CN104549518B - Ag-AgCl-polyhydroxymethyl acrylamide microgel photocatalytic composite material and preparation method thereof - Google Patents
Ag-AgCl-polyhydroxymethyl acrylamide microgel photocatalytic composite material and preparation method thereof Download PDFInfo
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- CN104549518B CN104549518B CN201510032584.5A CN201510032584A CN104549518B CN 104549518 B CN104549518 B CN 104549518B CN 201510032584 A CN201510032584 A CN 201510032584A CN 104549518 B CN104549518 B CN 104549518B
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Abstract
The invention discloses an Ag-AgCl-polyhydroxymethyl acrylamide microgel photocatalytic composite material and a preparation method thereof. The preparation method comprises the following steps: preparing a polyhydroxymethyl acrylamide microgel by inverse-phase emulsion polymerization, reducing a silver ammonia solution under mild conditions by using ethylene glycol as a reducer to synthesize a microgel-carried nano Ag composite material, and carrying out redox reaction with an organic matter CCl4 to finally obtain the Ag-AgCl-polyhydroxymethyl acrylamide microgel photocatalytic composite material. The preparation method is simple, green and environment-friendly; in the synthetic process, the organic pollutant CCl4 can be converted into pollution-free amorphous carbon, and the relative content of nano Ag and AgCl in the photocatalytic composite material can be effectively controlled by controlling the conversion degree of CCl4 to obtain the photocatalytic composite material with different catalytic activities; and the photocatalytic composite material can be used for photocatalytically degrading organic dyes, and can be recycled after degradation.
Description
Technical field
The invention belongs to photocatalytic activity material preparation technical field and in particular to a kind of richness hydroxyl polymer-network method
Optic catalytic composite material of load ag-agcl and preparation method thereof.
Background technology
Photocatalysis performance causes the concern of people in recent years, and it is mainly used in photocatalytic water, photocatalytic degradation Organic substance, life
The aspects such as thing sterilization, processing the Organic substance in industrial wastewater waste gas with photochemical degradating is a kind of economic and environment-friendly method, with regard to
Noble metal nano ag particle is combined with silver halide (agx) to be had surface plasmon resonance effect and is applied to photocatalytic degradation
The research of Organic substance in water becomes focus.Correlational study shows, the surface plasma resonance effect that Nanoparticle Modified produces increases
Strong catalyst to visible light-responded and efficiently separating so that photocatalytic activity improves to electron-hole, and because surface etc. from
Daughter resonance effect, so that ag@agcl not only can absorb visible ray strongly, prevents electron-hole under electrostatic force
Compound, meanwhile, cl on hole and interface-Reaction can generate with strong oxidizing property cl0Free radical, thus further increase
The photocatalytic activity of catalyst.Document report mainly prepares support type by the way of chemical deposition is combined with photoreduction method
Ag@agcl photocatalyst, for example, wang (angew chem int ed, 2008,47:7931-7933) adopt ion exchange and
Photoreduction method has synthesized ag@agcl plasma photocatalysis agent of different shapes；Zhou Jianwei etc. (material Leader, 2009,23:
177-180；Artificial intraocular lensess' journal, 2011,40:1563-1568) adopt chemical deposition-photoreduction met hod, ag-agcl is supported on
Mesoporous material mcm-41 and al2o3On, it is prepared for ag-agcl/mcm-41 and ag-agcl/al respectively2o3Composite photocatalyst material.
Catalytic effect during degradable organic pollutant for the photocatalyst of these methods synthesis is all preferable, but the conjunction of photocatalyst
One-tenth process is complex, and mostly needs to introduce other light sources in building-up process, causes the waste of resource.Additionally, related literary composition
Offer and also report, with silver nitrate for silver-colored source, with hexadecyl Trimethylamine be chlorine source and synthesis of surfactant ag-agcl receives
Rice corpuscles, and the different ag-agcl nanoparticle of pattern can be obtained by the concentration controlling hexadecyl Trimethylamine
(langmuir, 2015,31:602-610), the method synthesis is relatively simple, but ag-agcl nanoparticle in actual applications
It is difficult to reclaim, reuse.
Content of the invention
The technical problem to be solved is to provide a kind of ag-agcl- poly- n-methylolacrylamide microgel light
Catalytic composite materials and the preparation method of this composite.
The poly- n-methylolacrylamide of ag-agcl- solving the technical scheme is that present invention of above-mentioned technical problem is micro-
Gel optic catalytic composite material is prepared by following methods:
1st, prepare poly- n-methylolacrylamide microgel
Using reversed emulsion polymerization, with n, n '-methylene-bisacrylamide is cross-linking agent, Ammonium persulfate. is initiator,
Tetramethylethylenediamine be accelerator, span-80 and tween 80 mass ratio be 8～15:1 mixed liquor be surfactant, ring
Hexane is oil phase solvent, under inert gas shielding, n-methylolacrylamide polymerized at normal temperature is reacted 3～7 hours, is prepared into poly-
N-methylolacrylamide microgel.
2nd, prepare ag- poly- n-methylolacrylamide microgel composite
Poly- n-methylolacrylamide microgel is dispersed in ethylene glycol, adds freshly prepared silver ammino solution, often
Temperature stirring 30 minutes, adds naoh aqueous solution, and stirring added naoh aqueous solution after 1 hour, and poly- n-methylolacrylamide is micro- solidifying
The quality of glue is 1:2.5～3.2:0.5～0.8 with the ratio of the gross mass of the initial mass of silver nitrate, naoh in silver ammino solution, often
Temperature reaction 15～20 hours, is prepared into ag- poly- n-methylolacrylamide microgel composite.
3rd, synthesize ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material
Poly- for ag- n-methylolacrylamide microgel composite is added to ccl4In the mixed solution of isopropanol, ag-
Poly- n-methylolacrylamide microgel composite and ccl4Quality-volume ratio be 1g:7～20ml, ccl4Body with isopropanol
Long-pending ratio is 0.04～0.10:1, room temperature oscillating reactionss 8～15 hours, obtains ag-agcl- poly- n-methylolacrylamide microgel light
Catalytic composite materials.
In above-mentioned step 1, n-methylolacrylamide, n, n '-methylene-bisacrylamide, Ammonium persulfate., tetramethyl second
The mass ratio of diamidogen is 1:(0.035～0.045): (0.08～0.12): (0.035～0.045), preferably methylol acryloyl
Amine, n, n '-methylene-bisacrylamide, Ammonium persulfate., the mass ratio of tetramethylethylenediamine are 1:0.04:0.09:0.04.
In above-mentioned step 2, in the quality of preferably poly- n-methylolacrylamide microgel and silver ammino solution, silver nitrate is first
Prothyl amount, the ratio of the gross mass of naoh are 1:3:0.6.
In above-mentioned step 2, the volume of the further preferably naoh aqueous solution that second adds is to add for the first time
2 times of naoh aqueous solution volume.
On step 3 in, preferably ag- poly- n-methylolacrylamide microgel composite and ccl4Quality-volume ratio
For 1g:13ml.
The present invention with there is great amount of hydroxy group the poly- n-methylolacrylamide of micron order polymer-network method as carrier, using hydroxyl
Base and the high forces of nanometer ag, with ethylene glycol as reducing agent, reduce silver ammino solution in a mild condition using slow reducing process, will
Nano metal ag is carried on poly- n-methylolacrylamide micro-gel surface, larger surface area is had due to this microgel so as to
The load capacity of nano surface ag dramatically increases, obtain surface have pleated structure ag- poly- n-methylolacrylamide microgel multiple
Condensation material, then by itself and Organic substance ccl4Carry out redox reaction, finally give the poly- n-methylolacrylamide of ag-agcl-
Microgel optic catalytic composite material, this optic catalytic composite material granule larger it is easy to from reaction system separate.
The preparation method of the poly- n-methylolacrylamide microgel optic catalytic composite material of ag-agcl- of the present invention is simple, green
Environmental protection, not only can be by organic pollution ccl in its building-up process4It is converted into free of contamination agraphitic carbon, and by controlling
ccl4Transforming degree different catalysis can be obtained with the relative amount of nanometer ag and agcl in Effective Regulation optic catalytic composite material
The ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material of activity.The poly- n-methylolacrylamide of the present invention is micro-
The big size of gel is conducive to the stably dispersing of nanometer ag-agcl and giving full play to of performance, the poly- methylol of gained ag-agcl-
Acrylamide microgel optic catalytic composite material can be used for the organic dyestuff such as photo-catalytic degradation of methyl-orange, methyl blue, and degrades
Complete rear optic catalytic composite material recoverable.
Brief description
Fig. 1 is the environmental scanning electronic microscope figure of the poly- n-methylolacrylamide microgel of embodiment 1 preparation.
Fig. 2 is the environmental scanning electronic microscope figure of the ag- poly- n-methylolacrylamide microgel composite of embodiment 1 preparation.
Fig. 3 is the desk-top of the ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material of embodiment 1 preparation
Scanning electron microscope (SEM) photograph.
Fig. 4 is the enlarged drawing of Fig. 3.
Fig. 5 is poly- n-methylolacrylamide microgel (curve a) and the ag-agcl- poly- methylol propylene of embodiment 1 preparation
Amide microgel optic catalytic composite material (the xrd figure of curve b).
Fig. 6 be embodiment 1 preparation poly- n-methylolacrylamide microgel (the poly- n-methylolacrylamide of curve a), ag- is micro-
Gel complex material (curve b), the ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material (xps of curve c)
Full spectrogram.
Fig. 7 is ag- poly- n-methylolacrylamide microgel composite (curve b) and ag-agcl- poly- methylol acryloyl
Amine microgel composite (the Auger figure of silver element in curve c).
Fig. 8 is chlorine unit in ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material prepared by embodiment 1
The xps open score figure of element.
Fig. 9 is ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material (the curve a) of embodiment 1 preparation
With ag- poly- n-methylolacrylamide microgel composite (the xps open score figure of silver element in curve b).
Figure 10 is the environment of the ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material of embodiment 1 preparation
The energy spectrum diagram of scanning electron microscope (SEM) photograph marked region.
Figure 11 is the desk-top of the ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material of embodiment 2 preparation
Scanning electron microscope (SEM) photograph.
Figure 12 is the enlarged drawing of Figure 11.
Figure 13 is the environment of the ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material of embodiment 2 preparation
The energy spectrum diagram of scanning electron microscope (SEM) photograph marked region.
Figure 14 is the desk-top of the ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material of embodiment 3 preparation
Scanning electron microscope (SEM) photograph.
Figure 15 is the enlarged drawing of Figure 14.
Figure 16 is the environment of the ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material of embodiment 3 preparation
The energy spectrum diagram of scanning electron microscope (SEM) photograph marked region.
Figure 17 be blank control group (curve a), ag- poly- n-methylolacrylamide microgel composite (curve b) and
Ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material (curve d, the c, e) light degradation of embodiment 1～3 preparation
The degradation rate of methyl orange is with the change curve of degradation time.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
1st, prepare poly- n-methylolacrylamide microgel
In n2In atmosphere, 0.5g span-80 and 0.05g tween 80 are added in 70ml hexamethylene, stirs 1 hour, dispersion
Uniformly, it is configured to oil phase；1.2g n-methylolacrylamide is added in 5ml deionized water, stirs to being completely dissolved, be subsequently adding
0.05g n, n '-methylene-bisacrylamide, stirs to being completely dissolved, and the Ammonium persulfate. adding 0.5ml0.95mol/l is water-soluble
Liquid, is made into aqueous phase；Aqueous phase is added in above-mentioned scattered oil phase, is stirring evenly and then adding into the tetramethyl of 1ml 50g/l
Ethylenediamine solution, polymerized at normal temperature reacts 4 hours, and product deionized water and ethanol replace washing, natural subsidence, wash away oligomeric
Thing and unreacted monomer, dry naturally, obtain white powder poly- n-methylolacrylamide microgel (see Fig. 1).
2nd, prepare ag- poly- n-methylolacrylamide microgel composite
By 0.053g agno3It is dissolved in 1ml deionized water, be subsequently adding ammonia and be configured to silver ammino solution；By 0.018g
Poly- n-methylolacrylamide microgel is added in 30ml ethylene glycol, ultrasonic disperse 30 minutes, adds the silver-colored ammonia of above-mentioned new preparation
Solution, room temperature lucifuge stirs 30 minutes, is then added dropwise over the naoh aqueous solution of 1ml0.09mol/l in system, after dripping
Continue to stir 1 hour, then be added dropwise over the naoh aqueous solution of 2ml 0.09mol/l, continue stirring reaction 18 hours, product spends
Ionized water and ethanol replace washing, natural subsidence, and product dries naturally, obtains the poly- n-methylolacrylamide of black powder ag-
Microgel composite.From Figure 2 it can be seen that surface defines pleated structure after poly- n-methylolacrylamide microgel load ag.
3rd, synthesize ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material
Poly- for 0.006g ag- n-methylolacrylamide microgel composite is added to 80 μ l ccl4With 1ml isopropanol
Mixed solution in, room temperature oscillating reactionss 12 hours, reacted precipitation ethanol is replaced after washing with deionized water, natural
It is dried, obtain ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material (see Fig. 3 and 4).Can be seen by Fig. 5
Go out, ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material is micro- except the corresponding poly- n-methylolacrylamide of scope
Outside the unformed feature of gel, 38.2 °, 44.4 °, 64.6 °, 77.4 ° etc. characteristic diffraction peaks occurring respectively with cubic crystal
The diffraction of (111), (200), (220) and (311) lattice plane of system's silver is consistent；Additionally, 27.74 °, 32.16 °, 46.14 °,
54.74 °, 57.42 ° etc. equally characteristic peak, they correspond respectively to (111), (200), (220) of agcl, (311),
(222) crystal face.Can be drawn by Fig. 6～9, the ag3d of ag element in ag- poly- n-methylolacrylamide microgel composite3/2
With ag3d5/2In conjunction with can be 374.4ev, 368.3ev, ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material
The ag3d of middle ag element3/2With ag3d5/2In conjunction with can be ag element in the agcl of report in 372.7ev, 366.7ev, with document
ag3d3/2With ag3d5/2Compare in conjunction with energy (373.6ev, 367.6ev) and all decrease accordingly, see peak from the auger spectrum of ag
Shape also has in significant change, and the xps collection of illustrative plates of ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material and occurs
The peak of cl element.Agcl be there is also as can be seen that there is ag in optic catalytic composite material by Figure 10 and table 1.These characterize knot
The presence of ag-agcl composite construction of fruit all valid certificates.
Table 1 power spectrum elementary analysiss result
| Element | Wt% | At% |
| ck | 35.88 | 76.98 |
| ok | 4.52 | 7.29 |
| aum | 5.04 | 0.66 |
| clk | 4.17 | 3.03 |
| agl | 50.38 | 12.04 |
Embodiment 2
Poly- n-methylolacrylamide microgel and ag- poly- n-methylolacrylamide microgel composite in the present embodiment
Preparation method is same as Example 1.In the step 3 of embodiment 1, poly- for 0.006g ag- n-methylolacrylamide microgel is multiple
Condensation material is added to 50 μ l ccl4In the mixed solution of 1ml isopropanol, room temperature oscillating reactionss 12 hours, will be reacted heavy
After shallow lake ethanol replaces washing with deionized water, spontaneously dry, obtain ag-agcl- poly- n-methylolacrylamide microgel light and urge
Change composite, its characterization result is shown in Figure 11～13 and table 2.
Table 2 power spectrum elementary analysiss result
| Element | Wt% | At% |
| ck | 11.19 | 53.15 |
| aum | 6.28 | 1.82 |
| clk | 1.29 | 2.07 |
| agl | 81.25 | 42.96 |
Embodiment 3
Poly- n-methylolacrylamide microgel and ag- poly- n-methylolacrylamide microgel composite in the present embodiment
Preparation method is same as Example 1.In the step 3 of embodiment 1, poly- for 0.006g ag- n-methylolacrylamide microgel is multiple
Condensation material is added to 100 μ l ccl4In the mixed solution of 1ml isopropanol, room temperature oscillating reactionss 12 hours, will be reacted heavy
After shallow lake ethanol replaces washing with deionized water, spontaneously dry, obtain ag-agcl- poly- n-methylolacrylamide microgel light and urge
Change composite, its characterization result is shown in Figure 14～16 and table 3.
Table 3 power spectrum elementary analysiss result
| Element | Wt% | At% |
| ck | 9.94 | 43.03 |
| nk | 1.39 | 5.18 |
| ok | 1.63 | 5.30 |
| aum | 9.11 | 2.41 |
| clk | 6.61 | 9.70 |
| agl | 71.32 | 34.39 |
From the characterization result of embodiment 1～3, by the ccl that degrades4Effectively surface can be had pleated structure
The poly- n-methylolacrylamide of ag- is converted into ag-agcl- poly- n-methylolacrylamide optic catalytic composite material, and different ccl4With
The pattern of the ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material measuring has obvious difference, by power spectrum
It can be seen that the content of agcl is also different in the photocatalyst being formed.
In order to prove beneficial effects of the present invention, inventor adopts the poly- n-methylolacrylamide of ag- of embodiment 1 preparation micro-
The ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material photocatalysis fall of gel and embodiment 1～3 preparation
Solution methyl orange, concrete grammar and experimental result are as follows:
Respectively the ag-agcl- of poly- for 0.004g ag- n-methylolacrylamide microgel and embodiment 1～3 preparation is gathered
N-methylolacrylamide microgel optic catalytic composite material is added to 4 test tubes equipped with 5ml 10mg/l methyl orange aqueous solution
In, separately take a test tube to add 5ml 10mg/l methyl orange aqueous solution as blank；By 5 test tubes, magnetic force stirs in the dark
Mix 0.5 hour, be then placed in the photoreaction instrument with 500w mercury lamp (dominant wavelength λ=365nm) as light source and carry out photoreaction,
Carry out magnetic agitation, setting rotating speed is 400 revs/min in course of reaction, interval sampling in 10 minutes, take on a certain amount of after standing
Clear liquid, measures its absorbance with ultraviolet spectrophotometer, respectively further according to extinction before and after illumination at absorbing wavelength λ=465nm
The change of degree, calculates the degradation rate of methyl orange.Result is shown in Figure 17.
As seen from Figure 17, it is combined using the ag-agcl- poly- n-methylolacrylamide microgel photocatalysis of embodiment 3 preparation
Material degradation methyl orange 10 minutes, the degradation rate of methyl orange has reached 100%；The poly- hydroxyl of ag-agcl- using embodiment 1 preparation
After 30 minutes, all degraded completes methyl orange Methacrylamide microgel optic catalytic composite material degraded methyl orange, degradation rate
Reach 100%；Ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material degraded first using embodiment 2 preparation
After 50 minutes, methyl orange degradation rate reaches 54% to base orange；And blank control group and the degraded of ag- poly- n-methylolacrylamide microgel
Methyl orange 50 minutes, methyl orange is substantially undegraded.The ag-agcl- poly- n-methylolacrylamide microgel that the present invention obtains is described
Optic catalytic composite material has good photocatalysis effect, and ag- poly- n-methylolacrylamide microgel does not have photocatalytic.
Claims (7)
1. a kind of poly- n-methylolacrylamide microgel optic catalytic composite material of ag-agcl- preparation method it is characterised in that it
It is made up of following step:
(1) prepare poly- n-methylolacrylamide microgel
Using reversed emulsion polymerization, with n, n '-methylene-bisacrylamide is cross-linking agent, Ammonium persulfate. is initiator, tetramethyl
Base ethylenediamine be accelerator, span-80 and tween 80 mass ratio be 8～15:1 mixed liquor be surfactant, hexamethylene
For oil phase solvent, under inert gas shielding, n-methylolacrylamide polymerized at normal temperature is reacted 3～7 hours, is prepared into poly- hydroxyl first
Base acrylamide microgel；
(2) prepare ag- poly- n-methylolacrylamide microgel composite
Poly- n-methylolacrylamide microgel is dispersed in ethylene glycol, adds freshly prepared silver ammino solution, room temperature stirs
Mix 30 minutes, add naoh aqueous solution, stirring added naoh aqueous solution after 1 hour, poly- n-methylolacrylamide microgel
Quality is 1:2.5～3.2:0.5～0.8 with the ratio of the gross mass of the initial mass of silver nitrate, naoh in silver ammino solution, and room temperature is anti-
Answer 15～20 hours, be prepared into ag- poly- n-methylolacrylamide microgel composite；
(3) synthesize ag-agcl- poly- n-methylolacrylamide microgel optic catalytic composite material
Poly- for ag- n-methylolacrylamide microgel composite is added to ccl4In the mixed solution of isopropanol, the poly- hydroxyl of ag-
Methacrylamide microgel composite and ccl4Quality-volume ratio be 1g:7～20ml, ccl4Volume ratio with isopropanol
For 0.04～0.10:1, room temperature oscillating reactionss 8～15 hours, obtain ag-agcl- poly- n-methylolacrylamide microgel photocatalysis
Composite.
2. the preparation side of the poly- n-methylolacrylamide microgel optic catalytic composite material of ag-agcl- according to claim 1
Method it is characterised in that: in described step (1), n-methylolacrylamide, n, n '-methylene-bisacrylamide, Ammonium persulfate.,
The mass ratio of tetramethylethylenediamine is 1:(0.035～0.045): (0.08～0.12): (0.035～0.045).
3. the preparation side of the poly- n-methylolacrylamide microgel optic catalytic composite material of ag-agcl- according to claim 1
Method it is characterised in that: in described step (1), n-methylolacrylamide, n, n '-methylene-bisacrylamide, Ammonium persulfate.,
The mass ratio of tetramethylethylenediamine is 1:0.04:0.09:0.04.
4. the preparation side of the poly- n-methylolacrylamide microgel optic catalytic composite material of ag-agcl- according to claim 1
Method it is characterised in that: in described step (2), silver nitrate in the quality of poly- n-methylolacrylamide microgel and silver ammino solution
Initial mass, the gross mass of naoh ratio be 1:3:0.6.
5. the preparation side of the poly- n-methylolacrylamide microgel optic catalytic composite material of ag-agcl- according to claim 1
Method it is characterised in that: in described step (2), the volume of the second naoh aqueous solution adding is the naoh adding for the first time
2 times of aqueous solution volume.
6. the preparation side of the poly- n-methylolacrylamide microgel optic catalytic composite material of ag-agcl- according to claim 1
Method it is characterised in that: in described step (3), ag- poly- n-methylolacrylamide microgel composite and ccl4Quality-
Volume ratio is 1g:13ml.
7. the ag-agcl- poly- n-methylolacrylamide microgel photocatalysis of claim 1～6 any one method preparation are combined
Material.
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| KR100884018B1 (en) * | 2006-10-02 | 2009-02-17 | 창성엔지니어링 주식회사 | HIGH PHOTOCATALYTIC ACITIVITY OF MESOPOROUS TiO2 AND VISIBLE LINGT PHOTOCATALYST WITH HYDROTHERAMAL TREATMENT AND METHODE OF MANUFACTURING THEREOF |
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| CN100586552C (en) * | 2007-06-29 | 2010-02-03 | 江南大学 | Composite material of Nano grains of silver and carriers of polymer microballons, and preparation method thereof |
| CN102125816B (en) * | 2011-01-25 | 2013-01-09 | 运城学院 | Vapor phase reduction method for preparing organic-inorganic composite microsphere carrying silver nanoparticles on surface |
| CN103464203B (en) * | 2013-08-26 | 2015-06-17 | 陕西师范大学 | Preparation method of thermosensitive microgel asymmetric supported nano silver catalyst |
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| KR100884018B1 (en) * | 2006-10-02 | 2009-02-17 | 창성엔지니어링 주식회사 | HIGH PHOTOCATALYTIC ACITIVITY OF MESOPOROUS TiO2 AND VISIBLE LINGT PHOTOCATALYST WITH HYDROTHERAMAL TREATMENT AND METHODE OF MANUFACTURING THEREOF |
| CN101658485A (en) * | 2009-09-10 | 2010-03-03 | 东华大学 | Nanometer hybridized hydrogel with durable broad spectrum antibacterial performance and preparation method thereof |
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