CN102690527B - Preparation method of Ag3PO4/ion exchange resin compound - Google Patents
Preparation method of Ag3PO4/ion exchange resin compound Download PDFInfo
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- CN102690527B CN102690527B CN201210188768.7A CN201210188768A CN102690527B CN 102690527 B CN102690527 B CN 102690527B CN 201210188768 A CN201210188768 A CN 201210188768A CN 102690527 B CN102690527 B CN 102690527B
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- exchange resin
- ion exchange
- preparation
- ag3po4
- anionite
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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
4mixture preparation method, mainly relates to a kind of Ag
3pO
4/ ion exchange resin complexes preparation method.
(2) background technology:
Ag
3pO
4owing to thering is catalysis, the performance such as antibacterial, therefore, industrial, be usually used in antiseptic-germicide and photocatalyst.In recent years, for improving Ag
3pO
4range of application, Ag
3pO
4mixture technology of preparing is one of focus of the subject researchs such as materialogy, chemistry.Chinese patent (CN102151577A) discloses a kind of Ag
3pO
4/ Mg-Al LDO visible ray composite photo-catalyst and preparation and application thereof, obtain Ag
3pO
4particle diameter is 15-250 nanometer, Ag
3pO
4with magnalium bimetallic oxide Mg-Al LDO mass ratio be 1: 10-5: 1.But this kind of Ag
3pO
4composite materials need to first be prepared Mg-Al-CO
3lDO, then by Mg-Al-CO
3lDO joins in Leaching Properties of Soluble Phosphorus acid salt solution and reacts, and after washing, being dried, also need to calcine 2-4h at 400-600, and preparation process is comparatively loaded down with trivial details, has affected 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 applicable 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 Leaching Properties of Soluble Phosphorus acid salt solution, and absorption exchange 2-8 hour, after filtering, being dried, joins AgNO by above-mentioned anionite-exchange resin
3in solution, react 10-60 minute, after filtration, at 60 ℃-100 ℃, dry 2-10 hour, can make Ag
3pO
4/ ion exchange resin complexes.
Wherein Leaching Properties of Soluble Phosphorus hydrochlorate is sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, potassiumphosphate, potassium primary phosphate and dipotassium hydrogen phosphate.
Wherein the concentration of Leaching Properties of Soluble Phosphorus acid salt aqueous solution is 0.1-1M.
AgNO wherein
3the concentration of the aqueous solution is 0.05-0.5M.
Owing to having taked technique scheme, anionite-exchange resin is first joined to absorption exchange in Leaching Properties of Soluble Phosphorus acid salt solution, then join AgNO
3in solution, react, after filtration, dry after, can make Ag
3pO
4/ ion exchange resin complexes.With existing Ag
3pO
4mixture is preparation method compare, this kind of Ag
3pO
4the preparation method of/ion exchange resin complexes has the advantages such as low, simple to operate, the applicable suitability for industrialized production of cost.Ag prepared by the present invention
3pO
4/ ion exchange resin complexes is by Ag
3pO
4nano particle and anionite-exchange resin form, and therefore have Ag
3pO
4the catalysis of nano particle, anti-microbial effect and ion-exchange resin absorption, therefore can be used for the numerous areas such as photochemical catalysis, anti-biotic material.
(4) accompanying drawing explanation: Fig. 1 is Ag of the present invention
3pO
4ag prepared by/ion exchange resin complexes preparation method
3pO
4/ ion exchange resin complexes stereoscan photograph.
(5) embodiment:
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment mono-
In beaker, 0.5 gram of Cl type anionite-exchange resin is joined in 100 milliliters, 0.1M disodium phosphate soln, and on vibrator, vibrates 8 hours, then filter, dry after, above-mentioned anionite-exchange resin is joined to 90 milliliters, 0.1M AgNO
3in solution, react 40 minutes, after filtration, at 60 ℃, dry 10 hours, can make 1.0 grams of Ag
3pO
4/ ion exchange resin complexes.Measurement result: the Ag of preparation
3pO
4/ ion exchange resin complexes has been analyzed Ag by Japanese Shimadzu-6000X x ray diffractometer x
3pO
4crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations microsphere surface pattern, result shows: as seen from Figure 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 between 5-25 μ m, anionite-exchange resin is at internal layer.
Embodiment bis-
In beaker, 1 gram of Cl type anionite-exchange resin is joined in 40 milliliters, 1M sodium radio-phosphate,P-32 solution, and on vibrator, vibrates 2 hours, then filter, dry after, above-mentioned anionite-exchange resin is joined to 50 milliliters, 0.5M AgNO
3in solution, react 10 minutes, after filtration, at 100 ℃, dry 2 hours, can make 2.6 grams of Ag
3pO
4/ ion exchange resin complexes.Measurement result: the Ag of preparation
3pO
4/ ion exchange resin complexes has been analyzed Ag by Japanese Shimadzu-6000X x ray diffractometer x
3pO
4crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations microsphere surface pattern, 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 between 20-40 μ m, anionite-exchange resin is at internal layer.
Embodiment tri-
In beaker, 1 gram of Cl type anionite-exchange resin is joined in 50 milliliters, 0.8M disodium phosphate soln, and on vibrator, vibrates 4 hours, then filter, dry after, above-mentioned anionite-exchange resin is joined to 70 milliliters, 0.3MAgNO
3in solution, react 30 minutes, after filtration, at 70 ℃, dry 9 hours, can make 2.5 grams of Ag
3pO
4/ ion exchange resin complexes.Measurement result: the Ag of preparation
3pO
4/ ion exchange resin complexes has been analyzed Ag by Japanese Shimadzu-6000X x ray diffractometer x
3pO
4crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations microsphere surface pattern, 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 between 15-35 μ m, anionite-exchange resin is at internal layer.
Embodiment tetra-
In beaker, 0.4 gram of OH type anionite-exchange resin is joined in 70 milliliters, 0.3M potassium dihydrogen phosphate, and on vibrator, vibrates 6 hours, then filter, dry after, above-mentioned anionite-exchange resin is joined to 100 milliliters, 0.05MAgNO
3in solution, react 60 minutes, after filtration, at 80 ℃, dry 6 hours, can make 0.9 gram of Ag
3pO
4/ ion exchange resin complexes.Measurement result: the Ag of preparation
3pO
4/ ion exchange resin complexes has been analyzed Ag by Japanese Shimadzu-6000X x ray diffractometer x
3pO
4crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations microsphere surface pattern, 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 between 10-30 μ m, anionite-exchange resin is at internal layer.
Embodiment five
In beaker, 1 gram of OH type anionite-exchange resin is joined in 60 milliliters, 0.4M dipotassium hydrogen phosphate solution, and on vibrator, vibrates 5 hours, then filter, dry after, above-mentioned anionite-exchange resin is joined to 70 milliliters, 0.3MAgNO
3in solution, react 30 minutes, after filtration, at 70 ℃, dry 9 hours, can make 2.2 grams of Ag
3pO
4/ ion exchange resin complexes.Measurement result: the Ag of preparation
3pO
4/ ion exchange resin complexes has been analyzed Ag by Japanese Shimadzu-6000X x ray diffractometer x
3pO
4crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations microsphere surface pattern, 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 between 12-32 μ m, anionite-exchange resin is at internal layer.
Embodiment six
In beaker, 0.5 gram of OH type anionite-exchange resin is joined in 90 milliliters, 0.2M potassium phosphate solution, and on vibrator, vibrates 7 hours, then filter, dry after, above-mentioned anionite-exchange resin is joined to 60 milliliters, 0.2M AgNO
3in solution, react 35 minutes, after filtration, at 90 ℃, dry 4 hours, can make 1.1 grams of Ag
3pO
4/ ion exchange resin complexes.Measurement result: the Ag of preparation
3pO
4/ ion exchange resin complexes has been analyzed Ag by Japanese Shimadzu-6000X x ray diffractometer x
3pO
4crystal formation, the Japanese Hitachi X of company 650 scanning electron microscopic observations microsphere surface pattern, 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 between 8-28 μ m, anionite-exchange resin is at internal layer.
Claims (4)
1.Ag
3pO
4/ ion exchange resin complexes preparation method:
Anionite-exchange resin is joined in Leaching Properties of Soluble Phosphorus acid salt solution, and absorption exchange 2-8 hour, after filtering, being dried, joins AgNO by above-mentioned anionite-exchange resin
3in solution, react 10-60 minute, after filtration, at 60 ℃-100 ℃, dry 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, Leaching Properties of Soluble Phosphorus hydrochlorate is sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, potassiumphosphate, potassium primary phosphate and dipotassium hydrogen phosphate.
3. Ag according to claim 1
3pO
4/ ion exchange resin complexes preparation method, wherein the concentration of Leaching Properties of Soluble Phosphorus acid salt aqueous solution 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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| CN102690527B true CN102690527B (en) | 2014-04-09 |
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| 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 |
| 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 |
| 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 |
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 |
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2012
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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 |
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