CN106925308A - A kind of surface plasma nano catalysis material and its preparation method and application - Google Patents
A kind of surface plasma nano catalysis material and its preparation method and application Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 58
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 229910000161 silver phosphate Inorganic materials 0.000 claims abstract description 73
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 42
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 42
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000015556 catabolic process Effects 0.000 claims abstract description 24
- 238000006731 degradation reaction Methods 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 239000011780 sodium chloride Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 13
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 13
- 238000013019 agitation Methods 0.000 claims abstract description 11
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 8
- 230000002045 lasting effect Effects 0.000 claims abstract description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 26
- 229910019142 PO4 Inorganic materials 0.000 claims description 25
- 239000011941 photocatalyst Substances 0.000 claims description 18
- 239000006210 lotion Substances 0.000 claims description 16
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 8
- 229910052724 xenon Inorganic materials 0.000 claims description 8
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 8
- 235000010270 methyl p-hydroxybenzoate Nutrition 0.000 claims description 7
- 239000004292 methyl p-hydroxybenzoate Substances 0.000 claims description 7
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 24
- 238000005286 illumination Methods 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 4
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 19
- 238000002835 absorbance Methods 0.000 description 18
- 150000004702 methyl esters Chemical class 0.000 description 17
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 14
- 239000002131 composite material Substances 0.000 description 9
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 9
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 7
- 238000005342 ion exchange Methods 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 238000003795 desorption Methods 0.000 description 6
- 230000002708 enhancing effect Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000002421 anti-septic effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000000474 nursing effect Effects 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 238000006862 quantum yield reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229940011871 estrogen Drugs 0.000 description 1
- 239000000262 estrogen Substances 0.000 description 1
- GZQKNULLWNGMCW-PWQABINMSA-N lipid A (E. coli) Chemical compound O1[C@H](CO)[C@@H](OP(O)(O)=O)[C@H](OC(=O)C[C@@H](CCCCCCCCCCC)OC(=O)CCCCCCCCCCCCC)[C@@H](NC(=O)C[C@@H](CCCCCCCCCCC)OC(=O)CCCCCCCCCCC)[C@@H]1OC[C@@H]1[C@@H](O)[C@H](OC(=O)C[C@H](O)CCCCCCCCCCC)[C@@H](NC(=O)C[C@H](O)CCCCCCCCCCC)[C@@H](OP(O)(O)=O)O1 GZQKNULLWNGMCW-PWQABINMSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000011954 pollution control method Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
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- 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
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- 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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of surface plasma nano catalysis material and its preparation method and application.The surface plasma nano catalysis material includes the component of following parts by weight：Ag3PO4：62% ~ 94%, AgCl：6%~38%.The present invention is first by NaH2PO4It is substantially soluble in deionized water, AgNO is added dropwise under mechanical agitation state3Solution, by the way that photochemical catalyst Ag is obtained after lasting stirring3PO4, it is washed with deionized；Then it is added dropwise over NaCl solution to it；Resulting solution centrifugation, is washed with deionized, drying, and catalysis material Ag is obtained3PO4/AgCl.The present invention effectively inhibits Ag using the plasma resonance effect of AgCl3PO4Photoetch with decompose, improve its stability and photocatalytic activity under light illumination.The preparation method is simple, and cost is relatively low, can be in Photocatalytic Activity for Degradation organic pollution.
Description
Technical field
The present invention relates to a kind of surface plasma nano catalysis material Ag3PO4/ AgCl and its preparation method and application,
Belong to nano-photocatalyst material field.
Background technology
Preservative and antibacterials are widely used in personal-care supplies and medical.With expanding economy, people
Use of the class to nursing materials and medicine progressively increases, wherein the accumulation of the preservative for containing and antiseptic in human body and environment
Content also increases increasingly.Parabens is because its own excellent antiseptic property is so as in individuals such as toothpaste, perfume
It is widely used in the food such as nursing materials and beverage, can.Additionally, research finds the performance of P-hydroxybenzoic acid lipid
A certain degree of estrogen active is gone out, this is probably one of the reason for causing breast cancer.Based on this, Environmental Protection Agency is classified as
Emerging environmental contaminants.But the unique chemical constitution of parabens causes the chemical stability pole of its molecule
Height, therefore, traditional physics or chemical treatment method is difficult to be degraded.Catalysis material can destroy many constitutionally stable
Persistent organic pollutants, have turned into a kind of environment pollution control method with important application prospect at present.With TiO2It is base
Traditional catalysis material of plinth has photoresponse narrow range, the low shortcoming of quantum efficiency.In order to widen photoresponse scope, people adopt
With various Research on Methods novel visible catalysis materials, wherein surface plasma catalysis material is emerging study hotspot,
Surface plasma catalysis material has concentrated precious metal surface plasma resonance effect and compound semiconductor photocatalytic material
Advantage.By adjusting size, shape and the residing microenvironment of noble metal nano particles, photocatalysis material can be effectively widened
Expect the absorption to visible ray.Catalysis material and organic contamination can be also effectively reduced by the contact between metal and semiconductor
Contact berrier between thing molecule, makes the electronics inside system or hole effectively be transferred out, and has effectively facilitated photocatalysis body
The separation of photo-generate electron-hole pair, can improve the efficiency of Photocatalytic Degradation of Organic in system.But at present on Ag3PO4With
Application of the AgCl composite surface plasma nano materials in terms of photocatalysis has not been reported.
The content of the invention
The present invention is intended to provide a kind of surface plasma nano catalysis material, the surface plasma nano photocatalysis
Material is silver orthophosphate（Ag3PO4）- silver chlorate（AgCl）It is compound.The invention provides the surface plasma nano catalysis material
Preparation method and application, the material can photocatalysis degradation organic contaminant under visible light.
The invention provides a kind of surface plasma nano catalysis material, including following components in percentage by weight：
Ag3PO4：62% ~ 94%,
AgCl：6%~38%；
Ag3PO4With splendid photocatalytic activity, but easily there is light decomposition and photoetch, i.e. less stable；The presence of AgCl
Ag can be suppressed3PO4Photodissociation with corrosion, effectively raise its stability.
The invention provides a kind of preparation method of above-mentioned surface plasma nano catalysis material, including following step
Suddenly：
（1）Ag3PO4Preparation：NaH is completely dissolved with water2PO4Afterwards, dissolving is added drop-wise under mechanical agitation state complete
AgNO3In solution, persistently stir 4-6 hours again at room temperature, photochemical catalyst Ag is obtained3PO4, it is washed with deionized to water lotion
PH value be 6~7；
NaH2PO4And AgNO3Quality proportioning be：0.01~0.05:0.08~0.12；
（2）Surface plasma nano catalysis material Ag3PO4The preparation of/AgCl：To（1）In obtained Ag3PO4Middle dropwise addition
NaCl solution；Resulting solution centrifugal is separated after stirring 10-20 min, is washed with deionized to the pH value of water lotion and is
6~7, dried in drying baker, composite photo-catalyst Ag is obtained3PO4/AgCl；
NaCl and AgNO3Quality proportioning be：0.005~0.02:0.05~0.15.
Ag3PO4Not only for reaction template but also Ag ions can be provided, by ion exchange in Ag3PO4Surface forms AgCl, has
What is imitated enhances Ag3PO4Stability.
In above-mentioned preparation method, step（1）Described in Ag3PO4What is prepared concretely comprises the following steps：
1. the NaH of 0.6g is weighed2PO4It is dissolved in 50ml deionized waters, is fully added dropwise under mechanical agitation state after dissolving
50 ml concentration are the AgNO of 0.3M3Solution, i.e. sodium dihydrogen phosphate and silver nitrate in mass ratio 0.023：0.1 proportioning；
2. by NaH2PO4Solution and AgNO3After solution mixing, at room temperature in lasting stirring 4-6 hours.Further, step is 2.
Described in mixing time be 5 hours.
In above-mentioned preparation method, NaH2PO4Rate of addition for per second two drop；The rate of addition of NaCl solution is per second two
Drop.
In above-mentioned preparation method, step（2）Described in concentration of sodium chloride solution be 0.05-0.15 M.
Further, step（2）Described in sodium chloride and silver nitrate in mass ratio 0.011:0.1 proportioning.
In above-mentioned preparation method, step（2）Described in stirring time be 15 min；Step（2）Described in drying
The drying temperature that case is set is 75 DEG C.
The invention provides a kind of application of above-mentioned surface plasma nano catalysis material in degradation of organic substances.
The surface plasma nano catalysis material Ag3PO4/AgCl is particularly suitable for having as degraded in field of Environment Protection
The photochemical catalyst of machine thing, with wide range of application.Described catalysis material is pressed when methyl p-hydroxybenzoate is degraded
Methyl p-hydroxybenzoate concentration is 20 mg/L, takes 0.1g nano-photocatalyst materials, and light source is the xenon lamp of 300 W, uses optical filter
Ultraviolet light is filtered out, the reaction time is 40 min.
In the present invention, silver orthophosphate（Ag3PO4）Energy gap it is narrow, quantum yield is high（It is bigger than under the same conditions other
The quantum yield of multi-catalyst is high by nearly 20%）, splendid photocatalytic activity is shown in the degraded of organic pollution.With
Ag3PO4For the composite photo-catalyst of matrix has an absorptivity very high, and can prevent photoproduction load in conjunction with silver orthophosphate
（Ag3PO4）With silver chlorate（AgCl）The photoetch phenomenon that the former occurs in Photocatalytic Degradation Process can be effectively improved after compound,
So as to improve photocatalysis stability.
Beneficial effects of the present invention：
（1）AgCl is supported on Ag by the present invention3PO4Surface, using the plasma resonance effect of AgCl, effectively inhibit
Ag3PO4Photoetch with decompose, it is ensured that its stability under light illumination, and effectively increase its absorption to visible ray.
（2）The surface plasma nano catalysis material Ag that the present invention is provided3PO4The preparation process is simple of/AgCl, into
This relatively low, preparation time is short.
（3）The surface plasma nano catalysis material Ag that the present invention is provided3PO4/ AgCl, with photoresponse wide ranges,
The advantages of quantum efficiency is high, can be applied to field of Environment Protection, be especially applicable to the organic pollution in photocatalytic degradation water body.
Brief description of the drawings
Fig. 1 is the gained surface plasma nano catalysis material Ag of embodiment 13PO4The scanning electron microscope (SEM) photograph of/AgCl；
Fig. 2 is the design sketch of 1000 times of amplification in Fig. 1.
Fig. 3 is the gained surface plasma nano catalysis material Ag of embodiment 1 ~ 63PO4/ AgCl drops in visible light catalytic
Solve the degradation kinetics figure of methyl p-hydroxybenzoate.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Embodiment 1：
（1）Ag3PO4Preparation：Weigh 1.275g NaH2PO4, it is dissolved in 50 ml water, until completely dissolved, in mechanical agitation shape
The AgNO that 50ml concentration is 0.3 M is added dropwise under state3Solution, persistently stirs 5 hours again at room temperature, and photochemical catalyst is obtained
Ag3PO4, it is 6~7 to be washed with deionized to the pH value of water lotion；
（2）Ag3PO4The preparation of/AgCl：To（1）In obtained Ag3PO4It is added dropwise over the NaCl solution that 88 ml concentration are 0.1M.
Ag3PO4Not only for reaction template but also Ag ions can be provided, by ion exchange in Ag3PO4Surface forms AgCl, effective enhancing
Ag3PO4Stability.Resulting solution centrifugal is separated after stirring 15min, is washed with deionized to the pH of water lotion
It is 6~7 to be worth, and is dried in 75 DEG C of drying baker, and composite photocatalyst material Ag is obtained3PO4/AgCl-1；
（3）Ag3PO4/ AgCl active testings：With the P-hydroxybenzoic acid that Photocatalytic Activity for Degradation initial concentration is 20 mg/L
Methyl esters evaluates the photocatalytic activity of catalyst.Concretely comprise the following steps：Light source is the xenon lamp of 300W；Weigh the surface plasma of 0.1g
Body nano-photocatalyst material Ag3PO4/ AgCl-1 is put into 100 mL methyl ester solutions, and lucifuge stirs 30min to reach suction before reaction
Attached desorption equilibrium, every 5/5/10/10/10 min, takes 3 mL reaction solutions, filtering, using ultra-violet and visible spectrophotometer point
Analysis substrate absorbance change.Using C/C0To evaluate degradation rate, wherein C is the absorbance of solution after illumination t min, C0It is solution
Initial absorbance.Photocatalytic degradation experimental result shows, after illumination 40min, the degradation rate of methyl p-hydroxybenzoate is reachable
90%。
Embodiment 2
（1）Ag3PO4Preparation：Weigh 1.1g NaH2PO4, it is dissolved in 50 ml water, until completely dissolved, in mechanical agitation state
Under be added dropwise over the AgNO that 50ml concentration is 0.3 M3Solution, persistently stirs 5 hours again at room temperature, and photochemical catalyst Ag is obtained3PO4,
It is 6~7 to be washed with deionized to the pH value of water lotion；
（2）Ag3PO4The preparation of/AgCl：To（1）In obtained Ag3PO4It is added dropwise over the NaCl solution that 70 ml concentration are 0.1M.
Ag3PO4Not only for reaction template but also Ag ions can be provided, by ion exchange in Ag3PO4Surface forms AgCl, effective enhancing
Ag3PO4Stability.Resulting solution centrifugal is separated after stirring 15min, is washed with deionized to the pH of water lotion
It is 6~7 to be worth, and is dried in 75 DEG C of drying baker, and composite photocatalyst material Ag is obtained3PO4/AgCl-2；
（3）Ag3PO4/ AgCl active testings：With the P-hydroxybenzoic acid that Photocatalytic Activity for Degradation initial concentration is 20 mg/L
Methyl esters evaluates the photocatalytic activity of catalyst.Concretely comprise the following steps：Light source is the xenon lamp of 300W；Weigh the surface plasma of 0.1g
Body nano-photocatalyst material Ag3PO4/ AgCl-2 is put into 100 mL methyl ester solutions, and lucifuge stirs 30min to reach suction before reaction
Attached desorption equilibrium, every 5/5/10/10/10 min, takes 3 mL reaction solutions, filtering, using ultra-violet and visible spectrophotometer point
Analysis substrate absorbance change.Using C/C0To evaluate degradation rate, wherein C is the absorbance of solution after illumination t min, C0It is solution
Initial absorbance.Photocatalytic degradation experimental result shows, after illumination 40min, the degradation rate of methyl esters is up to 92%.
Embodiment 3
（1）Ag3PO4Preparation：Weigh 0.8g NaH2PO4, it is dissolved in 50 ml water, until completely dissolved, in mechanical agitation state
Under be added dropwise over 50ml concentration be 0.3M AgNO3Solution, persistently stirs 5 hours again at room temperature, and photochemical catalyst Ag is obtained3PO4,
It is 6~7 to be washed with deionized to the pH value of water lotion；
（2）Ag3PO4The preparation of/AgCl：To（1）In obtained Ag3PO4It is added dropwise over the NaCl solution that 60 ml concentration are 0.1M.
Ag3PO4Not only for reaction template but also Ag ions can be provided, by ion exchange in Ag3PO4Surface forms AgCl, effective enhancing
Ag3PO4Stability.Resulting solution centrifugal is separated after stirring 15min, is washed with deionized to the pH of water lotion
It is 6~7 to be worth, and is dried in 75 DEG C of drying baker, and composite photocatalyst material Ag is obtained3PO4/AgCl-3；
（3）Ag3PO4/ AgCl active testings：With the P-hydroxybenzoic acid that Photocatalytic Activity for Degradation initial concentration is 20 mg/L
Methyl esters evaluates the photocatalytic activity of catalyst.Concretely comprise the following steps：Light source is the xenon lamp of 300W；Weigh the surface plasma of 0.1g
Body nano-photocatalyst material Ag3PO4/ AgCl-3 is put into 100 mL methyl ester solutions, and lucifuge stirs 30min to reach suction before reaction
Attached desorption equilibrium, every 5/5/10/10/10 min, takes 3 mL reaction solutions, filtering, using ultra-violet and visible spectrophotometer point
Analysis substrate absorbance change.Using C/C0To evaluate degradation rate, wherein C is the absorbance of solution after illumination t min, C0It is solution
Initial absorbance.Photocatalytic degradation experimental result shows that after the min of illumination 40, the degradation rate of methyl esters is up to 94%.
Embodiment 4：
（1）Ag3PO4Preparation：Weigh 0.6g NaH2PO4, it is dissolved in 50 ml water, until completely dissolved, in mechanical agitation state
Under be added dropwise over 50ml concentration be 0.3M AgNO3Solution, persistently stirs 5 hours again at room temperature, and photochemical catalyst Ag is obtained3PO4,
It is 6~7 to be washed with deionized to the pH value of water lotion；
（2）Ag3PO4The preparation of/AgCl：To（1）In obtained Ag3PO4It is added dropwise over the NaCl solution that 50 ml concentration are 0.1M.
Ag3PO4Not only for reaction template but also Ag ions can be provided, by ion exchange in Ag3PO4Surface forms AgCl, effective enhancing
Ag3PO4Stability.Resulting solution centrifugal is separated after stirring 15min, is washed with deionized to the pH of water lotion
It is 6~7 to be worth, and is dried in 75 DEG C of drying baker, and composite photocatalyst material Ag is obtained3PO4/AgCl-4；
（3）Ag3PO4/ AgCl active testings：With the P-hydroxybenzoic acid that Photocatalytic Activity for Degradation initial concentration is 20 mg/L
Methyl esters evaluates the photocatalytic activity of catalyst.Concretely comprise the following steps：Light source is the xenon lamp of 300W；Weigh the surface plasma of 0.1g
Body nano-photocatalyst material Ag3PO4/ AgCl-4 is put into 100 mL methyl ester solutions, and lucifuge stirs 30min to reach suction before reaction
Attached desorption equilibrium, every 5/5/10/10/10 min, takes 3 mL reaction solutions, filtering, using ultra-violet and visible spectrophotometer point
Analysis substrate absorbance change.Using C/C0To evaluate degradation rate, wherein C is the absorbance of solution after illumination t min, C0It is solution
Initial absorbance.Photocatalytic degradation experimental result shows, after illumination 40min, the degradation rate of methyl esters is up to 100%.
Embodiment 5：
（1）Ag3PO4Preparation：Weigh 0.45g NaH2PO4, it is dissolved in 50 ml water, until completely dissolved, in mechanical agitation shape
The AgNO that 50ml concentration is 0.3M is added dropwise under state3Solution, persistently stirs 5 hours again at room temperature, and photochemical catalyst is obtained
Ag3PO4, it is 6~7 to be washed with deionized to the pH value of water lotion；
（2）Ag3PO4The preparation of/AgCl：To（1）In obtained Ag3PO4It is added dropwise over the NaCl solution that 40 ml concentration are 0.1M.
Ag3PO4Not only for reaction template but also Ag ions can be provided, by ion exchange in Ag3PO4Surface forms AgCl, effective enhancing
Ag3PO4Stability.Resulting solution centrifugal is separated after stirring 15min, is washed with deionized to the pH of water lotion
It is 6~7 to be worth, and is dried in 75 DEG C of drying baker, and composite photocatalyst material Ag is obtained3PO4/AgCl-5；
（3）Ag3PO4/ AgCl active testings：With the P-hydroxybenzoic acid that Photocatalytic Activity for Degradation initial concentration is 20 mg/L
Methyl esters evaluates the photocatalytic activity of catalyst.Concretely comprise the following steps：Light source is the xenon lamp of 300W；Weigh the surface plasma of 0.1g
Body nano-photocatalyst material Ag3PO4/ AgCl-5 is put into 100 mL methyl ester solutions, and lucifuge stirs 30min to reach suction before reaction
Attached desorption equilibrium, every 5/5/10/10/10 min, takes 3 mL reaction solutions, filtering, using ultra-violet and visible spectrophotometer point
Analysis substrate absorbance change.Using C/C0To evaluate degradation rate, wherein C is the absorbance of solution after illumination t min, C0It is solution
Initial absorbance.Photocatalytic degradation experimental result shows, after illumination 40min, the degradation rate of methyl esters is up to 100%.
Embodiment 6：
（1）Ag3PO4Preparation：Weigh 0.32g NaH2PO4, it is dissolved in 50 ml water, until completely dissolved, in mechanical agitation shape
The AgNO that 50ml concentration is 0.3M is added dropwise under state3Solution, persistently stirs 5 hours again at room temperature, and photochemical catalyst is obtained
Ag3PO4, it is 6~7 to be washed with deionized to the pH value of water lotion；
（2）Ag3PO4The preparation of/AgCl：To（1）In obtained Ag3PO4It is added dropwise over the NaCl solution that 30 ml concentration are 0.1M.
Ag3PO4Not only for reaction template but also Ag ions can be provided, by ion exchange in Ag3PO4Surface forms AgCl, effective enhancing
Ag3PO4Stability.Resulting solution centrifugal is separated after stirring 15min, is washed with deionized to the pH of water lotion
It is 6~7 to be worth, and is dried in 75 DEG C of drying baker, and composite photocatalyst material Ag is obtained3PO4/AgCl-6；
（3）Ag3PO4/ AgCl active testings：With the P-hydroxybenzoic acid that Photocatalytic Activity for Degradation initial concentration is 20 mg/L
Methyl esters evaluates the photocatalytic activity of catalyst.Concretely comprise the following steps：Light source is the xenon lamp of 300W；Weigh the surface plasma of 0.1g
Body nano-photocatalyst material Ag3PO4/ AgCl-6 is put into 100 mL methyl ester solutions, and lucifuge stirs 30min to reach suction before reaction
Attached desorption equilibrium, every 5/5/10/10/10 min, takes 3 mL reaction solutions, filtering, using ultra-violet and visible spectrophotometer point
Analysis substrate absorbance change.Using C/C0To evaluate degradation rate, wherein C is the absorbance of solution after illumination t min, C0It is solution
Initial absorbance.Photocatalytic degradation experimental result shows, after illumination 40min, the degradation rate of methyl esters is up to 100%.
Effect detection explanation：
Electronic Speculum is detected：Fig. 1, Fig. 2 are the scanning electron microscope (SEM) photograph of gained photochemical catalyst.Wherein Fig. 1 is the scanning electron microscope (SEM) photograph under μm unit,
Fig. 2 is the scanning electron microscope (SEM) photograph under nm units.Ag as obtained by Electronic Speculum is prepared to embodiment 13PO4/ AgCl is detected, considerable
Measure and be supported on Ag3PO4The AgCl on surface is in granular form or spherical shape, and its size dimension is about between 1~4nm.
Fig. 3 is the gained surface plasma nano catalysis material Ag of embodiment 1 ~ 63PO4/ AgCl drops in visible light catalytic
Solve the degradation kinetics figure of methyl p-hydroxybenzoate.It can be seen that the min of catalysis material 40 prepared in the present invention
It is interior can be by the degradable of methyl p-hydroxybenzoate that initial concentration is 20 mg/L, it is seen that the catalysis material has excellent
Photocatalysis performance.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (9)
1. a kind of surface plasma nano catalysis material, it is characterised in that：Including following components in percentage by weight：
Ag3PO4：62% ~ 94%,
AgCl：6%~38%.
2. the preparation method of the surface plasma nano catalysis material described in a kind of claim 1, it is characterised in that：Including
Following steps：
（1）Ag3PO4Preparation：NaH is completely dissolved with water2PO4Afterwards, the complete AgNO of dissolving is added drop-wise under mechanical agitation state3
In solution, persistently stir 4-6 hours again at room temperature, photochemical catalyst Ag is obtained3PO4, it is washed with deionized to the pH value of water lotion
It is 6~7；
NaH2PO4And AgNO3Quality proportioning be：0.01~0.05:0.08~0.12；
（2）Surface plasma nano catalysis material Ag3PO4The preparation of/AgCl：To（1）Obtained Ag3PO4Middle dropwise addition NaCl
Solution；Resulting solution centrifugal is separated after stirring 10-20 min, be washed with deionized the pH value to water lotion for 6~
7, dried in drying baker, nano-photocatalyst material Ag is obtained3PO4/AgCl；
NaCl and AgNO3Quality proportioning be：0.005~0.02:0.05~0.15.
3. the preparation method of surface plasma nano catalysis material according to claim 2, it is characterised in that：Step
（1）Described in Ag3PO4What is prepared concretely comprises the following steps：
1. the NaH of 0.6g is weighed2PO4It is dissolved in 50ml deionized waters, is fully added dropwise to 50 under mechanical agitation state after dissolving
Ml concentration is the AgNO of 0.3M3Solution, i.e. sodium dihydrogen phosphate and silver nitrate in mass ratio 0.023：0.1 proportioning；
2. by NaH2PO4Solution and AgNO3After solution mixing, at room temperature in lasting stirring 5 hours.
4. the preparation method of surface plasma nano catalysis material according to claim 2, it is characterised in that：
NaH2PO4Rate of addition for per second two drop；The rate of addition of NaCl solution is per second two drops.
5. the preparation method of surface plasma nano catalysis material according to claim 2, it is characterised in that：Step
（2）Described in NaCl solution concentration be 0.05-0.15 M.
6. the preparation method of surface plasma nano catalysis material according to claim 2, it is characterised in that：Step
（2）Middle NaCl and AgNO3Quality proportioning be：0.011: 0.1.
7. the preparation method of surface plasma nano catalysis material according to claim 1, it is characterised in that：Step
（2）Described in stirring time be 15 min；Step（2）Described in drying baker set drying temperature be 75 DEG C.
8. application of the surface plasma nano catalysis material described in a kind of claim 1 in degradation of organic substances.
9. application according to claim 8, it is characterised in that：The nano-photocatalyst material takes 0.1g, used as substrate
Methyl p-hydroxybenzoate concentration is 20 mg/L, and the light source is the xenon lamp of 300 W, and ultraviolet light is filtered out with optical filter, reaction
Time is 40 min.
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| CN107744821A (en) * | 2017-09-29 | 2018-03-02 | 天津大学 | A kind of magnetic photocatalyst with SPR responses and preparation method thereof |
| CN113797945A (en) * | 2021-10-03 | 2021-12-17 | 桂林理工大学 | Ag/AgCl/Ag3PO4Preparation method of heterojunction composite photocatalyst |
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| CN102247874A (en) * | 2011-05-26 | 2011-11-23 | 上海电力学院 | Silver chloride-silver phosphate composite photocatalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102247874A (en) * | 2011-05-26 | 2011-11-23 | 上海电力学院 | Silver chloride-silver phosphate composite photocatalyst and preparation method thereof |
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| YINGPU BI ET AL.: "Facile synthesis of rhombic dodecahedral AgX/Ag3PO4(X = Cl, Br, I)heterocrystals with enhanced photocatalytic properties and stabilitiesw", 《PHYS. CHEM. CHEM. PHYS.》 * |
| ZHIHONG CHEN ET AL.: "High-Efficiency Visible-Light-Driven Ag3PO4/AgI Photocatalysts:Z‑Scheme Photocatalytic Mechanism for Their Enhanced Photocatalytic Activity", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107744821A (en) * | 2017-09-29 | 2018-03-02 | 天津大学 | A kind of magnetic photocatalyst with SPR responses and preparation method thereof |
| CN113797945A (en) * | 2021-10-03 | 2021-12-17 | 桂林理工大学 | Ag/AgCl/Ag3PO4Preparation method of heterojunction composite photocatalyst |
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