CN104128204A - Preparation method of silver phosphate/resin compound - Google Patents

Preparation method of silver phosphate/resin compound Download PDF

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Publication number
CN104128204A
CN104128204A CN201410342622.2A CN201410342622A CN104128204A CN 104128204 A CN104128204 A CN 104128204A CN 201410342622 A CN201410342622 A CN 201410342622A CN 104128204 A CN104128204 A CN 104128204A
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resin
preparation
silver orthophosphate
solution
distilled water
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崔康平
许为义
王郑
朱越
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Hefei University of Technology
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Hefei University of Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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Abstract

The invention discloses a preparation method of a silver phosphate/resin compound. The preparation method comprises the following steps of preparing phosphate ion resin (PO4<3-> resin), and preparing PVP-containing silver phosphate/resin compound. Through the preparation method, silver phosphate having good visible light catalytic oxidation performances is uniformly and stably compounded to the resin surface so that silver phosphate/resin photocatalyst particles having large particle sizes are obtained. The silver phosphate/resin compound can treat and purify waste water by natural light/sunshine catalytic oxidation, prevents secondary pollution may produced in waste water treatment and is convenient for photocatalyst recovery and reuse.

Description

A kind of preparation method of silver orthophosphate/resin complexes
Technical field
The invention belongs to technical field of sewage, be specifically related to a kind of preparation method of silver orthophosphate/resin complexes.
Background technology
The utilization of solar energy and the control of environmental pollution are facing mankind and key subjects urgently to be resolved hurrily.Own people's discovery TiO 2as light anode, carrying out UV-irradiation can decomposing H 2o is H 2and O 2since, nano-TiO 2photocatalytic Oxidation With Semiconductors technology has obtained in environmental pollution improvement field paying close attention to widely.Yet conventional broad-band gap catalysis material TiO 2, because quantization efficiency is low, be about 4%, and light-catalyzed reaction can only carry out under ultraviolet light, greatly limited its utilization to sunshine, also because need UV-irradiation, make this technical operation cost up, use occasion limited.Therefore explore and exploitation efficiently to utilize the novel semi-conductor photochemical catalyst of visible ray be the hot issue of current research.
At present, semiconductor Ag is found in research 3pO 4there is good visible light photocatalysis active, and to Ag 3pO 4in photocatalytic degradation water, organic matter has carried out correlative study.Yet, semiconductor Ag 3pO 4improper use, may cause than the even more serious heavy metal of organic pollution and phosphate and pollute, how can be efficiently, safe utilization visible ray-Ag 3pO 4come the organic pollution in catalytic degradation water to there is not yet report.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of silver orthophosphate/resin complexes, has solved the problem that the catalyst existing in prior art is difficult to recovery and recycling and secondary pollution.
The technical solution adopted in the present invention is, a kind of preparation method of silver orthophosphate/resin complexes specifically implements according to following steps:
The preparation of step 1, phosphate anion resin, prepares PO 4 3-resin;
Step 2, containing the preparation of the silver orthophosphate of PVP/resin complexes, prepare silver orthophosphate/resin complexes.
Feature of the present invention is also,
The preparation of phosphate anion resin is specifically implemented according to following steps:
Taking exchange capacity is the anion exchange resin of 3.2mmol/g and the Na of 0.1mol/L 3pO 4solution; Anion exchange resin is placed in to tool plug conical flask, with distilled water washing 3～5 times, drains the distilled water after washing, then add the Na of 0.1mol/L 3pO 4solution, vibration, standing, take the Na with above-mentioned 0.1mol/L 3pO 4the Na of the isopyknic 0.1mol/L of solution 3pO 4solution, the Na of replacing 0.1mol/L 3pO 4solution; Repeat aforesaid operations three times, by distilled water washing 3～5 times for the ion exchange resin after above-mentioned processing, filter, put into drying box and dry, make PO 4 3-resin.
Silver orthophosphate/resin complexes preparation containing PVP is specifically implemented according to following steps: the AgNO that takes 0.1mol/L 3solution and PVP, stir and dissolve, and obtains mixed liquor; Take the PO in step 1 4 3-resin is placed in beaker; Above-mentioned mixed liquor is poured in above-mentioned beaker and soaked PO 4 3-resin, the sample 3-5 time after processing with distilled water flushing, outwells remaining distilled water, dries and obtains silver orthophosphate/resin complexes.
Taking exchange capacity is the anion exchange resin of 3.2mmol/g and the Na of 0.1mol/L 3pO 4solution is 1 according to mass volume ratio (g/mL): 25-1: 30 carry out.
Duration of oscillation is: 5～10min, time of repose is 3～5h.
Take the AgNO of 0.1mol/L 3solution and PVP are 10000 according to volume mass than (mL/g): 1-100000: 1 carries out.
The PO taking 4 3-the AgNO of resin and 0.1mol/L 3the mass volume ratio of solution (g/mL) is 1: 25-1: 50.
Soak time is 45-60min.
The invention has the beneficial effects as follows:
(1) adopt silver orthophosphate visible light catalytic technology to substitute conventional titanium dioxide ultraviolet catalysis technique at present, be more applicable for wastewater treatment, and reduce cost for wastewater treatment and investment.
(2) by being easy to phosphate radical residual in the aqueous solution and silver ion, adopt resin adsorption and surface chemistry intermediate processing to make stable silver orthophosphate/resin particle thing, not only in wastewater treatment process, avoid secondary pollution, and be convenient to recovery and the recycling of photochemical catalyst after wastewater treatment.
The present invention by the silver orthophosphate with better visible light catalytic oxidation performance evenly, stably composite in resin surface, be made into silver orthophosphate/resin photocatalyst granular of greater particle size, can utilize natural daylight/sunlight catalytic oxidation processes and purifying liquid waste, and avoid the issuable secondary pollution of wastewater treatment process and facilitate recovery and the recycling of photochemical catalyst.
Accompanying drawing explanation
Fig. 1 be under Different Light silver orthophosphate resin complexes to methylene blue waste water decoloring design sketch;
Fig. 2 is silver orthophosphate/resin complexes photochemical catalytic oxidation sewage treatment technology process figure.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The invention provides a kind of preparation method of silver orthophosphate/resin complexes, specifically according to following steps, implement:
The preparation of step 1, phosphate anion resin: be 1 according to mass volume ratio (g/mL): 25-1: 30 to take exchange capacity be the anion exchange resin of 3.2mmol/g and the Na of 0.1mol/L 3pO 4solution; Anion exchange resin is placed in to tool plug conical flask, with distilled water washing 3～5 times, drains the distilled water after washing, then add the Na of 0.1mol/L 3pO 4solution, after vibration 5～10min, standing 3～5h, takes the Na with above-mentioned 0.1mol/L 3pO 4the Na of the isopyknic 0.1mol/L of solution 3pO 4solution, the Na of replacing 0.1mol/L 3pO 4solution; Repeat aforesaid operations three times, by distilled water washing 3～5 times for the ion exchange resin after above-mentioned processing, filter, put into drying box and dry, make PO 4 3-resin.
Step 2, containing the preparation of the silver orthophosphate of PVP/resin complexes: according to volume mass, than (g/mL), be 1000: 1-100000: 1 takes the AgNO of 0.1mol/L 3solution and PVP, stir and dissolve, and takes the PO in step 1 4 3-resin is placed in beaker, the PO taking 4 3-the AgNO of resin and 0.1mol/L 3solution is 1: 25-1: 50; Above-mentioned mixed liquor is poured in above-mentioned beaker and soaked PO 4 3-resin 45-60min, the sample 3-5 time after processing with distilled water flushing, outwells remaining distilled water, dries and obtains silver orthophosphate/resin complexes.
In this preparation method, at AgNO 3in solution, add PVP, after dissolving, then soak PO with it 4 3-resin anion (R.A.); Oxygen in PVP molecular structure has the not lone pair electrons of Cheng Jian, be easy to form coordinate bond with metal ion, the preferential adsorbing metal ions in these positions, and develop into thus the preferred growth adsorption site of product particle, be that first silver ion will be attracted to PVP above, PVP is as a kind of stabilizing agent, when with phosphate radical resin reaction, silver ion on PVP slowly discharges, and makes to form at resin surface that one deck is evenly distributed, constitutionally stable Ag 3pO 4particle.Therefore, above-mentioned committed step is to guarantee that silver orthophosphate is in all even stable distributions of resin surface, thereby obtains best catalytic oxidation effect, and prevents that silver orthophosphate dissolving from causing secondary pollution.
Crucial reagent in the present invention has Na 3pO 4, anion exchange resin, AgNO 3, polyvinylpyrrolidone (PVP); Utilize anion exchange resin exchange adsorption Na 3pO 4phosphate radical, obtain phosphate anion resin; Utilize PVP absorption AgNO 3silver ion, then with phosphate anion resin reaction, form silver orthophosphate resin complexes.
Phosphate anion resin for time, the mass ratio of sodium phosphate and anion exchange resin should be greater than 0.53, guarantees that exchange process sodium phosphate is excessive, makes anion exchange resin exchange completely.
The consumption of polyvinylpyrrolidone (PVP) by mass percentage should be between 0.1%-0.2%, and optimum value is 0.175%.PVP consumption is very few, effective stably dispersing silver orthophosphate particle, and PVP consumption is too much, and the complex compound that itself and silver ion form is more stable, is unfavorable for that silver orthophosphate forms, and hinders the photocatalysis of silver orthophosphate resin.
Embodiment 1
The preparation of step 1, phosphate anion resin: the anion exchange resin (exchange capacity is 3.2mmol/g) that takes 2.5g is placed in the tool plug conical flask of 250mL, with distilled water washing 3～5 times, drains the distilled water after washing, then adds the Na of 0.1mol/L 3pO 4solution 64mL, after vibration 5min, standing 3.5h, the Na of the 0.1mol/L more renewing 3pO 4solution 64mL, repeats aforesaid operations three times, by distilled water washing 3～5 times for the ion exchange resin after above-mentioned processing, filters, and puts into drying box and dries, and just makes PO 4 3-resin.
Step 2, containing the preparation of the silver orthophosphate of PVP/resin complexes: take above-mentioned PO 4 3-resin anion (R.A.) 2.5g is placed in beaker, measures the AgNO of 100mL0.1mol/L 3solution, and add 10mg PVP, after dissolving, pour in above-mentioned beaker and soak PO 4 3-resin anion (R.A.) 45min, the sample 3-5 time after processing with distilled water flushing, outwells remaining distilled water, dries and obtains silver orthophosphate/resin complexes.
Embodiment 2
The preparation of step 1, phosphate anion resin: the anion exchange resin (exchange capacity is 3.2mmol/g) that takes 2.5g is placed in the tool plug conical flask of 250mL, with distilled water washing 3～5 times, drains the distilled water after washing, then adds the Na of 0.1mol/L 3pO 4solution 62.5mL, after vibration 8min, standing 3h, takes the Na with above-mentioned 0.1mol/L 3pO 4the Na of the isopyknic 0.1mol/L of solution 3pO 4solution, the Na of replacing 0.1mol/L 3pO 4solution; Repeat aforesaid operations three times, by distilled water washing 3～5 times for the ion exchange resin after above-mentioned processing, filter, put into drying box and dry, make PO 4 3-resin.
Step 2, containing the preparation of the silver orthophosphate of PVP/resin complexes, take above-mentioned PO 4 3-resin anion (R.A.) 2.5g is placed in beaker, measures the AgNO of 62.5mL0.1mol/L 3solution, and add 62.5mg PVP, stir and dissolve; Above-mentioned mixed liquor is poured in above-mentioned beaker and soaked PO 4 3-resin 60min, the sample 3-5 time after processing with distilled water flushing, outwells remaining distilled water, dries and obtains silver orthophosphate/resin complexes.
Embodiment 3
The preparation of step 1, phosphate anion resin: the anion exchange resin (exchange capacity is 3.2mmol/g) that takes 2.5g is placed in the tool plug conical flask of 250mL, with distilled water washing 3～5 times, drains the distilled water after washing, then adds the Na of 0.1mol/L 3pO 4solution 75mL, after vibration 10min, standing 5h, takes the Na with above-mentioned 0.1mol/L 3pO 4the Na of the isopyknic 0.1mol/L of solution 3pO 4solution, the Na of replacing 0.1mol/L 3pO 4solution; Repeat aforesaid operations three times, by distilled water washing 3～5 times for the ion exchange resin after above-mentioned processing, filter, put into drying box and dry, make PO 4 3-resin.
Step 2, take above-mentioned PO 4 3-resin anion (R.A.) 2.5g is placed in beaker, measures the AgNO of 125mL0.1mol/L 3solution, and add 1.25mg PVP, stir and dissolve; Above-mentioned mixed liquor is poured in above-mentioned beaker and soaked PO 4 3-resin 50min, the sample 3-5 time after processing with distilled water flushing, outwells remaining distilled water, dries and obtains silver orthophosphate/resin complexes.
Silver orthophosphate/resin complexes that the present invention prepares can be used for the wastewater treatment of photochemical catalytic oxidation, specifically according to following steps, implements:
Step 1, press 1-2g/m 3in the shallow-layer reaction tank that to add silver orthophosphate/resin complexes be 0.3-0.5m in effective depth, reaction tank bottom arranges wears blank pipe aerating system, and aeration rate is pressed 0.1-0.2m 3air/m 2pool surface calculates;
Step 2, introducing waste water aeration, reaction 2-3h under sunshine (or fluorescent lamp) irradiates;
Step 3, reaction tank water outlet are through sedimentation basin sedimentation separation, and supernatant enters subsequent treatment unit or discharge, and sediment is back to recycling in reaction tank.
Embodiment 4
Press 1g/m 3in the shallow-layer reaction tank that to add silver orthophosphate/resin complexes be 0.3 in effective depth, reaction tank bottom arranges wears blank pipe aerating system, and aeration rate is pressed 0.15m 3air/m 2pool surface calculates; Introduce waste water aeration, reaction 2h under sunshine (or fluorescent lamp) irradiates; Reaction tank water outlet is through sedimentation basin sedimentation separation, and supernatant enters subsequent treatment unit or discharge, and sediment is back to recycling in reaction tank.
Embodiment 5
Press 2g/m 3in the shallow-layer reaction tank that to add silver orthophosphate/resin complexes be 0.4m in effective depth, reaction tank bottom arranges wears blank pipe aerating system, and aeration rate is pressed 0.2m 3air/m 2pool surface calculates; Introduce waste water aeration, reaction 3h under sunshine (or fluorescent lamp) irradiates; Reaction tank water outlet is through sedimentation basin sedimentation separation, and supernatant enters subsequent treatment unit or discharge, and sediment is back to recycling in reaction tank.
Embodiment 6
Press 1.5g/m 3in the shallow-layer reaction tank that to add silver orthophosphate/resin complexes be 0.5m in effective depth, reaction tank bottom arranges wears blank pipe aerating system, and aeration rate is pressed 0.1m 3air/m 2pool surface calculates; Introduce waste water aeration, reaction 2.5h under sunshine (or fluorescent lamp) irradiates; Reaction tank water outlet is through sedimentation basin sedimentation separation, and supernatant enters subsequent treatment unit or discharge, and sediment is back to recycling in reaction tank.
In the present invention, the effect of aeration is to make silver orthophosphate/resin compounded composition granule in aeration tank, be suspended state, fully mix with waste water, under radiation of visible light, by the photocatalytic oxidation of silver orthophosphate, by Pollutants in Wastewater degraded, realize useless water purification and decolouring.
Silver orthophosphate/resin complexes dosage, reaction tank effective depth, aeration rate, reaction time are most important to wastewater treatment.
(1) silver orthophosphate/resin complexes dosage is 1-2g/m 3, dosage is very few, reacts insufficient, and dosage is too much, easily in reaction tank, deposits, and reduces reaction efficiency;
(2) reaction tank effective depth is 0.3-0.5m, and the degree of depth is too little, and reaction tank floor space increases, and the degree of depth is excessive, and light is difficult for penetrating, and reaction efficiency declines;
(3) aeration rate is 0.1-0.2m 3air/m 2pool surface, aeration rate is too small, can not make silver orthophosphate/resin complexes fully suspend and mix with waste water, reacts insufficient, and aeration rate is excessive, waste energy consumption;
(4) reaction time is 2-3h, and the time is too short, reacts insufficient, overlong time, and the investment of increase and operation energy consumption are considerably less to the raising of waste water treatment efficiency, uneconomical.

Claims (8)

1. a preparation method for silver orthophosphate/resin complexes, is characterized in that, specifically according to following steps, implements:
The preparation of step 1, phosphate anion resin, prepares PO 4 3-resin;
Step 2, containing the preparation of the silver orthophosphate of PVP/resin complexes, prepare silver orthophosphate/resin complexes.
2. the preparation method of silver orthophosphate/resin complexes according to claim 1, is characterized in that, the preparation of described phosphate anion resin is specifically implemented according to following steps:
Taking exchange capacity is the anion exchange resin of 3.2mmol/g and the Na of 0.1mol/L 3pO 4solution; Anion exchange resin is placed in to tool plug conical flask, with distilled water washing 3～5 times, drains the distilled water after washing, then add the Na of 0.1mol/L 3pO 4solution, vibration, standing, take the Na with above-mentioned 0.1mol/L 3pO 4the Na of the isopyknic 0.1mol/L of solution 3pO 4solution, the Na of replacing 0.1mol/L 3pO 4solution; Repeat aforesaid operations three times, by distilled water washing 3～5 times for the ion exchange resin after above-mentioned processing, filter, put into drying box and dry, make PO 4 3-resin.
3. the preparation method of silver orthophosphate/resin complexes according to claim 1, is characterized in that, the preparation of the described silver orthophosphate containing PVP/resin complexes is specifically implemented according to following steps: the AgNO that takes 0.1mol/L 3solution and PVP, stir and dissolve, and obtains mixed liquor; Take the PO in step 1 4 3-resin is placed in beaker; Above-mentioned mixed liquor is poured in above-mentioned beaker and soaked PO 4 3-resin, the sample 3-5 time after processing with distilled water flushing, outwells remaining distilled water, dries and obtains silver orthophosphate/resin complexes.
4. the preparation method of silver orthophosphate/resin complexes according to claim 2, is characterized in that, described in to take exchange capacity be the anion exchange resin of 3.2mmol/g and the Na of 0.1mol/L 3pO 4solution is 1 according to mass volume ratio (g/mL): 25-1: 30 carry out.
5. the preparation method of silver orthophosphate/resin complexes according to claim 2, is characterized in that, described duration of oscillation is: 5～10min, described time of repose is 3～5h.
6. the preparation method of silver orthophosphate/resin complexes according to claim 3, is characterized in that, described in take the AgNO of 0.1mol/L 3solution and PVP are 10000 according to volume mass than (mL/g): 1-100000: 1 carries out.
7. the preparation method of silver orthophosphate/resin complexes according to claim 3, is characterized in that, described in the PO that takes 4 3-the AgNO of resin and 0.1mol/L 3the mass volume ratio of solution (g/mL) is 1: 25-1: 50.
8. the preparation method of silver orthophosphate/resin complexes according to claim 3, is characterized in that, described soak time is 45-60min.
CN201410342622.2A 2014-07-17 2014-07-17 Preparation method of silver phosphate/resin compound Pending CN104128204A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108043368A (en) * 2018-01-12 2018-05-18 西安鸿钧睿泽新材料科技有限公司 A kind of preparation method of resin group carbonic anhydride adsorption agent
CN111683905A (en) * 2018-02-09 2020-09-18 阿奎斯水空气系统有限公司林道雷布斯坦分公司 Water hardness stabilization using anion exchangers
CN112058285A (en) * 2020-09-17 2020-12-11 安庆师范大学 Ag/Ag3PO4Preparation method and application of carbonized resin compound

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CN102000594A (en) * 2010-11-26 2011-04-06 大连理工大学 Preparation method of visible light photo catalyst silver and silver phosphate and application thereof
CN102690527A (en) * 2012-06-04 2012-09-26 徐志兵 Preparation method of Ag3PO4/ion exchange resin compound

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108043368A (en) * 2018-01-12 2018-05-18 西安鸿钧睿泽新材料科技有限公司 A kind of preparation method of resin group carbonic anhydride adsorption agent
CN111683905A (en) * 2018-02-09 2020-09-18 阿奎斯水空气系统有限公司林道雷布斯坦分公司 Water hardness stabilization using anion exchangers
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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Application publication date: 20141105