CN102167389B - High-activity silver chloride convex crystal and preparation method thereof - Google Patents
High-activity silver chloride convex crystal and preparation method thereof Download PDFInfo
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- CN102167389B CN102167389B CN2011100413532A CN201110041353A CN102167389B CN 102167389 B CN102167389 B CN 102167389B CN 2011100413532 A CN2011100413532 A CN 2011100413532A CN 201110041353 A CN201110041353 A CN 201110041353A CN 102167389 B CN102167389 B CN 102167389B
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Abstract
The invention relates to a high-activity silver chloride convex crystal and a preparation method thereof. The crystal has a convex bent crystal face. The preparation method comprises the following steps of: dissolving a chloric ionic solution to deionized water, fully stirring for 2-4h at a room temperature, then adding silver nitride to the stirred solution, stirring for 30-60min so that the solution is uniformly mixed, putting the mixed solution into a high pressure autoclave with a polytetrafluoroethylene liner, reacting for 1-8h at 120-160 DEG C, and then cooling, separating and drying to obtain the high-activity silver chloride convex crystal. In the invention, the synthesis method and the experimental steps are simple, the preparation yield is high, and the mass production can be achieved; the synthesized silver chloride convex crystal has the convex bent crystal face and higher surface activity; and a photocatalyst prepared from the silver chloride convex crystal has strong absorbability in a visible region and stronger photocatalysis activity.
Description
Technical field
The present invention relates to a kind of high reactivity Silver monochloride crystal, particularly a kind of high reactivity convex surface Silver monochloride crystal and preparation method thereof can be used for the environmental technology field of visible light degradable organic pollutant.
Background technology
The development of emerging conductor photocatalysis technology is curbed environmental pollution and is solved the energy starved cleaning technique for the mankind provide a kind of.Through photocatalysis technology, utilize organic pollutant and the heavy metal contaminants of sun power in can degradation of sewage, also can hydrogen energy source be provided photodissociation water simultaneously.So photocatalysis technology more and more obtains people's attention.But present photocatalysis technology very major part also is in the fundamental research stage, and the preparation that mainly concentrates on visible light-responded material is explored.Silver monochloride is a kind of photochromics, is widely used in imaging field, but its application in photocatalysis field has important breakthrough in recent years.Silver monochloride has become very important material in the photocatalysis field.But preparing method's difference has significant effects to its activity.Improve the crystallinity of Silver monochloride or change pattern and can increase its activity in photochemical catalysis.
Silver monochloride is a research focus being applied in of photocatalysis field in recent years." German applied chemistry " (Angew.Chem.Int.Ed.2008; 47,7931-7933), " Europe chemistry " (Chem.Eur.J.2010; 16; 538-544) with " chemical communication " (Chem.Commun., 2009,6551-6553) reported the application of Silver monochloride at the Photocatalytic Activity for Degradation organic pollutant.But preparing method's more complicated of the Silver monochloride of its report.Therefore, with simple experimental technique and the synthetic Silver monochloride crystal of step important practical application meaning is arranged with high reactivity pattern.
Summary of the invention
The purpose of this invention is to provide a kind of high reactivity Silver monochloride convex surface crystal and preparation method thereof; The crooked crystal face of this convex surface crystal tool protrusion; The photocatalyst that changes into generation has higher photocatalytic activity, and ability is degradable organic pollutant effectively, the big separate easily of particle.
A kind of high reactivity Silver monochloride convex surface crystal, this crystal has the crooked crystal face of protrusion.
Above-mentioned Silver monochloride convex surface crystal diameter is 0.2 ~ 4 μ m, has higher surface activity, has higher photocatalytic activity behind the formation photocatalyst, relatively is adapted at degradable organic pollutant in the practical application.
Above-mentioned high reactivity Silver monochloride convex surface crystalline preparation method, step is following:
(1) chloride ionic liquid is dissolved into the abundant 2 ~ 4h of stirring in the deionized water;
(2) after above-mentioned stirring, add Silver Nitrate in the solution, stir and solution was mixed in 30 ~ 60 minutes;
(3) mixing solutions is transferred to had in the teflon-lined autoclave, at 140 ~ 160 ℃ of reaction 1 ~ 8h down, behind the naturally cooling, spinning, washing, dry product.
The consumption mass ratio relation extents of described chloride ionic liquid and deionized water, Silver Nitrate is (0.4-1.0): (50-100): 0.4
Described chloride ionic liquid is chlorination 1-hexadecyl-3-Methylimidazole (C
16MimCl).
The photocatalyst that makes under the illumination of above-mentioned Silver monochloride convex surface crystal.
The Preparation of catalysts method is: above-mentioned Silver monochloride convex surface crystal is added in the deionized water (mass ratio is 0.2:100), and with 500W xenon lamp irradiation 1h, the filtration washing drying obtains under constantly stirring.
Silver monochloride convex surface crystal of the present invention and preparation method thereof has following advantage:
1. utilize the stablizer of chloride ionic liquid chlorination 1-hexadecyl-3-Methylimidazole, through the synthesizing chlorinated silver-colored convex surface crystal of method of the auxiliary hydro-thermal of ionic liquid as synthesizing chlorinated silver-colored convex surface crystalline reaction chlorine source and control crystal growth.The Silver monochloride convex surface crystalline size that forms can be regulated through reaction times and temperature of reaction easily;
2. compound method and experimental procedure are simple, and the preparation productive rate is high, can prepare in a large number;
3. synthetic Silver monochloride convex surface crystal has unique pattern, the crooked crystal face of plane of crystal, and its surfactivity is higher, and its photocatalyst that under illumination, forms has very strong absorption at visible region;
4. compare with the crystal formation photocatalyst of the cube Silver monochloride of ortho-water thermal synthesis, the activity of the crystal formation photocatalyst of Silver monochloride convex surface is higher relatively under visible light.
The available following method of test of the photocatalytic activity that the present invention is proposed is carried out:
Photochemical catalysis test (transverse section 30cm in glass beaker
2, high 5cm) carry out under the normal temperature and pressure.Light source is selected the 500W xenon lamp for use.Come the photocatalytic activity of assess sample with tropeolin-D.Take by weighing 0.2g sample dispersion (20mg/L) in the 100mL methyl orange solution.Before the light-catalyzed reaction test, lucifuge magnetic agitation 30min makes tropeolin-D reach adsorption equilibrium at catalyst surface, and every at a distance from 5min sampling 5mL after the beginning illumination, spinning is got supernatant and used the measurement of ultraviolet-visible spectrophotometer absorbancy.As a comparison, with ortho-water by the use of thermal means synthetic Silver monochloride crystal formation photocatalyst and the adulterated TiO of N
2Under equal experiment condition, carried out the photocatalytic activity test.
Through the photochemical catalysis test, the crystal formation photocatalyst of Silver monochloride convex surface can be intact with methyl orange degradation at 15min, and the photocatalyst that the Silver monochloride of common Hydrothermal Preparation forms is complete with methyl orange degradation at 30min, the adulterated TiO of N
2At 30min with methyl orange degradation 20%.It is thus clear that with ionic liquid synthetic Silver monochloride convex surface crystal on photocatalytic applications with the cube Silver monochloride crystal and the adulterated TiO of N of common Hydrothermal Preparation
2Compare and have higher activity.
Description of drawings
Fig. 1 is the X ray picture of the embodiment of the invention 1 product;
Fig. 2 is the SEM figure of the embodiment of the invention 1 product;
Fig. 3 is the photocatalyst and the N doped Ti O of instance 1 product of the present invention and formation
2The ultraviolet-visible diffuse-reflectance absorb figure;
Fig. 4 is the X-ray diffractogram of the embodiment of the invention 2 products;
Fig. 5 is the SEM figure of the embodiment of the invention 2 products.
Embodiment:
Embodiment 1
Measure the 90ml deionized water and join in the beaker, take by weighing 0.4g ionic liquid (C
16MimCl) join above-mentioned solution, constantly stir ionic liquid is dissolved in the water fully, form all with solution, subsequently the solution that 10ml contains the 0.4g Silver Nitrate is injected above-mentioned solution rapidly, constantly stirring makes the uniform milky white solution of solution.It is that 120ml has the teflon-lined autoclave that mixture is put into volume, 160 ℃ of reactions 4 hours, naturally cools to room temperature; Use the centrifugal method sample separation; And cleaning sample respectively 3 times with deionized water and absolute ethyl alcohol, dry 24h obtains product Silver monochloride convex surface crystal.Get 0.2g Silver monochloride curved crystals and put in the 100ml deionized water, constantly stir 1h down in 500W xenon lamp irradiation, then filtration washing and in vacuum chamber dry formation photocatalyst.
Accompanying drawing 1 (red) is the X-ray diffractogram of present embodiment products therefrom; Can know by figure; Peak position on the standard card of the Silver monochloride of equal cube of phase of each diffraction peak of this product (JCPDS file no.31-1238) (green) is corresponding, and it is stronger not have assorted peak and diffraction peak, explains that product is pure cube phase Silver monochloride.Accompanying drawing 2 is the SEM figure of present embodiment products therefrom, and at 1-2 μ m, plane of crystal is the crooked crystal face of protrusion by the size of scheming to know crystal grain.Accompanying drawing 3 is the photocatalyst (indigo plant) and the N doped Ti O of present embodiment products therefrom (red) and formation thereof
2The UV, visible light diffuse-reflectance of (deceiving) absorbs the contrast of figure, can find out that it had stronger absorption at visible region after Silver monochloride convex surface crystal changed into photocatalyst, and this is owing to changing into the surface plasma body resonant vibration effect of photocatalyst silver nano-grain.
Above detection with analysis integrated proof the product that obtains of present embodiment be convex surface Silver monochloride crystal cube mutually.The Silver monochloride convex surface crystal that adopts the inventive method preparation has stronger visible light-respondedly being converted into after light is urged agent, and have the high light catalytic efficiency (, has obtained in photocatalytic degradation organic contamination field using effectively.
Measure the 50ml deionized water and join in the beaker, take by weighing 1g ionic liquid (C
16MimCl) join above-mentioned solution, constantly stirring is dissolved ionic liquid fully, measures the solution 10ml that contains the 0.4g Silver Nitrate subsequently and injects above-mentioned solution rapidly, constantly stirs to make solution even.It is that 100ml has the teflon-lined autoclave that mixture is put into volume, 160 ℃ of reactions 4 hours, naturally cools to room temperature, the spinning sample, and clean sample respectively 3 times, vacuum-drying 24 hours with deionized water and absolute ethyl alcohol.
Accompanying drawing 4 is the X-ray diffractogram of this enforcement products therefrom, is known by figure, and this product is the Silver monochloride crystal of pure cube phase.Accompanying drawing 5 is the SEM figure of the product of present embodiment, and the Silver monochloride convex surface crystalline size that can be found out by Fig. 5 reaches 3-5 μ m.The reason that size increases is that higher reaction density makes crystal grow into large-sized Silver monochloride convex surface crystal fast, has reflected that also ionic liquid also can play good function of stabilizer under higher reaction density condition simultaneously.
Embodiment 3
Measure the 100ml deionized water and join in the beaker, take by weighing 0.4g ionic liquid (C
16MimCl) join above-mentioned solution, constantly stirring is dissolved ionic liquid fully, takes by weighing the 0.4g Silver Nitrate subsequently and dissolves in the above-mentioned solution, constantly stirs to make solution even.It is that 120ml has the teflon-lined autoclave that mixture is put into volume, at 140 ℃ of reaction 8h, naturally cools to room temperature, uses the centrifugal method sample separation, and cleans sample respectively 3 times with deionized water and absolute ethyl alcohol, vacuum-drying 24h.
Claims (1)
1. high reactivity Silver monochloride convex surface crystalline preparation method is characterized in that step is following:
Measure the 50ml deionized water and join in the beaker, take by weighing 1g ionic liquid C
16MimCl joins above-mentioned solution, constantly stirs ionic liquid is dissolved fully, measures the solution 10ml that contains the 0.4g Silver Nitrate subsequently and injects above-mentioned solution rapidly, constantly stirs to make solution even; It is that 100ml has the teflon-lined autoclave that mixture is put into volume, 160 ℃ of reactions 4 hours, naturally cools to room temperature, the spinning sample, and clean sample respectively 3 times, vacuum-drying 24 hours with deionized water and absolute ethyl alcohol.
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| CN2011100413532A CN102167389B (en) | 2011-02-21 | 2011-02-21 | High-activity silver chloride convex crystal and preparation method thereof |
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| CN102167389B true CN102167389B (en) | 2012-11-07 |
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| CN102698776B (en) * | 2012-05-28 | 2014-04-16 | 华北电力大学 | Method for preparing silver chloride particles with flower-shaped micrometer structures |
| CN103466684B (en) * | 2013-09-05 | 2015-03-11 | 山东大学 | High-activity cubic-block silver chloride micron-crystal and electrochemical preparation method thereof |
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Non-Patent Citations (1)
| Title |
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| Zaizhu Lou et al..One-step synthesis of AgBr microcrystals with different morphologies by ILs-assisted hydrothermal method.《CrystEngComm》.2011,第13卷1789-1793. * |
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