CN102690527A - Preparation method of Ag3PO4/ion exchange resin compound - Google Patents
Preparation method of Ag3PO4/ion exchange resin compound Download PDFInfo
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- CN102690527A CN102690527A CN2012101887687A CN201210188768A CN102690527A CN 102690527 A CN102690527 A CN 102690527A CN 2012101887687 A CN2012101887687 A CN 2012101887687A CN 201210188768 A CN201210188768 A CN 201210188768A CN 102690527 A CN102690527 A CN 102690527A
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- CN
- China
- Prior art keywords
- exchange resin
- ion exchange
- preparation
- ag3po4
- anionite
- 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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Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000003456 ion exchange resin Substances 0.000 title abstract description 8
- 229920003303 ion-exchange polymer Polymers 0.000 title abstract description 8
- 229910000161 silver phosphate Inorganic materials 0.000 title abstract 7
- -1 ion exchange resin compound Chemical class 0.000 title abstract 5
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 8
- 239000010452 phosphate Substances 0.000 claims abstract description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 7
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical class C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 34
- 239000011347 resin Substances 0.000 claims description 30
- 229920005989 resin Polymers 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 16
- 101710134784 Agnoprotein Proteins 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 3
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 3
- 229940093916 potassium phosphate Drugs 0.000 claims description 3
- 235000011009 potassium phosphates Nutrition 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229940061607 dibasic sodium phosphate Drugs 0.000 claims description 2
- 235000019797 dipotassium phosphate Nutrition 0.000 claims description 2
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 229940045641 monobasic sodium phosphate Drugs 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 229960003975 potassium Drugs 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 229960003339 sodium phosphate Drugs 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical group [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 239000003957 anion exchange resin Substances 0.000 abstract 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract 3
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910003023 Mg-Al Inorganic materials 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 description 2
- 235000019800 disodium phosphate Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 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 1
- 229910001051 Magnalium Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Catalysts (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of a Ag3PO4/ion exchange resin compound. The preparation method comprises the steps of: adding anion exchange resin into a soluble phosphate solution, carrying out adsorption exchange for 2-8h, filtering, drying, adding the anion exchange resin into AgNO3 solution for reacting for 10-60min, filtering, and then drying at a temperature of 60-100 DEG C for 2-10h to obtain the Ag3PO4/ion exchange resin compound. In the Ag3PO4/ion exchange resin compound, Ag3PO4 is arranged on the outer layer, and the anion exchange resin is arranged in the inner layer. Compared with the existing preparation method of the Ag3PO4 compound, the preparation method of the Ag3PO4/ion exchange resin compound has the advantages of low cost, simpleness in operation, suitability for industrial production, and the like.
Description
(1) technical field:
The present invention relates to a kind of Ag
3PO
4The mixture preparation method mainly relates to a kind of Ag
3PO
4/ ion exchange resin complexes preparation method.
(2) background technology:
Ag
3PO
4Owing to have catalysis, performance such as antibiotic, therefore, in industry, be usually used in antiseptic-germicide and photocatalyst.In recent years, for improving Ag
3PO
4Range of application, Ag
3PO
4The mixture technology of preparing is one of focus of subject researchs such as materialogy, chemistry.Chinese patent (CN102151577A) discloses a kind of Ag
3PO
4/ Mg-Al LDO visible light composite photo-catalyst and preparation thereof and application obtain Ag
3PO
4Particle diameter is the 15-250 nanometer, Ag
3PO
4With magnalium bimetallic oxide Mg-Al LDO mass ratio be 1: 10-5: 1.But this kind Ag
3PO
4Composite materials needs preparation Mg-Al-CO earlier
3LDO is then with Mg-Al-CO
3LDO joins in the solvable aqueous phosphate solution and reacts, and after washing, the drying, also need calcine 2-4h at 400-600, and the preparation process is comparatively loaded down with trivial details, has influenced Ag
3PO
4Composite materials is in the application in a lot of fields.
(3) summary of the invention:
The object of the present invention is to provide the Ag that a kind of cost is low, simple to operate, be fit to suitability for industrialized production
3PO
4/ ion exchange resin preparation method.
For achieving the above object Ag of the present invention
3PO
4/ ion exchange resin preparation method is: anionite-exchange resin is joined in the solvable aqueous phosphate solution, and absorption exchange 2-8 hour after filtration, the drying, joins AgNO with above-mentioned anionite-exchange resin
3Reaction is 10-60 minute in the solution, after the filtration, 60 ℃-100 ℃ bakings 2-10 hour, can make Ag
3PO
4/ ion exchange resin complexes.
Wherein solvable phosphoric acid salt is sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate, dibasic, potassiumphosphate, potassium primary phosphate and potassium hydrogenphosphate.
Wherein the concentration of solvable aqueous phosphatic is 0.1-1M.
AgNO wherein
3The concentration of the aqueous solution is 0.05-0.5M.
Owing to taked technique scheme, anionite-exchange resin is joined absorption exchange in the solvable aqueous phosphate solution earlier, join AgNO again
3React in the solution, after filtration, drying, can make Ag
3PO
4/ ion exchange resin complexes.With existing Ag
3PO
4Mixture is the preparation method compare, this kind Ag
3PO
4The preparation method of/ion exchange resin complexes has advantages such as low, simple to operate, the suitable suitability for industrialized production of cost.The Ag of the present invention's preparation
3PO
4/ ion exchange resin complexes is by Ag
3PO
4Nano particle and anionite-exchange resin are formed, and therefore have Ag
3PO
4Therefore the catalysis of nano particle, anti-microbial effect and ion-exchange resin absorption can be used for numerous areas such as photochemical catalysis, anti-biotic material.
(4) description of drawings: Fig. 1 is Ag according to the invention
3PO
4The Ag of/ion exchange resin complexes preparation method preparation
3PO
4/ ion exchange resin complexes stereoscan photograph.
(5) embodiment:
Below in conjunction with embodiment the present invention is done further explain.
Embodiment one
In beaker, 0.5 gram Cl type anionite-exchange resin is joined in 100 milliliters, 0.1M disodium phosphate soln, and vibration 8 hours on vibrator, filter then, after the drying, above-mentioned anionite-exchange resin joined 90 milliliters, 0.1M AgNO
3Reaction is 40 minutes in the solution, after the filtration, 60 ℃ of oven dry 10 hours, can make 1.0 gram Ag
3PO
4/ ion exchange resin complexes.Measure the result: the Ag of preparation
3PO
4/ ion exchange resin complexes through day island proper Tianjin-6000X x ray diffractometer x analyzed Ag
3PO
4Crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations the microsphere surface pattern, the result shows: visible by Fig. 1, prepared Ag
3PO
4/ ion exchange resin complexes is by anionite-exchange resin and Ag
3PO
4Granulometric composition is bilayer structure, diameter between 500-1000 μ m, Ag
3PO
4Particle is at skin, and thickness is that anionite-exchange resin is at internal layer between the 5-25 μ m.
Embodiment two
In beaker, 1 gram Cl type anionite-exchange resin is joined in 40 milliliters, 1M sodium radio-phosphate,P-32 solution, and vibration 2 hours on vibrator, filter then, after the drying, above-mentioned anionite-exchange resin joined 50 milliliters, 0.5M AgNO
3Reaction is 10 minutes in the solution, after the filtration, 100 ℃ of oven dry 2 hours, can make 2.6 gram Ag
3PO
4/ ion exchange resin complexes.Measure the result: the Ag of preparation
3PO
4/ ion exchange resin complexes through day island proper Tianjin-6000X x ray diffractometer x analyzed Ag
3PO
4Crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations the microsphere surface pattern, the result shows: prepared Ag
3PO
4/ ion exchange resin complexes is by anionite-exchange resin and Ag
3PO
4Granulometric composition is bilayer structure, diameter between 600-1200 μ m, Ag
3PO
4Particle is at skin, and thickness is that anionite-exchange resin is at internal layer between the 20-40 μ m.
Embodiment three
In beaker, 1 gram Cl type anionite-exchange resin is joined in 50 milliliters, 0.8M disodium phosphate soln, and vibration 4 hours on vibrator, filter then, after the drying, above-mentioned anionite-exchange resin joined 70 milliliters, 0.3MAgNO
3Reaction is 30 minutes in the solution, after the filtration, 70 ℃ of oven dry 9 hours, can make 2.5 gram Ag
3PO
4/ ion exchange resin complexes.Measure the result: the Ag of preparation
3PO
4/ ion exchange resin complexes through day island proper Tianjin-6000X x ray diffractometer x analyzed Ag
3PO
4Crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations the microsphere surface pattern, the result shows: prepared Ag
3PO
4/ ion exchange resin complexes is by anionite-exchange resin and Ag
3PO
4Granulometric composition is bilayer structure, diameter between 500-1100 μ m, Ag
3PO
4Particle is at skin, and thickness is that anionite-exchange resin is at internal layer between the 15-35 μ m.
Embodiment four
In beaker, 0.4 gram OH type anionite-exchange resin is joined in 70 milliliters, 0.3M potassium dihydrogen phosphate, and vibration 6 hours on vibrator, filter then, after the drying, above-mentioned anionite-exchange resin joined 100 milliliters, 0.05MAgNO
3Reaction is 60 minutes in the solution, after the filtration, 80 ℃ of oven dry 6 hours, can make 0.9 gram Ag
3PO
4/ ion exchange resin complexes.Measure the result: the Ag of preparation
3PO
4/ ion exchange resin complexes through day island proper Tianjin-6000X x ray diffractometer x analyzed Ag
3PO
4Crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations the microsphere surface pattern, the result shows: prepared Ag
3PO
4/ ion exchange resin complexes is by anionite-exchange resin and Ag
3PO
4Granulometric composition is bilayer structure, diameter between 500-1000 μ m, Ag
3PO
4Particle is at skin, and thickness is that anionite-exchange resin is at internal layer between the 10-30 μ m.
Embodiment five
In beaker, 1 gram OH type anionite-exchange resin is joined in 60 milliliters, 0.4M dipotassium hydrogen phosphate solution, and vibration 5 hours on vibrator, filter then, after the drying, above-mentioned anionite-exchange resin joined 70 milliliters, 0.3MAgNO
3Reaction is 30 minutes in the solution, after the filtration, 70 ℃ of oven dry 9 hours, can make 2.2 gram Ag
3PO
4/ ion exchange resin complexes.Measure the result: the Ag of preparation
3PO
4/ ion exchange resin complexes through day island proper Tianjin-6000X x ray diffractometer x analyzed Ag
3PO
4Crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations the microsphere surface pattern, the result shows: prepared Ag
3PO
4/ ion exchange resin complexes is by anionite-exchange resin and Ag
3PO
4Granulometric composition is bilayer structure, diameter between 500-1000 μ m, Ag
3PO
4Particle is at skin, and thickness is that anionite-exchange resin is at internal layer between the 12-32 μ m.
Embodiment six
In beaker, 0.5 gram OH type anionite-exchange resin is joined in 90 milliliters, 0.2M potassium phosphate solution, and vibration 7 hours on vibrator, filter then, after the drying, above-mentioned anionite-exchange resin joined 60 milliliters, 0.2M AgNO
3Reaction is 35 minutes in the solution, after the filtration, 90 ℃ of oven dry 4 hours, can make 1.1 gram Ag
3PO
4/ ion exchange resin complexes.Measure the result: the Ag of preparation
3PO
4/ ion exchange resin complexes through day island proper Tianjin-6000X x ray diffractometer x analyzed Ag
3PO
4Crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations the microsphere surface pattern, the result shows: prepared Ag
3PO
4/ ion exchange resin complexes is by anionite-exchange resin and Ag
3PO
4Granulometric composition is bilayer structure, diameter between 500-1000 μ m, Ag
3PO
4Particle is at skin, and thickness is that anionite-exchange resin is at internal layer between the 8-28 μ m.
Claims (4)
1.Ag
3PO
4/ ion exchange resin complexes preparation method:
Anionite-exchange resin is joined in the solvable aqueous phosphate solution, and absorption exchange 2-8 hour after filtration, the drying, joins AgNO with above-mentioned anionite-exchange resin
3Reaction is 10-60 minute in the solution, after the filtration, 60 ℃-100 ℃ bakings 2-10 hour, can make Ag
3PO
4/ ion exchange resin complexes.
2. Ag according to claim 1
3PO
4/ ion exchange resin complexes preparation method, solvable phosphoric acid salt is sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate, dibasic, potassiumphosphate, potassium primary phosphate and potassium hydrogenphosphate.
3. Ag according to claim 1
3PO
4/ ion exchange resin complexes preparation method, wherein the concentration of solvable aqueous phosphatic is 0.1-1M.
4. Ag according to claim 1
3PO
4/ ion exchange resin complexes material, wherein AgNO
3The concentration of the aqueous solution is 0.05-0.5M.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210188768.7A CN102690527B (en) | 2012-06-04 | 2012-06-04 | Preparation method of Ag3PO4/ion exchange resin compound |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210188768.7A CN102690527B (en) | 2012-06-04 | 2012-06-04 | Preparation method of Ag3PO4/ion exchange resin compound |
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| Publication Number | Publication Date |
|---|---|
| CN102690527A true CN102690527A (en) | 2012-09-26 |
| CN102690527B CN102690527B (en) | 2014-04-09 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104128203A (en) * | 2014-07-17 | 2014-11-05 | 合肥工业大学 | Silver phosphate/resin compound and use thereof |
| CN104128204A (en) * | 2014-07-17 | 2014-11-05 | 合肥工业大学 | Preparation method of silver phosphate/resin compound |
| CN107803221A (en) * | 2017-11-23 | 2018-03-16 | 郑州圣莱特空心微珠新材料有限公司 | Float type phosphoric acid silver-based visible light catalyst and its preparation method and application |
| CN112058285A (en) * | 2020-09-17 | 2020-12-11 | 安庆师范大学 | Ag/Ag3PO4Preparation method and application of carbonized resin compound |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080306181A1 (en) * | 2007-06-08 | 2008-12-11 | Garey Jr Harold Elbridge | Antimicrobial polyurethane resins and products made therefrom |
| CN102151577A (en) * | 2011-01-28 | 2011-08-17 | 东华大学 | Ag3PO4/Mg-Al LDO (Layered Double Oxide) visible light composite photo catalyst, preparation and application thereof |
-
2012
- 2012-06-04 CN CN201210188768.7A patent/CN102690527B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080306181A1 (en) * | 2007-06-08 | 2008-12-11 | Garey Jr Harold Elbridge | Antimicrobial polyurethane resins and products made therefrom |
| CN102151577A (en) * | 2011-01-28 | 2011-08-17 | 东华大学 | Ag3PO4/Mg-Al LDO (Layered Double Oxide) visible light composite photo catalyst, preparation and application thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104128203A (en) * | 2014-07-17 | 2014-11-05 | 合肥工业大学 | Silver phosphate/resin compound and use thereof |
| CN104128204A (en) * | 2014-07-17 | 2014-11-05 | 合肥工业大学 | Preparation method of silver phosphate/resin compound |
| CN107803221A (en) * | 2017-11-23 | 2018-03-16 | 郑州圣莱特空心微珠新材料有限公司 | Float type phosphoric acid silver-based visible light catalyst and its preparation method and application |
| CN107803221B (en) * | 2017-11-23 | 2020-07-03 | 郑州圣莱特空心微珠新材料有限公司 | Floating type silver phosphate-based visible-light-driven photocatalyst and preparation method and application thereof |
| CN112058285A (en) * | 2020-09-17 | 2020-12-11 | 安庆师范大学 | Ag/Ag3PO4Preparation method and application of carbonized resin compound |
| CN112058285B (en) * | 2020-09-17 | 2022-12-02 | 安庆师范大学 | Ag/Ag 3 PO 4 Preparation method and application of carbonized resin compound |
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| Publication number | Publication date |
|---|---|
| CN102690527B (en) | 2014-04-09 |
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