CN201410827832A CN104495777B CN 104495777 B CN104495777 B CN 104495777B CN 201410827832 A CN201410827832 A CN 201410827832A CN 104495777 B CN104495777 B CN 104495777B
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 42
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 30
- 229910000161 silver phosphate Inorganic materials 0.000 title claims abstract description 26
- 229940019931 silver phosphate Drugs 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 23
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 12
- 239000010452 phosphate Substances 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 238000009938 salting Methods 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000012153 distilled water Substances 0.000 description 12
- 229910000474 mercury oxide Inorganic materials 0.000 description 8
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000001488 sodium phosphate Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 3
- 235000019799 monosodium phosphate Nutrition 0.000 description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 description 3
- 235000011008 sodium phosphates Nutrition 0.000 description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 3
- 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 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- Catalysts (AREA)
Abstract
The invention belongs to catalysis material technical field, more particularly to a kind of polyhedral silver phosphate nano material and preparation method thereof.The present invention adds in triethanolamine in silver nitrate solution, stirs evenly, obtains mixed solution；Phosphate solution is added in the mixed solution while stirring, after completion of dropwise addition, after 5~30min of normal-temperature reaction, centrifugation takes precipitation, dries, obtains polyhedral silver phosphate nano material；Silver nitrate is 3 with phosphatic molar ratio:1, the molar ratio of triethanolamine and silver nitrate is 1:12~1:14.The present invention uses conventional reagent triethanolamine, by controlling silver nitrate and phosphatic concentration, so as to fulfill the regulation and control of silver orthophosphate pattern.The preparation method of the present invention is simply easily achieved, and is not required traditional two-step method, a step that can synthesize polyhedral silver phosphate nano material, be can be applied to industrialized production.
Description
Technical field
The invention belongs to catalysis material technical field, more particularly to a kind of polyhedral silver phosphate nano material and its preparation
Method.
Background technology
The more traditional water technology of photocatalysis technology is with reaction condition is mild, speed is fast, efficient, simple for process clean
The advantages that net and non-secondary pollution, the effective means of water pollution control has been increasingly becoming it.2010, Ye seminars found phosphoric acid
Silver nano material have photochemical catalyst effect, energy gap is about 2.3eV, can absorbing wavelength be less than about 530nm too
Positive energy.At identical conditions, silver orthophosphate catalytic activity is be currently known catalyst several times.At present, multiple rule pattern
Ag3PO4Nano material there has been preliminary research, but the octahedra silver orthophosphate of polyhedral silver phosphate such as ten or dodecahedron phosphoric acid
Silver is also rarely found to be had been reported that.
The content of the invention
The present invention primary and foremost purpose be to overcome shortcoming and deficiency in the prior art, a kind of polyhedron phosphoric acid is provided
The preparation method of silver nano material.
Another object of the present invention is to provide the polyhedral silver phosphate nano material obtained with above-mentioned preparation method.
It is still another object of the present invention to provide the polyhedral silver phosphate applications to nanostructures.
The purpose of the present invention is achieved through the following technical solutions：A kind of method for preparing polyhedral silver phosphate nano material,
Include the following steps：Triethanolamine is added in silver nitrate solution, stirs evenly, obtains mixed solution；While stirring by phosphoric acid
Salting liquid is added in the mixed solution, and after completion of dropwise addition, after 5~30min of normal-temperature reaction, centrifugation takes precipitation, dries, obtains
To polyhedral silver phosphate nano material；Silver nitrate is 3 with phosphatic molar ratio:1, the molar ratio of triethanolamine and silver nitrate is
1:12~1:14.
The polyhedral silver phosphate nano material is received for ten octahedra phosphoric acid silver nano materials or dodecahedron silver orthophosphate
Rice material.
The silver nitrate solution is silver nitrate aqueous solution；
The phosphate solution is phosphate aqueous solution；
The phosphate is preferably sodium phosphate, disodium hydrogen phosphate or sodium dihydrogen phosphate；
The stirring is preferably magnetic agitation or electric stirring；
The mixing speed is preferably 1300r/min；
The drying temperature is preferably 30~90 DEG C.
The energy gap of the polyhedral silver phosphate nano material is~2.3eV.
A kind of polyhedral silver phosphate nano material, is obtained by above-mentioned preparation method.
The polyhedral silver phosphate nano material can be applied to photocatalysis technology field.
The present invention is had the following advantages compared with the prior art and effect：The present invention using conventional reagent triethanolamine,
By controlling silver nitrate and phosphatic concentration, so as to fulfill the regulation and control of silver orthophosphate pattern.Obtained polyhedral silver phosphate nanometer
The energy gap of material is~2.3eV, can absorbing wavelength be less than the~solar energy of 530nm.Under the same conditions, polyhedron phosphorus
The catalytic activity of sour silver nano material is be currently known catalyst several times.The preparation method of the present invention is simply easily achieved, no
It needs traditional two-step method, a step that can synthesize polyhedral silver phosphate nano material, can be applied to industrialized production.
Description of the drawings
Fig. 1 is the micro- electron-microscope scanning figure of ten octahedra phosphoric acid silver nano materials of embodiment 1；
Fig. 2 is the micro- electron-microscope scanning figure of the dodecahedron phosphoric acid silver nano material of embodiment 4.
Specific embodiment
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) 0.003mol silver nitrates are dissolved in 30mL distilled water, are configured to silver nitrate solution；
(2) molar ratio of triethanolamine (TEA), triethanolamine and silver nitrate is added in into the silver nitrate solution of step (1)
For 1:12；
(3) sodium phosphate of 0.001mol is dissolved in 30mL distilled water, is configured to sodium radio-phosphate,P-32 solution；
(4) under conditions of magnetic agitation (mixing speed 1300r/min), by the phosphate solution of step (3) dropwise
It is added in the mixed solution of step (2), after completion of dropwise addition, (25 DEG C) reaction 30min, obtain yellow mercury oxide under room temperature；
(5) yellow mercury oxide obtained by step (4) is centrifuged, collects precipitation, washed respectively with distilled water and absolute ethyl alcohol successively
It washs 3 times, is dried in 60 DEG C of air, obtain ten octahedra phosphoric acid silver nano materials；The taboo of ten octahedra phosphoric acid silver nano materials
Bandwidth is~2.3eV.
The micro- electron-microscope scanning figure of the octahedra phosphoric acid silver nano material of described ten is shown in Fig. 1；It will be seen from figure 1 that it obtains
Ten octahedra phosphoric acid silver nano material uniform particle sizes.
Embodiment 2
(1) 0.003mol silver nitrates are dissolved in 30mL distilled water, are configured to silver nitrate solution；
(2) molar ratio of triethanolamine (TEA), triethanolamine and silver nitrate is added in into the silver nitrate solution of step (1)
For 1:12；
(3) disodium hydrogen phosphate of 0.001mol is dissolved in 30mL distilled water, is configured to disodium phosphate soln；
(4) under conditions of magnetic agitation (mixing speed 1300r/min), by the phosphate solution of step (3) dropwise
It is added in the mixed solution of step (2), after completion of dropwise addition, (25 DEG C) reaction 20min, obtain yellow mercury oxide under room temperature；
(5) yellow mercury oxide obtained by step (4) is centrifuged, collects precipitation, washed respectively with distilled water and absolute ethyl alcohol successively
It washs 3 times, is dried in 60 DEG C of air, obtain ten octahedra phosphoric acid silver nano materials；The taboo of ten octahedra phosphoric acid silver nano materials
Bandwidth is~2.3eV.
Embodiment 3
(1) 0.003mol silver nitrates are dissolved in 30mL distilled water, are configured to silver nitrate solution；
(2) molar ratio of triethanolamine (TEA), triethanolamine and silver nitrate is added in into the silver nitrate solution of step (1)
For 1:13；
(3) sodium dihydrogen phosphate of 0.001mol is dissolved in 30mL distilled water, is configured to sodium dihydrogen phosphate；
(4) under conditions of magnetic agitation (mixing speed 1300r/min), by the phosphate solution of step (3) dropwise
It is added in the mixed solution of step (2), after completion of dropwise addition, (25 DEG C) reaction 5min, obtain yellow mercury oxide under room temperature；
(5) yellow mercury oxide obtained by step (4) is centrifuged, collects precipitation, washed respectively with distilled water and absolute ethyl alcohol successively
It washs 3 times, is dried in 30 DEG C of air, obtain ten octahedra phosphoric acid silver nano materials；The taboo of ten octahedra phosphoric acid silver nano materials
Bandwidth is~2.3eV.
Embodiment 4
(1) 0.003mol silver nitrates are dissolved in 30mL distilled water, are configured to silver nitrate solution；
(2) molar ratio of triethanolamine (TEA), triethanolamine and silver nitrate is added in into the silver nitrate solution of step (1)
For 1:14；
(3) sodium phosphate of 0.001mol is dissolved in 30mL distilled water, is configured to sodium radio-phosphate,P-32 solution；
(4) under conditions of magnetic agitation (mixing speed 1300r/min), by the phosphate solution of step (3) dropwise
It is added in the mixed solution of step (2), after completion of dropwise addition, (25 DEG C) reaction 30min, obtain yellow mercury oxide under room temperature；
(5) yellow mercury oxide obtained by step (4) is centrifuged, collects precipitation, washed respectively with distilled water and absolute ethyl alcohol successively
It washs 3 times, is dried in 90 DEG C of air, obtain dodecahedron phosphoric acid silver nano material；The taboo of dodecahedron phosphoric acid silver nano material
Bandwidth is~2.3eV.
The micro- electron-microscope scanning figure of the dodecahedron phosphoric acid silver nano material is shown in Fig. 2；Figure it is seen that it obtains
Dodecahedron phosphoric acid silver nano material uniform particle sizes.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (5)
- A kind of 1. method for preparing polyhedral silver phosphate nano material, which is characterized in that include the following steps：By triethanolamine plus Enter in silver nitrate solution, stir evenly, obtain mixed solution；Phosphate solution is added in the mixed solution while stirring In, after completion of dropwise addition, after 5~30min of normal-temperature reaction, centrifugation takes precipitation, dries, obtains polyhedral silver phosphate nano material；Nitre Acid is silver-colored and phosphatic molar ratio is 3:1, the molar ratio of triethanolamine and silver nitrate is 1:14；The polyhedral silver phosphate is received The energy gap of rice material is 2.3eV；The polyhedral silver phosphate nano material is ten octahedra phosphoric acid silver nano materials.
- 2. the method according to claim 1 for preparing polyhedral silver phosphate nano material, which is characterized in that the nitric acid Silver-colored solution is silver nitrate aqueous solution.
- 3. the method according to claim 1 for preparing polyhedral silver phosphate nano material, which is characterized in that the phosphoric acid Salting liquid is phosphate aqueous solution.
- 4. the method according to claim 1 for preparing polyhedral silver phosphate nano material, which is characterized in that the stirring For magnetic agitation or electric stirring.
- 5. the method according to claim 1 for preparing polyhedral silver phosphate nano material, which is characterized in that the drying Temperature is 30~90 DEG C.
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| CN105435823B (en) * | 2015-12-11 | 2017-08-25 | 华南理工大学 | A kind of granatohedron silver phosphate photocatalyst and preparation and application |
| CN107442145A (en) * | 2017-07-14 | 2017-12-08 | 华南师范大学 | A kind of preparation method of polyhedral silver phosphate visible light catalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103263937A (en) * | 2013-06-17 | 2013-08-28 | 南京信息工程大学 | Method for preparing tetrahedral silver phosphate photocatalyst |
| CN104014354A (en) * | 2014-06-16 | 2014-09-03 | 中国矿业大学 | Method for improving visible light catalytic performance of Ag3PO4 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103263937A (en) * | 2013-06-17 | 2013-08-28 | 南京信息工程大学 | Method for preparing tetrahedral silver phosphate photocatalyst |
| CN104014354A (en) * | 2014-06-16 | 2014-09-03 | 中国矿业大学 | Method for improving visible light catalytic performance of Ag3PO4 |
Non-Patent Citations (1)
| Title |
|---|
| Morphology-controlled synthesis of Ag3PO4 microcrystals for high performance photocatalysis;Yang-Sen Xu et al;《CrystEngComm》;20130425;第15卷;5407-5411 * |
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