CN103157438A - Preparation method of carbon microsphere/nanometer iron oxide magnetic composite material - Google Patents
Preparation method of carbon microsphere/nanometer iron oxide magnetic composite material Download PDFInfo
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- CN103157438A CN103157438A CN2013101230951A CN201310123095A CN103157438A CN 103157438 A CN103157438 A CN 103157438A CN 2013101230951 A CN2013101230951 A CN 2013101230951A CN 201310123095 A CN201310123095 A CN 201310123095A CN 103157438 A CN103157438 A CN 103157438A
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Abstract
The invention discloses a preparation method of a carbon microsphere/nanometer iron oxide magnetic composite material, relates to a preparation method of the magnetic composite material for water treatment, and aims at solving the problems that the existing adsorbent is low in heavy metal adsorption capacity and unlikely to separate and remove. The preparation method comprises the following steps of: firstly, carrying out hydrothermal reaction onto glucose, washing by deionized water and absolute ethyl alcohol after cooling, and obtaining the carbon microspheres by vacuum-drying; secondly, adding the carbon microspheres into water for carrying out ultrasonic dispersion, adding trivalent iron salt and bivalent iron salt to the solution, heating and stirring the solution, dropping alkaline solution to regulate the pH of the solution and carrying out water-bath ageing; separating solid products by magnets and obtaining the magnetic composite material after washing the solid products through vacuum-drying. The carbon microsphere/nanometer iron oxide magnetic composite material obtained by the preparation method disclosed by the invention is large in adsorption capacity, has equilibrium adsorption capacity of 71.03mg.g<-1> to Cd2<+> at 25 DEG C, and is capable of being quickly separated by a magnetic separation method and mainly applied to the water treatment field.
Description
Technical field
The present invention relates to a kind of water treatment preparation method, the particularly preparation method of a kind of carbosphere/nano-iron oxide magnetic composite of magnetic composite.
Background technology
Heavy metal wastewater thereby is that environmental pollution is the most serious and the mankind are endangered one of maximum industrial wastewater, because heavy metal contaminants can't be biodegradable and destroy, harm time is long, in a single day the waste water that contains heavy metal be thrown into environment, can by the effect of drinking-water and food chain, cause serious harm to the human physical and mental health.Existing heavy metal treatment technology mainly contains chemical precipitation method, oxidizing process and reducing process, ion-exchange, absorption method, electrochemical process and membrane separation process etc.Absorption method because of its have selectively good, process the advantages such as low concentration heavy metal water is effective, workable and be widely used.But because existing adsorbent (as Powdered Activated Carbon) adsorption capacity is little, be difficult to separate, reclaim.For above problem, the adsorbent that need to develop efficiently, the heavy metal adsorption capacity is large, is easy to separate.
Magnetic separates and can carry out more fast and efficiently Selective Separation, can be by with ferromagnetic material and the compound magnetic adsorbent for preparing of adsorbent, and this technology is for the active carbon of modification.As Fuertes etc., Powdered Activated Carbon is dropped into Fe (NO
3)
3Alcohol dispersion liquid in, (Fuertes A B.Chem.Mater., 2006,18 (6): 1676), but the standby temperature of this legal system is higher, operates more complicated to obtain the magnetic active carbon of tool through heat treatment under nitrogen atmosphere.Ferriferous oxide coprecipitation preparation temperature is low, and is simple to operate, so the standby magnetic adsorbent composite of available this legal system.Oliveira etc. just utilize the ferriferous oxide coprecipitation to prepare magnetic active carbon, magnetic active carbon can be separated from water by add magnetic field in system.The BET specific surface area analysis shows, is deposited on the iron oxide particle of activated carbon surface to specific area, pore structure and the absorption property of active carbon impact (Oliveira L C A.Carbon, 2002,40 (12): 2178) not almost all.But active carbon is less to the heavy metal adsorption amount, for this problem, proposes to adopt the carbosphere of hydro-thermal method preparation to replace active carbon as adsorbent.The carbosphere of hydro-thermal method preparation has the following advantages: take living beings as raw material, the source is abundant, low price; Without strong acid and strong base, only with water as solvent; Preparation temperature is lower, and flow process is simple; Have huge specific area, size is controlled; The surface contains enriches oxy radical, can Adsorption of Heavy Metals, and be easy to modification, the heavy metal adsorption effect is improved greatly, than modified activated carbon advantages of good adsorption effect.So just can solve the little problem of adsorbent Adsorption of Heavy Metals capacity.
Summary of the invention
The present invention seeks in order to solve the little and problem of easily separated removal not of existing adsorbent heavy metal adsorption capacity, and propose the preparation method of a kind of carbosphere/nano-iron oxide magnetic composite.
The preparation method of carbosphere of the present invention/nano-iron oxide magnetic composite follows these steps to realize:
One, the D/W with 0.1~0.2g/mL changes in the polytetrafluoroethyllining lining stainless steel cauldron, after reacting 12~20h under the condition of 180~190 ℃, naturally cool to room temperature, after centrifugation, with deionized water and absolute ethyl alcohol, centrifugal products therefrom is washed till neutrality successively, then vacuum drying obtains carbosphere;
two, the carbosphere that step 1 is obtained joins in deionized water, through the ultrasonic decentralized configuration concentration carbosphere dispersion liquid that is 2.0~3.0g/L, add successively trivalent iron salt and divalent iron salt in the carbosphere dispersion liquid, after iron salt dissolved, the carbosphere dispersion liquid is heated to 60~80 ℃, stir 15.0~30.0min, keep stirring, dropwise add again alkaline solution, regulation system pH to 8~11, reaction 0.5~1.0h is placed on 100 ℃ of water-bath ageing 3.0~4.0h, naturally cool to room temperature, then isolate solid product with magnet, use respectively deionized water and absolute ethanol washing solid product to neutral, obtain carbosphere/nano-iron oxide magnetic composite through vacuum drying,
Wherein the mass ratio of the gross mass of the described trivalent iron salt of step 2 and divalent iron salt and carbosphere is (1~4): 1, and trivalent iron salt is ferric sulfate or iron chloride, divalent iron salt is ferrous sulfate or frerrous chloride; Alkaline solution is sodium hydroxide solution, potassium hydroxide solution or ammonia spirit.
The present invention first adopts hydrothermal reaction at low temperature to prepare the carbosphere that particle diameter is 0.2~1 μ m, then the ferriferrous oxide nano crystalline substance that is 40~150nm with particle diameter by the ferriferous oxide coprecipitation is wrapped on carbosphere.The carbosphere that obtains by preparation method of the present invention/nano-iron oxide magnetic composite has following characteristics: (1) magnetic composite surface contains enriches oxy radical, can Adsorption of Heavy Metals, at 25 ℃ to Cd
2+(initial concentration 50mgL
-1) equilibrium adsorption capacity be 71.03mgg
-1(2) have magnetic, can separate fast by magnetism separate method, reclaim; (3) preparation flow is simple, can complete preparation process at a lower temperature.The present invention is mainly used in water treatment.
Description of drawings
Fig. 1 is the surface sweeping electromicroscopic photograph of the carbosphere/nano-iron oxide magnetic composite of embodiment 1 preparation;
Fig. 2 is the transmission electron microscope photo of the carbosphere/nano-iron oxide magnetic composite of embodiment 1 preparation;
Fig. 3 is the design sketch that carbosphere/the nano-iron oxide magnetic composite is dispersed in water of embodiment 1 preparation;
Fig. 4 is the design sketch of the carbosphere/after the nano-iron oxide magnetic composite separates by magnet of embodiment 1 preparation.
The specific embodiment
The preparation method of present embodiment carbosphere/nano-iron oxide magnetic composite follows these steps to implement:
One, the D/W with 0.1~0.2g/mL changes in the polytetrafluoroethyllining lining stainless steel cauldron, after reacting 12~20h under the condition of 180~190 ℃, naturally cool to room temperature, after centrifugation, with deionized water and absolute ethyl alcohol, centrifugal products therefrom is washed till neutrality successively, then vacuum drying obtains carbosphere;
two, the carbosphere that step 1 is obtained joins in deionized water, through the ultrasonic decentralized configuration concentration carbosphere dispersion liquid that is 2.0~3.0g/L, add successively trivalent iron salt and divalent iron salt in the carbosphere dispersion liquid, after iron salt dissolved, the carbosphere dispersion liquid is heated to 60~80 ℃, stir 15.0~30.0min, keep stirring, dropwise add again alkaline solution, regulation system pH to 8~11, reaction 0.5~1.0h is placed on 100 ℃ of water-bath ageing 3.0~4.0h, naturally cool to room temperature, then isolate solid product with magnet, use respectively deionized water and absolute ethanol washing solid product to neutral, obtain carbosphere/nano-iron oxide magnetic composite through vacuum drying,
Wherein the mass ratio of the gross mass of the described trivalent iron salt of step 2 and divalent iron salt and carbosphere is (1~4): 1, and trivalent iron salt is ferric sulfate or iron chloride, divalent iron salt is ferrous sulfate or frerrous chloride; Alkaline solution is sodium hydroxide solution, potassium hydroxide solution or ammonia spirit.
Present embodiment carbosphere/nano-iron oxide magnetic composite can be used for be removed the heavy metal ion such as the cadmium, lead, chromium of water, and the heavy metal adsorption capacity is higher, at 25 ℃ to Cd
2+(initial concentration 50mgL
-1) equilibrium adsorption capacity 71.03mgg
-1, having improved the adsorption capacity of heavy metal, can separate fast by simple magnetism separate method after Adsorption of Heavy Metal Ions.
The specific embodiment two: what present embodiment was different from the specific embodiment one is that the step 1 D/W changes in the polytetrafluoroethyllining lining stainless steel cauldron, and the compactedness of D/W in the polytetrafluoroethyllining lining stainless steel cauldron is 70%~80%.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: present embodiment is different from the specific embodiment one or two be step 1 through centrifugation, be 7000~10000 to turn/rotating speed centrifugation 5.0~15.0min of min.Other step and parameter are identical with the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three is that vacuum drying in step 1 and step 2 is vacuum drying 12h at the temperature of 50 ℃.Other step and parameter are identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different from one of specific embodiment one to four is that the ultrasonic dispersion of step 2 is the power ultrasonic dispersion 10.0~20.0min with 100W.Other step and parameter are identical with one of specific embodiment one to four.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is that alkaline solution is the NaOH solution of 5.0mol/L.Other step and parameter are identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different from one of specific embodiment one to six is that the gross mass of trivalent iron salt and divalent iron salt and the mass ratio of carbosphere are 2:1.Other step and parameter are identical with one of specific embodiment one to six.
The specific embodiment eight: present embodiment is different from one of specific embodiment one to seven, and to be trivalent iron salt be (1~2) with the ratio of the amount of substance of divalent iron salt: 1.Other step and parameter are identical with one of specific embodiment one to seven.
The specific embodiment nine: what present embodiment was different from one of specific embodiment one to seven is that trivalent iron salt is iron chloride, and divalent iron salt is ferrous sulfate.Other step and parameter are identical with one of specific embodiment one to seven.
Embodiment one: the preparation method of the present embodiment carbosphere/nano-iron oxide magnetic composite follows these steps to implement:
One, be that the D/W of 0.1g/mL changes in the polytetrafluoroethyllining lining stainless steel cauldron of 50.0mL with 40mL concentration, after reaction 16h under the condition of 190 ℃, naturally cool to room temperature, 7000 to turn/the rotating speed centrifugation 10min of min, with deionized water and absolute ethyl alcohol, centrifugal products therefrom is washed till neutrality successively, then obtains carbosphere at 50 ℃ of lower vacuum drying 12h;
Two, step 1 is obtained the 0.1g carbosphere and join in the 50mL deionized water, through ultrasonic dispersion 15.0min configuration carbosphere dispersion liquid, add successively 0.1g FeCl in the carbosphere dispersion liquid
3H
2O and 0.1g FeSO
47H
2O, after iron salt dissolved, the carbosphere dispersion liquid is heated to 70 ℃, stir 30.0min, keep stirring, dropwise adding concentration is the NaOH solution of 5.0mol/L again, regulation system pH to 10, and reaction 0.5h is placed on 100 ℃ of water-bath ageing 4.0h, naturally cool to room temperature, then isolate solid product with magnet, use respectively deionized water and absolute ethanol washing solid product to neutral, obtain carbosphere/nano-iron oxide magnetic composite at 50 ℃ of lower vacuum drying 12h;
Wherein the power of the ultrasonic dispersion of step 2 is 100W.
The surface sweeping electromicroscopic photograph of the carbosphere of the present embodiment preparation/nano-iron oxide magnetic composite as shown in Figure 1;
The transmission electron microscope photo of the carbosphere of the present embodiment preparation/nano-iron oxide magnetic composite as shown in Figure 2;
The design sketch that carbosphere/the nano-iron oxide magnetic composite is dispersed in water of the present embodiment preparation as shown in Figure 3, carbosphere/nano-iron oxide magnetic composite at 25 ℃ to Cd
2+(initial concentration 50mgL
-1) equilibrium adsorption capacity 71.03mgg
-1, upon adsorption saturated after, can separate fast by magnet, the design sketch after separation as shown in Figure 4.
Claims (9)
1. the preparation method of carbosphere/nano-iron oxide magnetic composite is characterized in that the preparation method of carbosphere/nano-iron oxide magnetic composite follows these steps to realize:
One, the D/W with 0.1~0.2g/mL changes in the polytetrafluoroethyllining lining stainless steel cauldron, after reacting 12~20h under the condition of 180~190 ℃, naturally cool to room temperature, after centrifugation, with deionized water and absolute ethyl alcohol, centrifugal products therefrom is washed till neutrality successively, then vacuum drying obtains carbosphere;
two, the carbosphere that step 1 is obtained joins in deionized water, through the ultrasonic decentralized configuration concentration carbosphere dispersion liquid that is 2.0~3.0g/L, add successively trivalent iron salt and divalent iron salt in the carbosphere dispersion liquid, after iron salt dissolved, the carbosphere dispersion liquid is heated to 60~80 ℃, stir 15.0~30.0min, keep stirring, dropwise add again alkaline solution, regulation system pH to 8~11, reaction 0.5~1.0h is placed on 100 ℃ of water-bath ageing 3.0~4.0h, naturally cool to room temperature, then isolate solid product with magnet, use respectively deionized water and absolute ethanol washing solid product to neutral, obtain carbosphere/nano-iron oxide magnetic composite through vacuum drying,
Wherein the mass ratio of the gross mass of the described trivalent iron salt of step 2 and divalent iron salt and carbosphere is (1~4): 1, and trivalent iron salt is ferric sulfate or iron chloride, divalent iron salt is ferrous sulfate or frerrous chloride; Alkaline solution is sodium hydroxide solution, potassium hydroxide solution or ammonia spirit.
2. the preparation method of a kind of carbosphere according to claim 1/nano-iron oxide magnetic composite, it is characterized in that the step 1 D/W changes in the polytetrafluoroethyllining lining stainless steel cauldron, the compactedness of D/W in the polytetrafluoroethyllining lining stainless steel cauldron is 70%~80%.
3. the preparation method of a kind of carbosphere according to claim 1/nano-iron oxide magnetic composite, is characterized in that step 1 through centrifugation, is 7000~10000 to turn/rotating speed centrifugation 5.0~15.0min of min.
4. the preparation method of a kind of carbosphere according to claim 1/nano-iron oxide magnetic composite, is characterized in that the vacuum drying in step 1 and step 2 is vacuum drying 12h at the temperature of 50 ℃.
5. the preparation method of a kind of carbosphere according to claim 1/nano-iron oxide magnetic composite, is characterized in that the ultrasonic dispersion of step 2 is the power ultrasonic dispersion 10.0~20.0min with 100W.
6. the preparation method of a kind of carbosphere according to claim 1/nano-iron oxide magnetic composite, is characterized in that alkaline solution is the NaOH solution of 5.0mol/L.
7. the preparation method of a kind of carbosphere according to claim 1/nano-iron oxide magnetic composite, is characterized in that the gross mass of trivalent iron salt and divalent iron salt and the mass ratio of carbosphere are 2:1.
8. the preparation method of a kind of carbosphere according to claim 1/nano-iron oxide magnetic composite, is characterized in that trivalent iron salt and the ratio of the amount of substance of divalent iron salt are (1~2): 1.
9. the preparation method of a kind of carbosphere according to claim 8/nano-iron oxide magnetic composite, is characterized in that trivalent iron salt is iron chloride, and divalent iron salt is ferrous sulfate.
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