CN102553595A - Preparation method of nano ferrate/carbon nano tube composite materials - Google Patents
Preparation method of nano ferrate/carbon nano tube composite materials Download PDFInfo
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- CN102553595A CN102553595A CN2011104344508A CN201110434450A CN102553595A CN 102553595 A CN102553595 A CN 102553595A CN 2011104344508 A CN2011104344508 A CN 2011104344508A CN 201110434450 A CN201110434450 A CN 201110434450A CN 102553595 A CN102553595 A CN 102553595A
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Abstract
The invention discloses a preparation method of nano ferrate/carbon nano tube composite materials, which utilizes a carbon nano tube as a supporting material and adopts a method of solvothermal synthesis to prepare a series of nano ferrate/carbon nano tube composite materials which are even in dispersion, have magnetic property, include nano cobalt ferrite/carbon nano tubes, ferrous acid nickel/carbon nano tubes, ferrous acid copper/carbon nano tubes, zinc ferrite/carbon nano tubes, ferrous acid manganese/carbon nano tubes and the like, and have certain universality. Compared with the prior art, the preparation method of the nano ferrate/carbon nano tube composite materials utilizes ethanol as solvent. The prepared nano materials are uniform in grain size and excellent in performance and have good application prospect and economic benefits on aspects of photocatalysis sewage treatment, lithium ion batteries and the like.
Description
Technical field
The invention belongs to is being backing material with the CNT; Finely dispersed at its surface deposition; Magnetic Nano ferrite Composite Preparation technology, the method has certain versatility, utilizes the method can prepare a series of nano ferrite/carbon nano tube compound material; This nano ferrite/carbon nano tube compound material has the excellent photoelectric activity, has application promise in clinical practice and economic benefit at aspects such as photocatalysis sewage processing and lithium ion batteries.
Background technology
Ferrites such as nano-ferrous acid, nickel ferrite based magnetic loaded, coppe ferrite, zinc ferrite and ferrous acid manganese all are a kind of 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, and its preparation method need add a large amount of surfactants, and reaction temperature is higher; Process is relatively complicated, and does not make further about the performance of these ferrites and to probe into (S. H. Sun, H. Zeng; D. B. Robinson, S. Raoux, P. M. Rice; S. X. Wang, G. X. Li. Monodisperse MFe
2O
4(M=Fe, Co, Mn) Nanoparticles. J. Am. Chem. Soc. 2004,126,273-279).
Research according to present shows, can improve the photoelectric activity of ferrite effectively through the method for semiconductor doping.CNT is because its unique pore structure has applied to fields such as catalyst carrier, photoelectric material widely.Utilize CNT as carrier, ferrite is loaded to carbon nano tube surface, can be uniformly dispersed, stabilized nano ferrite/carbon nano tube compound material, this material has the excellent photoelectric activity.People such as Chen utilize hydro-thermal method only to prepare zinc ferrite/multi-walled carbon nano-tubes composite photo-catalyst; And its composite photo-catalyst of preparing methylene blue dye of under visible light, degrading need add hydrogen peroxide solution (C. H. Chen; Y. H. Liang, W. D. Zhang. ZnFe
2O
4/ MWCNTs composite with enhanced photocatalytic activity under visible-light irradiation. Journal of Alloys and Compounds. 2010,501,168-172).Up to the present preparation method about other nano ferrite/carbon nano tube compound materials but seldom is in the news.
Summary of the invention
The object of the present invention is to provide a kind of have certain versatility, can prepare a series of methods with the electroactive nano ferrite/carbon nano tube compound material of efficiency light.
The technical solution that realizes the object of the invention is: nano ferrite/carbon nano tube compound material is got by the following steps preparation:
The first step is carried out ultrasonic dispersion with CNT in red fuming nitric acid (RFNA);
Second step is with the further acidification in nitration mixture of the CNT in the first step;
The 3rd step is with the ultrasonic dispersion in ethanol of the CNT after the acidifying;
The 4th step is with ferric nitrate and nitrate stirring and dissolving in ethanol;
In the 5th step, the dispersion liquid and the 4th of the 3rd step gained is gone on foot gained solution mix and stir;
In the 6th step, the mixed liquor in the 5th step is transferred in the water heating kettle and reacts;
In the 7th step, the 6th step products therefrom centrifugation and washing, dry back are obtained nano ferrite/carbon nano tube compound material.
Ultrasonic jitter time described in the step 1 is 30-120 min.
Nitration mixture described in the step 2 is the concentrated sulfuric acid and red fuming nitric acid (RFNA), and volume ratio is 1:1, and described acidification temperature is 90-150 ℃, and the acidification time is 6-18 h.
Ultrasonic jitter time described in the step 3 is 60-180 min.
Mixing time described in the step 4 is 10-90 min, and described nitrate is nickel nitrate, cobalt nitrate, copper nitrate, zinc nitrate or manganese nitrate, and the mol ratio of described ferric nitrate and nitrate is 2:1.
Mixing time described in the step 5 is 30-120 min.
Reaction temperature described in the step 6 is 120-200 ℃, and the reaction time is 12-24 h.
Mass fraction 5 wt% ~ 35 wt% of the CNT in the step 7 in resulting nano ferrite/carbon nano tube compound material.
The preparation method of nano ferrite/carbon nano tube compound material of the present invention, compared with prior art, its advantage is: (1) the present invention adopts ethanol as solvent, the nano material uniform particle diameter of preparing, excellent performance; (2) the present invention adopts the method for two step acidification that CNT is carried out acidification; (3) preparation method of the present invention has certain versatility, adopts preparation method of the present invention can prepare a series of nano ferrite/carbon nano tube compound material; (4) nano ferrite/carbon nano tube compound material of application the present invention preparation has application promise in clinical practice and economic benefit in photocatalysis field; (5) nano ferrite/carbon nano tube compound material of application the present invention preparation has application promise in clinical practice and economic benefit aspect lithium ion battery.
Description of drawings
Fig. 1 is the XRD figure spectrum of instance 2 gained nano nickel ferrite/CNTs of the present invention (10 wt%) composite.
Fig. 2 is the Raman collection of illustrative plates of instance 2 gained nano nickel ferrite/CNTs of the present invention (10 wt%) composite.
Fig. 3 is the TEM and the EDS photo of instance 2 gained nano nickel ferrite/CNT (10wt%) composites of the present invention.
The specific embodiment
As shown in Figure 1, nano ferrite/CNT (5 wt% ~ 35 wt%) composite is got by the following steps preparation:
The first step is carried out ultrasonic dispersion 30-120 min with CNT in red fuming nitric acid (RFNA);
Second step joined the CNT in the first step in the mixed acid solution of the concentrated sulfuric acid that volume ratio is 1:1 and red fuming nitric acid (RFNA), was heated to 90-150 ℃, condensing reflux 6-18 h;
In the 3rd step, the CNT of getting after the acidifying joins in the ethanol ultrasonic dispersion 60-180 min;
The 4th step was that ferric nitrate and the nitrate of 2:1 joins stirring 10-90 min in the ethanol with mol ratio;
In the 5th step, the 3rd step gained system is mixed with the 4th step gained system, and stir 30-120 min;
The 6th step was transferred to the reaction system in the 5th step in the water heating kettle and reacts, and temperature is 120-200 ℃, and the reaction time is 12-24 h;
The 7th step with the product centrifugation of the 6th step, spent deionised water, and dry back obtains nano ferrite/CNT (5 wt% ~ 35 wt%) composite.
Embodiment 1:The preparation method of nano-ferrous acid/CNT (5 wt%) composite may further comprise the steps:
The first step is carried out ultrasonic dispersion 30 min with the CNT of 0.5 g in the red fuming nitric acid (RFNA) of 20 mL;
Second step joined 80 mL with the CNT in the first step, and volume ratio is in the mixed acid solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) of 1:1, is heated to 90 ℃, condensing reflux 18 h;
In the 3rd step, CNT 10 mg that get after the acidifying join in the ethanol of 20 mL ultrasonic dispersion 60 min;
In the 4th step, the cobalt nitrate of the ferric nitrate of 2 mmol and 1 mmol is joined in the ethanol of 60 mL and stir 10 min;
In the 5th step, the 3rd step gained system is mixed with the 4th step gained system, and stir 30 min;
The 6th step was transferred to the reaction system in the 5th step in the water heating kettle and reacts, and temperature is 120 ℃, and the reaction time is 24 h;
The 7th step with the product centrifugation of the 6th step, spent deionised water, and dry back obtains nano-ferrous acid/CNT (5 wt%) composite.
Embodiment 2:The preparation method of nano nickel ferrite/CNT (10 wt%) composite may further comprise the steps:
The first step is carried out ultrasonic dispersion 60 min with the CNT of 1.0 g in the red fuming nitric acid (RFNA) of 50 mL;
Second step joined 100mL with the CNT in the first step, and volume ratio is in the mixed acid solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) of 1:1, is heated to 100 ℃, condensing reflux 12 h;
In the 3rd step, CNT 30 mg that get after the acidifying join in the ethanol of 30 mL ultrasonic dispersion 90min;
In the 4th step, the nickel nitrate of the ferric nitrate of 2mmol and 1mmol is joined stirring 30 min in the ethanol of 50mL;
In the 5th step, the 3rd step gained system is mixed with the 4th step gained system, and stir 60 min;
The 6th step was transferred to the reaction system in the 5th step in the water heating kettle and reacts, and temperature is 140 ℃, and the reaction time is 20h;
The 7th step with the product centrifugation of the 6th step, spent deionised water, and dry back obtains nano nickel ferrite/CNT (10wt%) composite.
As shown in Figure 1, the nano nickel ferrite/CNT that makes (10 wt%) composite is spinel nano nickel ferrite based magnetic loaded (JCPDS 54-0964).
As shown in Figure 2, nickel ferrite based magnetic loaded and CNT well combine in the nano nickel ferrite/CNT that makes (10 wt%) composite.
As shown in Figure 3, the atomic ratio of iron and nickel is about 2:1 in the nano nickel ferrite/CNT that makes (10 wt%) composite, and nickel ferrite based magnetic loaded well has been coated on the surface of CNT.
Embodiment 3:The preparation method of nano ferrous acid copper/CNT (15 wt%) composite may further comprise the steps:
The first step is carried out ultrasonic dispersion 90 min with the CNT of 1.5 g in the red fuming nitric acid (RFNA) of 100 mL;
Second step joined 150 mL with the CNT in the first step, and volume ratio is in the mixed acid solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) of 1:1, is heated to 120 ℃, condensing reflux 10 h;
In the 3rd step, CNT 45 mg that get after the acidifying join in the ethanol of 40 mL ultrasonic dispersion 120 min;
In the 4th step, the copper nitrate of the ferric nitrate of 2 mmol and 1 mmol is joined in the ethanol of 40 mL and stir 50 min;
In the 5th step, the 3rd step gained system is mixed with the 4th step gained system, and stir 90 min;
The 6th step was transferred to the reaction system in the 5th step in the water heating kettle and reacts, and temperature is 160 ℃, and the reaction time is 18 h;
The 7th step with the product centrifugation of the 6th step, spent deionised water, and dry back obtains nano ferrous acid copper/CNT (15 wt%) composite.
Embodiment 4:The preparation method of nanometer zinc ferrite/CNT (20 wt%) composite may further comprise the steps:
The first step is carried out ultrasonic dispersion 100 min with the CNT of 2 g in the red fuming nitric acid (RFNA) of 150 mL;
Second step joined 200 mL with the CNT in the first step, and volume ratio is in the mixed acid solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) of 1:1, is heated to 140 ℃, condensing reflux 8 h;
In the 3rd step, CNT 60 mg that get after the acidifying join in the ethanol of 50 mL ultrasonic dispersion 150 min;
In the 4th step, the zinc nitrate of the ferric nitrate of 2 mmol and 1 mmol is joined in the ethanol of 50 mL and stir 70 min;
In the 5th step, the 3rd step gained system is mixed with the 4th step gained system, and stir 100 min;
The 6th step was transferred to the reaction system in the 5th step in the water heating kettle and reacts, and temperature is 180 ℃, and the reaction time is 16 h;
The 7th step with the product centrifugation of the 6th step, spent deionised water, and dry back obtains nanometer zinc ferrite/CNT (20 wt%) composite.
Embodiment 5:The preparation method of nanometer ferrous acid manganese/CNT (35 wt%) composite may further comprise the steps:
The first step is carried out ultrasonic dispersion 120 min with the CNT of 3 g in the red fuming nitric acid (RFNA) of 200 mL;
Second step joined 300 mL with the CNT in the first step, and volume ratio is in the mixed acid solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) of 1:1, is heated to 150 ℃, condensing reflux 6 h;
In the 3rd step, CNT 100 mg that get after the acidifying join in the ethanol of 60 mL ultrasonic dispersion 180 min;
In the 4th step, the manganese nitrate of the ferric nitrate of 2 mmol and 1 mmol is joined in the ethanol of 60 mL and stir 90 min;
In the 5th step, the 3rd step gained system is mixed with the 4th step gained system, and stir 120 min;
The 6th step was transferred to the reaction system in the 5th step in the water heating kettle and reacts, and temperature is 200 ℃, and the reaction time is 12 h;
The 7th step with the product centrifugation of the 6th step, spent deionised water, and dry back obtains nanometer ferrous acid manganese/CNT (35 wt%) composite.
Claims (8)
1. the preparation method of a nano ferrite/carbon nano tube compound material is characterized in that said method comprising the steps of:
In the 1st step, CNT is carried out ultrasonic dispersion in red fuming nitric acid (RFNA);
The 2nd step is with the further acidification in nitration mixture of the CNT in the 1st step;
The 3rd step is with the ultrasonic dispersion in ethanol of the CNT after the acidifying;
The 4th step is with ferric nitrate and nitrate stirring and dissolving in ethanol;
In the 5th step, the dispersion liquid and the 4th of the 3rd step gained is gone on foot gained solution mix and stir;
In the 6th step, the mixed liquor in the 5th step is transferred in the water heating kettle and reacts;
In the 7th step, the 6th step products therefrom centrifugation and washing, dry back are obtained nano ferrite/carbon nano tube compound material.
2. the preparation method of nano ferrite/carbon nano tube compound material according to claim 1 is characterized in that the ultrasonic jitter time described in the step 1 is 30-120 min.
3. the preparation method of nano ferrite/carbon nano tube compound material according to claim 1; It is characterized in that the nitration mixture described in the step 2 is the concentrated sulfuric acid and red fuming nitric acid (RFNA); Volume ratio is 1:1, and described acidification temperature is 90-150 ℃, and the acidification time is 6-18 h.
4. the preparation method of nano ferrite/carbon nano tube compound material according to claim 1 is characterized in that the ultrasonic jitter time described in the step 3 is 60-180 min.
5. the preparation method of nano ferrite/carbon nano tube compound material according to claim 1; It is characterized in that the mixing time described in the step 4 is 10-90 min; Described nitrate is nickel nitrate, cobalt nitrate, copper nitrate, zinc nitrate or manganese nitrate, and the mol ratio of described ferric nitrate and nitrate is 2:1.
6. the preparation method of nano ferrite/carbon nano tube compound material according to claim 1 is characterized in that the mixing time described in the step 5 is 30-120 min.
7. the preparation method of nano ferrite/carbon nano tube compound material according to claim 1 is characterized in that the reaction temperature described in the step 6 is 120-200 ℃, and the reaction time is 12-24h.
8. the preparation method of nano ferrite/carbon nano tube compound material according to claim 1 is characterized in that mass fraction 5 wt% ~ 35 wt% of the CNT in resulting nano ferrite/carbon nano tube compound material in the step 7.
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| CN111599604A (en) * | 2020-06-03 | 2020-08-28 | 邓新峰 | C-MnFe with shell-core structure2O4-CNT (carbon nanotube) supercapacitor electrode material and preparation method thereof |
| CN112436154A (en) * | 2020-12-01 | 2021-03-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of fuel cell cathode catalyst nano particle composite material |
| CN116328785A (en) * | 2023-03-27 | 2023-06-27 | 辽宁大学 | Manganese ferrite/tubular graphite phase carbon nitride heterojunction photocatalyst and preparation method and application thereof |
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