CN105597778A - Strontium ferrite-loaded nano silver composite material and preparing method thereof - Google Patents
Strontium ferrite-loaded nano silver composite material and preparing method thereof Download PDFInfo
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- CN105597778A CN105597778A CN201510787171.8A CN201510787171A CN105597778A CN 105597778 A CN105597778 A CN 105597778A CN 201510787171 A CN201510787171 A CN 201510787171A CN 105597778 A CN105597778 A CN 105597778A
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- strontium ferrite
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Abstract
The invention discloses a strontium ferrite-loaded nano silver composite material and a preparing method thereof. The composite material is formed by compounding a strontium ferrite carrier and nano silver particles, and the surface of strontium ferrite is coated with the nano silver particles by a catalytic reduction technology. The prepared composite material has the diameter of 0.5-3 [mu]m, the diameter of the coated silver particles is 5-30 nm, and the diameter and the coating quantity of the silver nanoparticles can be controlled. Because the strontium ferrite carrier in the composite material belongs to a permanent magnet, the composite material has the advantages of high coercivity, large saturation magnetization intensity, good stability and the like, and is conducive to recovery and recycling of a strontium ferrite-loaded nano silver composite catalyst. The prepared composite catalyst has excellent catalytic performance, is easy to recover and reuse, has the advantage of environmental protection, and can be applied to degradation of organic pollutants of industrial and domestic sewage.
Description
Technical field
The invention belongs to Nano-composite materials technical field, be specifically related to a kind of preparation method of strontium ferrite loaded with nano silver composite material.
Background technology
Because the discharge capacity of industrial wastewater is large, pollutant kind is many, and in waste water, contains the organic matter of a large amount of hard degradations, makes traditional water treatment technology particularly all helpless containing poorly soluble organic waste water to containing a large amount of organic pollutions. In recent years, catalytic oxidation technology especially with semi-conducting material as TiO2For becoming water, the photocatalysis oxidation technique of catalyst pollutes the study hotspot of processing, but it needs the irradiation of ultraviolet light to excite in actual applications, because the ratio of sunshine middle-ultraviolet lamp is only less than 5%, therefore its reaction efficiency has much room for improvement, and equipment needed thereby cost is high. In addition, numerous catalyst for sewage disposal are difficult to reclaim, and to environment, are unfavorable for recycling of catalyst simultaneously, cause the wasting of resources.
The present invention has announced a kind of nano-strontium ferrite loaded with nano silver composite material, this material has good catalytic performance, under non-photocatalysis, get final product the organic matter in effective degradation of sewage, and in carrier, contain promoter elements strontium, effectively improved activity and the stability of catalyst. Meanwhile, strontium ferrite belongs to permanent magnet, has excellent magnetic property, is conducive to effective recovery of catalyst and recycles.
Summary of the invention
The object of the present invention is to provide a kind of strontium ferrite loaded with nano silver composite material and preparation method thereof, catalytic efficiency and recycling performance when improving it as catalyst.
In order to solve above technical problem, the concrete technical scheme that the present invention adopts is as follows:
A preparation method for strontium ferrite loaded with nano silver composite material, is characterized in that comprising the following steps:
Step 1, the silver salt solution of configuration 0.05~1mol/L, to the NaOH solution that adds 0.5~2mol/L in described silver salt solution, produces that to add mass fraction after pitchy precipitation be 10%~15% ammoniacal liquor again, is stirred to precipitation and disappears, and obtains silver ammino solution;
Step 2, getting strontium ferrite powder joins in described silver ammino solution, strontium ferrite and simple substance silver mass ratio are 20~100:1, after ultrasonic processing 1h, adding mass fraction is the organic binder bond ethanolic solution of 1.0%-1.4%, organic binder bond ethanolic solution and silver ammino solution volume ratio are 1:1, obtain solution A after ultrasonic 10-30min;
Step 3, the strong reductant solution of configuration 0.05~0.1mol/L, dropwise joins in described solution A, and strong reductant and silver particles mol ratio are 2 ~ 4:1, under heating condition, stir, and obtain suspension;
Step 4, carries out centrifugal, separating treatment by described suspension, and gained precipitation is respectively washed three times with distilled water, absolute ethyl alcohol, obtains strontium ferrite loaded with nano silver composite material after oven dry.
In described step 1, silver salt is water-soluble silver-colored compound as any one or more mixture in silver nitrate, silver fluoride.
In described step 2, organic binder bond is the mixture of any or the two in PVAC polyvinylalcohol and polyvinylpyrrolidone PVP.
In described step 3, strong reductant is any one or two kinds of mixture in sodium borohydride, hydrazine hydrate.
In described step 3, heating condition is 30 DEG C-60 DEG C, in order to prevent that strontium ferrite composite is adsorbed, stirs as mechanical agitation, and mixing time is 2-4 hour.
In described step 4, bake out temperature is 45 DEG C ~ 80 DEG C.
A kind of strontium ferrite loaded with nano silver composite material, it is characterized in that: described strontium ferrite loaded with nano silver composite material is to be composited by strontium ferrite particle and nano silver particles, nano silver particles is coated on the surface of strontium ferrite, composite particle size is 0.5-3 μ m, and silver particles diameter is 5-30nm.
The present invention has beneficial effect.The present invention is by adopting catalytic reduction method to prepare strontium ferrite loaded with nano silver composite material, this technology of preparing can effectively be controlled diameter, the shape of nano silver particles, and the load capacity of nano silver particles, thereby can Effective Regulation catalyst for catalytic performance and the recovering effect of the organic pollution of degrading waste water. And strontium ferrite supported nano-silver catalyst of the present invention is by producing active oxygen catalytic degradation organic matter, does not need ultraviolet source and thermal source, operating cost is cheap.
Brief description of the drawings
Fig. 1 is the XRD figure of the strontium ferrite loading nano silvery composite catalyst prepared of embodiment 1;
Fig. 2 is the SEM figure of the strontium ferrite loading nano silvery composite catalyst prepared of embodiment 1;
Fig. 3 is the catalysis curve map of the catalytic degradation methyl blue of the strontium ferrite loading nano silvery composite catalyst prepared of embodiment 4.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is described in further details.
Embodiment 1
(1) get the liquor argenti nitratis ophthalmicus that 10ml concentration is 0.05mol/L, adding 2ml concentration is 0.5mol/LNaOH solution, produces that to add 1ml mass fraction after pitchy precipitation be 10% ammoniacal liquor again, is stirred to precipitation and disappears, and obtains silver ammino solution;
(2) get 0.3g strontium ferrite and join in described silver ammino solution, after ultrasonic 1h, adding 13ml mass fraction is 1.0% PVP solution, and ultrasonic 10min, obtains solution A; The hydrazine hydrate solution that is 0.05mol/L by 47ml concentration, dropwise joins A solution, mechanical agitation 2h, and reaction, obtains suspension at 30 DEG C;
(3) by described suspension centrifugation, and respectively wash three times with distilled water, absolute ethyl alcohol, 45 DEG C of oven dry, obtain diameter at 2.50 ± 0.5 μ m, and the diameter of silver particles is 10 ± 0.05nm, finely dispersed strontium ferrite supported nano-silver catalyst. As shown in Figure 1, SEM as shown in Figure 2 for the XRD of gained sample.
Embodiment 2
(1) get the liquor argenti nitratis ophthalmicus that 8ml concentration is 1mol/L, adding 1.5ml concentration is 2mol/LNaOH solution, produces that to add 1ml mass fraction after pitchy precipitation be 15% ammoniacal liquor again, is stirred to precipitation and disappears, and obtains silver ammino solution;
(2) get 0.3g strontium ferrite and join in described silver ammino solution, after ultrasonic 1h, adding 10ml mass fraction is 1.4% PVP solution, and ultrasonic 30min, obtains solution A; The hydrazine hydrate solution that is 0.1mol/L by 40ml concentration, dropwise joins A solution, mechanical agitation 2h, and reaction, obtains suspension at 60 DEG C;
(3) by described suspension centrifugation, and respectively wash three times with distilled water, absolute ethyl alcohol, 50 DEG C of oven dry, obtain diameter at 1.50 ± 0.5 μ m, and the diameter of silver particles is 20 ± 0.05nm, finely dispersed strontium ferrite supported nano-silver catalyst.
Embodiment 3
(1) get silver nitrate and the silver fluoride solution that 10ml concentration is 0.75mol/L, adding 1.0ml concentration is 1.0mol/LNaOH solution, produces that to add 1ml mass fraction after pitchy precipitation be 12% ammoniacal liquor again, is stirred to precipitation and disappears, and obtains silver ammino solution;
(2) get 0.4g strontium ferrite and join in described silver ammino solution, after ultrasonic 1h, adding 12ml mass fraction is 1.2% PVP solution, and ultrasonic 20min, obtains solution A; The hydrazine hydrate solution that is 0.075mol/L by 40ml concentration, dropwise joins A solution, mechanical agitation 2h, and reaction, obtains suspension at 45 DEG C;
(3) by described suspension centrifugation, and respectively wash three times with distilled water, absolute ethyl alcohol, 65 DEG C of oven dry, obtain diameter at 2.0 ± 0.5 μ m, and the diameter of silver particles is 15 ± 0.05nm, finely dispersed strontium ferrite supported nano-silver catalyst.
Embodiment 4
(1) get the liquor argenti nitratis ophthalmicus that 10ml concentration is 0.5mol/L, adding 2ml concentration is 1.25mol/LNaOH solution, produces that to add 1ml mass fraction after pitchy precipitation be 12.5% ammoniacal liquor again, is stirred to precipitation and disappears, and obtains silver ammino solution;
(2) get 0.3g strontium ferrite and join in described silver ammino solution, after ultrasonic 1h, adding 10ml mass fraction is 1.4% PVP solution, and ultrasonic 30min, obtains solution A; The hydrazine hydrate solution that is 0.075mol/L by 45ml concentration, dropwise joins A solution, mechanical agitation 4h, and reaction, obtains suspension at 50 DEG C;
(3) by described suspension centrifugation, and respectively wash three times with distilled water, absolute ethyl alcohol, 80 DEG C of oven dry, obtain diameter at 1.50 ± 0.5 μ m, the diameter of silver particles is 5 ± 0.05nm, finely dispersed strontium ferrite supported nano-silver catalyst, the ultraviolet spectra curve of its oxidation catalysis degraded methyl blue as shown in Figure 3.
Claims (7)
1. a preparation method for strontium ferrite loaded with nano silver composite material, is characterized in that comprising the following steps:
Step 1, the silver salt solution of configuration 0.05~1mol/L, to the NaOH solution that adds 0.5~2mol/L in described silver salt solution, produces that to add mass fraction after pitchy precipitation be 10%~15% ammoniacal liquor again, is stirred to precipitation and disappears, and obtains silver ammino solution;
Step 2, getting strontium ferrite powder joins in described silver ammino solution, strontium ferrite and simple substance silver mass ratio are 20~100:1, after ultrasonic processing 1h, adding mass fraction is the organic binder bond ethanolic solution of 1.0%-1.4%, organic binder bond ethanolic solution and silver ammino solution volume ratio are 1:1, obtain solution A after ultrasonic 10-30min;
Step 3, the strong reductant solution of configuration 0.05~0.1mol/L, dropwise joins in described solution A, and strong reductant and silver particles mol ratio are 2 ~ 4:1, under heating condition, stir, and obtain suspension;
Step 4, carries out centrifugal, separating treatment by described suspension, and gained precipitation is respectively washed three times with distilled water, absolute ethyl alcohol, obtains strontium ferrite loaded with nano silver composite material after oven dry.
2. the preparation method of a kind of strontium ferrite loaded with nano silver composite material according to claim 1, is characterized in that: in described step 1, silver salt is water-soluble silver-colored compound as any one or more mixture in silver nitrate, silver fluoride.
3. the preparation method of a kind of strontium ferrite loaded with nano silver composite material according to claim 1, is characterized in that: in described step 2, organic binder bond is the mixture of any or the two in PVAC polyvinylalcohol and polyvinylpyrrolidone PVP.
4. the preparation method of a kind of strontium ferrite loaded with nano silver composite material according to claim 1, is characterized in that: in described step 3, strong reductant is any one or two kinds of mixture in sodium borohydride, hydrazine hydrate.
5. the preparation method of a kind of strontium ferrite loaded with nano silver composite material according to claim 1, it is characterized in that: in described step 3, heating condition is 30 DEG C-60 DEG C, in order to prevent that strontium ferrite composite is adsorbed, stir as mechanical agitation, mixing time is 2-4 hour.
6. the preparation method of a kind of strontium ferrite loaded with nano silver composite material according to claim 1, is characterized in that: in described step 4, bake out temperature is 45 DEG C ~ 80 DEG C.
7. the ferrite loaded with nano silver composite material that utilizes the preparation method of a kind of strontium ferrite loaded with nano silver composite material described in claim 1 to prepare, it is characterized in that: described strontium ferrite loaded with nano silver composite material is to be composited by strontium ferrite particle and nano silver particles, nano silver particles is coated on the surface of strontium ferrite, composite particle size is 0.5-3 μ m, and silver particles diameter is 5-30nm.
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CN114799160A (en) * | 2021-01-27 | 2022-07-29 | 中国科学院理化技术研究所 | Method for modifying surface of magnetic particle |
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CN1557588A (en) * | 2004-01-13 | 2004-12-29 | 上海大学 | Method for manufacturing nano-silver |
CN102364616A (en) * | 2011-09-22 | 2012-02-29 | 华南师范大学 | Nanometer composite material Fe3O4@PS@Ag with core-shell structure and preparation method thereof |
CN102664085A (en) * | 2012-05-22 | 2012-09-12 | 中北大学 | Flower-like Fe2O3/Ag composite particle and preparation method thereof |
CN103480384A (en) * | 2013-09-18 | 2014-01-01 | 重庆大学 | Preparation method for bismuth vanadate composite photocatalyst loaded with strontium ferrite |
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Patent Citations (4)
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CN1557588A (en) * | 2004-01-13 | 2004-12-29 | 上海大学 | Method for manufacturing nano-silver |
CN102364616A (en) * | 2011-09-22 | 2012-02-29 | 华南师范大学 | Nanometer composite material Fe3O4@PS@Ag with core-shell structure and preparation method thereof |
CN102664085A (en) * | 2012-05-22 | 2012-09-12 | 中北大学 | Flower-like Fe2O3/Ag composite particle and preparation method thereof |
CN103480384A (en) * | 2013-09-18 | 2014-01-01 | 重庆大学 | Preparation method for bismuth vanadate composite photocatalyst loaded with strontium ferrite |
Non-Patent Citations (2)
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ZHENG HE ET AL.: ""Preparation and microwave-absorbing properties of silver-coated strontium ferrite with polyaniline via in situ polymerization"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114799160A (en) * | 2021-01-27 | 2022-07-29 | 中国科学院理化技术研究所 | Method for modifying surface of magnetic particle |
CN114799160B (en) * | 2021-01-27 | 2024-03-26 | 中国科学院理化技术研究所 | Method for modifying surface of magnetic particle |
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