CN102626658A - Ferrate/polyaniline magnetic nanometer catalytic agent and preparation method thereof - Google Patents
Ferrate/polyaniline magnetic nanometer catalytic agent and preparation method thereof Download PDFInfo
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Abstract
The invention adopts an in-situ oxidation polymerization method and enables the polyaniline to be wrapped on the surface of the magnetic ferrate, and a series of ferrate/polyaniline magnetic nano composite materials can be prepared by using the method and comprise cobalt ferrite/polyaniline, nickel ferrite/polyaniline, copper ferrite/polyaniline, zinc ferrite/polyaniline and manganese ferrite/polyaniline and the like. A prepared ferrate/polyaniline magnetic nanometer catalytic agent has obvious preferential adsorption performance and good photoelectrical activity, and has good application prospects and economic benefits in the fields of adsorption, photocatalysis, lithium ion batteries and the like.
Description
Technical field
The present invention relates to a kind of Catalysts and its preparation method, particularly a kind of ferrite/polyaniline magnetic nano-catalyst and preparation method thereof belongs to the materials chemistry field.
Background technology
Aspect dye wastewater treatment, method relatively more commonly used has absorption, approach such as photocatalytic degradation and biodegradation at present.Wherein absorption is because characteristics easy and simple to handle have obtained general application.Adsorbent commonly used at present mainly comprises active carbon, biomaterial, flyash etc.Yet more than numerous adsorbents characteristics of all not having the excellent selectivity absorption property and can be recycled.Recently people such as Debajyoti Mahanta find the to mix polyaniline of attitude has the performance of selective absorption, can selective absorption anionic dye [D. Mahanta et al. J. Phys. Chem. B 2008,112,10153-10157.].Select the magnetic adsorbent of row absorption property but seldom to be in the news yet have.
The photocatalytic degradation technology more and more receives people's attention because it efficiently reaches great application prospect.Polyaniline is used widely in photocatalysis field owing to special band structure in recent years.The Nano semiconductor composite that some polyanilines are modified is like TiO
2/ PANI, ZnO/PANI, CdS/PANI etc. all are produced out.Though yet these photochemical catalysts have certain photocatalytic activity, recovery and recycle aspect after being to use are not well solved.
Ferrites such as nano-ferrous acid, nickel ferrite based magnetic loaded, coppe ferrite, zinc ferrite and ferrous acid manganese all are a kind of magnetic Nano ferrites with spinel structure.They have high electric property, high Curie temperature and excellent stability, have applied to fields such as information storage, electricity device and pharmaceutical carrier widely.For example, the band gap of nickel ferrite based magnetic loaded is narrow, has only 2.19 eV; Be considered to a kind of desirable photochemical catalyst; But, in the preparation process, reunite easily, thereby reduced its surface-active because independent nano nickel ferrite specific grain surface is bigger; Make light induced electron can not effectively separate, limited its photocatalytic activity with the hole.People such as Sun prepare monodispersed cobalt ferrite and manganous ferrite nano-particle; Its preparation method need add a large amount of surfactants; Reaction temperature is higher, and process is relatively complicated, and does not make further about the performance of these ferrites and to probe into [S. H. Sun et al. J. Am. Chem. Soc. 2004; 126,273-279.].Research according to above shows; Polyaniline is modified the ferrite surface; Can be uniformly dispersed; Stable ferrite/polyaniline magnetic nano-catalyst, this material have significant selective absorption performance and good photoelectric activity, have application promise in clinical practice and economic benefit in fields such as absorption, photocatalysis and lithium ion batteries.
Summary of the invention
The object of the invention does not have the selective absorption performance to existing catalyst; Do not have magnetic; Can not easy recycle and reuse etc. problem, a kind of have significant selective absorption performance and good photocatalytic activity ferrite/polyaniline magnetic nano-catalyst and preparation method thereof are provided.
The technical solution that realizes the object of the invention is: ferrite/polyaniline magnetic nano-catalyst is got by the following steps preparation:
The first step is with trivalent iron salt and divalent transition metal inorganic salts stirring and dissolving in ethanol;
In second step, alkali is joined in the solution of the first step gained stirring and dissolving;
The 3rd step, after the mixed solution reaction with second step, centrifugation, dry back obtains nano ferrite;
In the 4th step, the nano ferrite that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the acid solution;
The 5th step joined aniline in the system of the 4th step gained again, and isolated by filtration, dry back obtain ferrite/polyaniline magnetic Nano material after reacting.
Trivalent iron salt described in the step 1 is ferric nitrate, iron chloride or ferric sulfate, and divalent transition metal salt is cobalt salt, nickel salt, mantoquita, zinc salt or manganese salt, and described mixing time is 10-90 min, and the mol ratio of trivalent iron salt and divalent transition metal salt is 2:1.
The mol ratio of alkali described in the step 2 and described divalent transition metal salt is (0 ~ 80): 1, and mixing time is 10-60 min, described alkali is NaOH, ammoniacal liquor or urea.
Reaction temperature described in the step 3 is 120-260 ℃, and the reaction time is 12-24 h.
The concentration of the acid solution described in the step 4 is 0.5 ~ 5 mol/L, and described acid is hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, p-methyl benzenesulfonic acid or citric acid.
Temperature described in the step 5 is 0 ~ 50 ℃, reaction time 6 ~ 24 h, and the mol ratio of described aniline and described ammonium persulfate is 0.1 ~ 10.
The content of polyaniline is 5-90 wt% in described ferrite/polyaniline magnetic nano-catalyst, and the content of ferrite is 10-95%.
Ferrite of the present invention/polyaniline magnetic nano-catalyst, preparation method and the application aspect the dyestuff processing thereof; Compared with prior art; Its advantage is: ferrite/polyaniline nano-composite material that (1) the present invention prepares has magnetic, can reclaim easily and recycle; (2) the present invention adopts the method for in-situ oxidizing-polymerizing reaction can prepare ferrite/polyaniline magnetic nano-catalyst that a series of different acid is mixed; (3) ferrite/polyaniline magnetic nano-catalyst of preparing of the present invention has excellent selectivity absorption property and visible light catalysis activity; (4) ferrite/polyaniline magnetic nano-catalyst of the present invention's preparation has excellent absorption property to anionic dye, under visible light, some waste water from dyestuff is had good photocatalysis effect.
Description of drawings
Fig. 1 is the XRD figure spectrum (a is that polyaniline, b are cobalt ferrite/polyaniline magnetic catalyst, and c is a cobalt ferrite) of instance 1 gained cobalt ferrite of the present invention/polyaniline magnetic catalyst.
The specific embodiment
Ferrite/polyaniline magnetic nano-catalyst is got by the following steps preparation:
The first step is that trivalent iron salt ferric nitrate, iron chloride or ferric sulfate and divalent transition metal salt cobalt nitrate, cobalt chloride, cobaltous sulfate, nickel nitrate, nickel chloride, nickelous sulfate, copper nitrate, copper chloride, copper sulphate, zinc nitrate, zinc chloride, zinc sulfate, manganese nitrate, manganese chloride or the manganese sulfate of 2:1 stirs 10-90 min in ethanol with mol ratio;
In second step, will be (0 ~ 80) with the mol ratio of the divalent transition metal salt that added in the step 1: 1 NaOH, ammoniacal liquor or urea join in the solution of first step gained, stir 10-60 min;
The 3rd step, with the mixed solution in second step after reacting 12-24 h under 120-260 ℃, centrifugation, dry back obtains nano ferrite;
In the 4th step, the nano ferrite that ammonium persulfate and the 3rd is gone on foot gained is dispersed in hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, p-methyl benzenesulfonic acid or the citric acid solution that concentration is 0.5 ~ 5 mol/L;
The 5th step; To be that 0.1 ~ 10 aniline joins in the system of the 5th step gained again with the mol ratio of the ammonium persulfate that added in the 4th step; Be to react 6 ~ 24 h under 0 ~ 50 ℃ the condition in temperature; Isolated by filtration, dry back obtain ferrite/polyaniline magnetic Nano material afterwards, and wherein, the content of polyaniline is 5-90wt%.
Embodiment 1:Cobalt ferrite/polyaniline magnetic nano-catalyst, polyaniline content is the preparation method of 5wt%, may further comprise the steps:
The first step is that ferric nitrate and the cobalt nitrate of 2:1 stirs 90min in ethanol with mol ratio;
Second step will be that the NaOH of 80:1 joins in the solution of first step gained with the mol ratio of the cobalt nitrate that added in the step 1, stir 60min;
The 3rd step, with the mixed solution in second step at 120 ℃ down behind the reaction 12h, centrifugation, dry back obtains nano-ferrous acid;
In the 4th step, the nano-ferrous acid that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the hydrochloric acid solution that concentration is 0.5mol/L;
The 5th step; To be that 0.1 aniline joins in the system of the 5th step gained again with the mol ratio of the ammonium persulfate that added in the 4th step; Be to react 24 h under 0 ℃ the condition in temperature; Isolated by filtration, dry back obtain cobalt ferrite/polyaniline magnetic Nano material afterwards, and wherein the content of polyaniline is 5wt%, and cobalt ferrite content is 95%.
As shown in Figure 1, be the XRD figure spectrum of polyaniline (a), cobalt ferrite/polyaniline magnetic Nano material (b) and cobalt ferrite (c).
Embodiment 2:Nickel ferrite based magnetic loaded/polyaniline magnetic nano-catalyst, polyaniline content is the preparation method of 90wt%, may further comprise the steps:
The first step is that ferric nitrate and the nickel chloride of 2:1 stirs 10min in ethanol with mol ratio;
Second step will be that the ammoniacal liquor of 60:1 joins in the solution of first step gained with the mol ratio of the divalent transition metal salt that added in the step 1, stir 10min;
The 3rd step, with the mixed solution in second step after reacting 24 h under 140 ℃, centrifugation, dry back obtains nano nickel ferrite;
In the 4th step, the nano nickel ferrite that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the sulfuric acid solution that concentration is 1mol/L;
The 5th step; To be that 10 aniline joins in the system of the 5th step gained again with the mol ratio of the ammonium persulfate that added in the 4th step; Be to react 6h under 50 ℃ the condition in temperature; Isolated by filtration, dry back obtain nickel ferrite based magnetic loaded/polyaniline magnetic Nano material afterwards, and wherein the content of polyaniline is 90 wt%, and nickel ferrite based magnetic loaded content is 10%.
Embodiment 3:Coppe ferrite/polyaniline magnetic nano-catalyst, polyaniline content is the preparation method of 10wt%, may further comprise the steps:
The first step is that ferric nitrate and the copper sulphate of 2:1 stirs 30 min in ethanol with mol ratio;
Second step will be that the urea of 40:1 joins in the solution of first step gained with the mol ratio of the divalent transition metal salt that added in the step 1, stir 25 min;
The 3rd step, with the mixed solution in second step after reacting 20h under 160 ℃, centrifugation, dry back obtains nano ferrous acid copper;
In the 4th step, the nano ferrous acid copper that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the phosphoric acid solution that concentration is 2mol/L;
The 5th step; To be that 1 aniline joins in the system of the 5th step gained again with the mol ratio of the ammonium persulfate that added in the 4th step; Be to react 20h under 5 ℃ the condition in temperature; Isolated by filtration, dry back obtain coppe ferrite/polyaniline magnetic Nano material afterwards, and wherein the content of polyaniline is 10 wt%, and coppe ferrite content is 90%.
Embodiment 4:Zinc ferrite/polyaniline magnetic nano-catalyst, polyaniline content is the preparation method of 30wt%, may further comprise the steps:
The first step is that iron chloride and the zinc chloride of 2:1 stirs 60 min in ethanol with mol ratio;
Second step will be that the NaOH of 20:1 joins in the solution of first step gained with the mol ratio of the divalent transition metal salt that added in the step 1, stir 35min;
The 3rd step, with the mixed solution in second step after reacting 18h under 180 ℃, centrifugation, dry back obtains nanometer zinc ferrite;
In the 4th step, the nanometer zinc ferrite that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the salpeter solution that concentration is 3mol/L;
The 5th step; To be that 3 aniline joins in the system of the 5th step gained again with the mol ratio of the ammonium persulfate that added in the 4th step; Be to react 16h under 10 ℃ the condition in temperature; Isolated by filtration, dry back obtain zinc ferrite/polyaniline magnetic Nano material afterwards, and wherein the content of polyaniline is 30 wt%, and zinc ferrite content is 70%.
Embodiment 5:Ferrous acid manganese/polyaniline magnetic nano-catalyst, polyaniline content is the preparation method of 50wt%, may further comprise the steps:
The first step is that iron chloride and the manganese sulfate of 2:1 stirs 80 min in ethanol with mol ratio;
Second step will be that the ammoniacal liquor of 10:1 joins in the solution of first step gained with the mol ratio of the divalent transition metal salt that added in the step 1, stir 45min;
The 3rd step, with the mixed solution in second step after reacting 16h under 200 ℃, centrifugation, dry back obtains nanometer ferrous acid manganese;
In the 4th step, the nanometer ferrous acid manganese that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the p-methyl benzenesulfonic acid solution that concentration is 5mol/L;
The 5th step; To be that 5 aniline joins in the system of the 5th step gained again with the mol ratio of the ammonium persulfate that added in the 4th step; Be to react 14h under 30 ℃ the condition in temperature; Isolated by filtration, dry back obtain ferrous acid manganese/polyaniline magnetic Nano material afterwards, and wherein the content of polyaniline is 50 wt%, and the content of ferrous acid manganese is 50%.
Embodiment 6:Cobalt ferrite/polyaniline magnetic nano-catalyst, polyaniline content is the preparation method of 70wt%, may further comprise the steps:
The first step is that ferric sulfate and the cobaltous sulfate of 2:1 stirs 90min in ethanol with mol ratio;
Second step will be that the NaOH of 50:1 joins in the solution of first step gained with the mol ratio of the cobalt nitrate that added in the step 1, stir 60min;
The 3rd step, with the mixed solution in second step at 200 ℃ down behind the reaction 12h, centrifugation, dry back obtains nano-ferrous acid;
In the 4th step, the nano-ferrous acid that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the hydrochloric acid solution that concentration is 4mol/L;
The 5th step; To be that 7 aniline joins in the system of the 5th step gained again with the mol ratio of the ammonium persulfate that added in the 4th step; Be to react 15 h under 15 ℃ the condition in temperature; Isolated by filtration, dry back obtain cobalt ferrite/polyaniline magnetic Nano material afterwards, and wherein the content of polyaniline is 70wt%, and cobalt ferrite content is 30%.
Claims (5)
1. ferrite/polyaniline magnetic nano-catalyst, the content that it is characterized in that polyaniline in the said catalyst is 5-90 wt%, the content of ferrite is 10-95%.
2. ferrite according to claim 1/polyaniline magnetic nano-catalyst is characterized in that said catalyst is prepared by following steps:
The first step is with trivalent iron salt and divalent transition metal inorganic salts stirring and dissolving in ethanol;
In second step, alkali is joined in the solution of the first step gained stirring and dissolving;
The 3rd step, after the mixed solution reaction with second step, centrifugation, dry back obtains nano ferrite;
In the 4th step, the nano ferrite that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the acid solution;
The 5th step joined aniline in the system of the 4th step gained again, and isolated by filtration, dry back obtain ferrite/polyaniline magnetic Nano material after reacting.
3. ferrite according to claim 1 and 2/polyaniline magnetic nano-catalyst; It is characterized in that the trivalent iron salt described in the step 1 is ferric nitrate, iron chloride or ferric sulfate; The divalent transition metal inorganic salts are cobalt salt, nickel salt, mantoquita, zinc salt or manganese salt; Described mixing time is 10-90 min, and the mol ratio of trivalent iron salt and divalent transition metal salt is 2:1;
The mol ratio of alkali described in the step 2 and described divalent transition metal salt is (0 ~ 80): 1, and mixing time is 10-60 min, described alkali is NaOH, ammoniacal liquor or urea;
Reaction temperature described in the step 3 is 120-260 ℃, and the reaction time is 12-24 h;
The concentration of the acid solution described in the step 4 is 0.5 ~ 5 mol/L, and described acid is hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, p-methyl benzenesulfonic acid or citric acid;
Temperature described in the step 5 is 0 ~ 50 ℃, reaction time 6 ~ 24 h, and the mol ratio of described aniline and described ammonium persulfate is 0.1 ~ 10.
4. the preparation method of ferrite/polyaniline magnetic nano-catalyst is characterized in that said method comprising the steps of:
The first step is with trivalent iron salt and divalent transition metal inorganic salts stirring and dissolving in ethanol;
In second step, alkali is joined in the solution of the first step gained stirring and dissolving;
The 3rd step, after the mixed solution reaction with second step, centrifugation, dry back obtains nano ferrite;
In the 4th step, the nano ferrite that ammonium persulfate and the 3rd is gone on foot gained is dispersed in the acid solution;
The 5th step joined aniline in the system of the 4th step gained again, and isolated by filtration, dry back obtain ferrite/polyaniline magnetic Nano material after reacting.
5. the preparation method of ferrite according to claim 4/polyaniline magnetic nano-catalyst; It is characterized in that the trivalent iron salt described in the step 1 is ferric nitrate, iron chloride or ferric sulfate; The divalent transition metal inorganic salts are cobalt salt, nickel salt, mantoquita, zinc salt or manganese salt; Described mixing time is 10-90 min, and the mol ratio of trivalent iron salt and divalent transition metal salt is 2:1;
The mol ratio of alkali described in the step 2 and described divalent transition metal salt is (0 ~ 80): 1, and mixing time is 10-60 min, described alkali is NaOH, ammoniacal liquor or urea;
Reaction temperature described in the step 3 is 120-260 ℃, and the reaction time is 12-24 h;
The concentration of the acid solution described in the step 4 is 0.5 ~ 5 mol/L, and described acid is hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, p-methyl benzenesulfonic acid or citric acid;
Temperature described in the step 5 is 0 ~ 50 ℃, reaction time 6 ~ 24 h, and the mol ratio of described aniline and described ammonium persulfate is 0.1 ~ 10.
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| CN103482706A (en) * | 2013-10-15 | 2014-01-01 | 大连交通大学 | Hollow spherical nano manganese ferrite, and preparation method and application thereof |
| CN103495727A (en) * | 2013-10-21 | 2014-01-08 | 黑龙江大学 | Core-shell nano-copper nickel solid solution/polyaniline composite materials and preparation method thereof |
| CN104437493A (en) * | 2014-12-05 | 2015-03-25 | 北京科技大学 | Method for preparing cathode composite catalyst of bioelectrochemical system |
| CN104743633A (en) * | 2015-04-16 | 2015-07-01 | 安徽工业大学 | Method for degrading organic waste water by photo-assisted activation of potassium hydrogen persulfate through bismuth ferrite |
| CN105161701A (en) * | 2015-09-23 | 2015-12-16 | 西北工业大学 | Preparing method for polyaniline/hollow ZnFe2O4 composite negative electrode materials of lithium battery |
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| CN103482706A (en) * | 2013-10-15 | 2014-01-01 | 大连交通大学 | Hollow spherical nano manganese ferrite, and preparation method and application thereof |
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| CN104437493A (en) * | 2014-12-05 | 2015-03-25 | 北京科技大学 | Method for preparing cathode composite catalyst of bioelectrochemical system |
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| CN108745308A (en) * | 2018-05-07 | 2018-11-06 | 江苏大学 | A kind of conductive traces Ag@PANI/CoFe2O4The preparation method and applications of/C |
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| CN109513460A (en) * | 2018-11-20 | 2019-03-26 | 扬州大学 | A kind of synthetic method of beta carotene degradation catalyst |
| CN109794293A (en) * | 2019-01-24 | 2019-05-24 | 杭州师范大学 | A kind of application of iron-based photochemical catalyst and its rhodamine B degradation |
| CN109794293B (en) * | 2019-01-24 | 2021-09-21 | 杭州师范大学 | Iron-based photocatalyst and application thereof in degrading rhodamine B |
| CN109926090A (en) * | 2019-03-13 | 2019-06-25 | 扬州大学 | A kind of catalyst and preparation method thereof for synthesizing Imatinib |
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