CN103566886B - Method for preparing magnetic activated carbon through DC cataphoresis deposition method - Google Patents
Method for preparing magnetic activated carbon through DC cataphoresis deposition method Download PDFInfo
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- CN103566886B CN103566886B CN201310571607.0A CN201310571607A CN103566886B CN 103566886 B CN103566886 B CN 103566886B CN 201310571607 A CN201310571607 A CN 201310571607A CN 103566886 B CN103566886 B CN 103566886B
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- active carbon
- molysite
- colloidal sol
- magnetic
- activated carbon
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Abstract
The invention discloses a method for preparing magnetic activated carbon through the DC cataphoresis deposition method. The method comprises the following steps: by utilizing the property that ferriferous colloidal particles in molysite collosol carry positive charge, and under the action of an additional pulse electric field, iron colloid particles are directionally electrophoresed into an activated carbon fine pores fixed near a negative pole; then the product obtained in the last step is impregnated in an alkali solution to be subjected to in-situ co-precipitation reaction so as to obtain the magnetic activated carbon. The method provided by the invention can realize green and efficient preparation of ferromagnetic magnetic activated carbon. Compared with a traditional method, the method provided by the invention has the advantages that the content of magnetic objects in the magnetic activated carbon is high, the magnetism is strong, the technology is simple, the cost is relatively low, and the method is suitable for industrial production after being modified.
Description
One, technical field
The present invention relates to a kind of preparation method of magnetic active carbon, specifically a kind of method being prepared magnetic active carbon by direct current electrophoretic deposition.
Two, background technology
Active carbon is widely used in fields such as catalytic reaction, bio-separation, cleaner productions as catalyst carrier and adsorbent.In application process, the recovery of active carbon adopts filtration method to realize usually, and the low weak effect of separative efficiency, have impact on it and apply.The research and development main purpose of magnetic active carbon gives active carbon with magnetic, makes it in use can realize quick, inexpensive, efficient separation and recovery.At present, magnetic active carbon is applied more field and is comprised the industry such as sewage disposal and noble metal recovery.
The existing preparation method of magnetic active carbon comprises:
1, absorption method: carry out finishing to magnetic nanoparticle, by adsorption and chemisorption, is attached to the inwall of activated carbon capillary.
2, sol impregnation method: the precursor sol preparing magnetic material, makes magnetic micelle enter activated carbon capillary road by infusion process, then obtains magnetic active carbon by the process such as subsequent chemical reaction, high-temperature process.
3, magnetic fluid infusion process: prepare magnetic fluid, makes the magnetic nanoparticle in magnetic fluid enter activated carbon capillary road by normal pressure or impregnating by pressure method, then obtains magnetic active carbon by processes such as oven dry.
, there is the shortcoming of following several respects in these traditional magnetic active carbon preparation methods:
1, owing to lacking enough power, the microchannel of magnetic-particle or magnetic micelle active carbon more difficult to get access, therefore in magnetic active carbon, effective magnetic material content is lower, and magnetic is more weak and unstable.
2, dipping or absorption method process is slow, efficiency is low, therefore prepare magnetic active carbon by these methods and be unwell to large-scale production.
3, magnetic fluid infusion process, prepares magnetic fluid complex process, and reagent consumption is large, easily produces pollution; Sol impregnation method, the treatment process after micelle dipping needs the condition such as high temperature, vacuum, and preparation cost is high.
Three, summary of the invention
The present invention is the weak point for avoiding existing for above-mentioned existing magnetic active carbon technology of preparing, aim to provide a kind of method being prepared magnetic active carbon by direct current electrophoretic deposition, technical problem to be solved improves specific magnetization and the preparation efficiency of magnetic active carbon, reduce production cost, to be suitable for suitability for industrialized production.
The present invention utilizes the character that in molysite colloidal sol, micelle is positively charged, under the effect of external electric field, making the directed electrophoresis of iron content colloidal solid in the Micro-v oid of active carbon being fixed on negative electrode, then obtaining magnetic active carbon by soaking generation original position coprecipitation reaction in aqueous slkali.
The present invention prepares the method for magnetic active carbon by direct current electrophoretic deposition, comprises each unit process of the preparation of molysite colloidal sol, electrophoretic deposition and post processing:
The preparation of described molysite colloidal sol is with FeCl
2and/or FeSO
4and FeCl
3for solute, be solvent with deionized water, according to Fe
3+and Fe
2+the proportions molysite colloidal sol of mol ratio 2:1, regulates the concentration of molysite colloidal sol and pH value to make the zeta potential of iron content micelle be 10-30meV; The pH value of molysite colloidal sol is regulated by hydrochloric acid solution or sodium hydroxide solution; The zeta potential of iron content micelle by electrophoresis technique determining, to grasp the carrying capacity size of iron content micelle under variable concentrations and pH value condition.
Described electrophoretic deposition is for electrophoretic liquid with described molysite colloidal sol, take carbon-point as anode, the copper sheet being covered with active carbon with surface constructs electrophoretic apparatus for negative electrode, electrode spacing 5-12cm, arranging extra electric field is DC pulse electric field, voltage 6-18v, pulse frequency 0.1-10Hz, effective pulsewidth occupation rate 60-80%, the electrophoretic deposition time is 240-720 second; The setting direction of extra electric field is the direction making the moving direction of iron content micelle point to negative electrode place, and iron content micelle is directed and is squeezed in activated carbon capillary hole under electrophoretic action.
Described post processing is that the alkali lye that the active carbon prepared by electrophoretic deposition is under agitation placed in pH value 10-11 floods 5-10min, namely obtains magnetic active carbon after 110-130 DEG C of drying.
In the preparation process of molysite colloidal sol, the concentration of molysite colloidal sol is about 0.5M, and pH value controls at 3.5-5.5.
The copper sheet that described surface is covered with active carbon industrial activited carbon grinding is sized to particle diameter≤0.15mm and is coated and fixed by fine-structure mesh to obtain behind the surface of copper sheet, control active carbon layer thickness≤2.0mm, to make the more all even microchannel entering active carbon fully of charged iron content micelle.
Described alkali lye is ammoniacal liquor or sodium hydroxide solution.
The present invention detects magnetic nanoparticle and the ferromagnetism of magnetic active carbon, the micro-structural of molysite nano particle/active carbon by the instrument such as vibrating specimen magnetometer, electron microscope, calculates magnetic material content to facilitate and estimates its magnetic suck effect.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the inventive method significantly improves the magnetic of magnetic active carbon, specific magnetization is refined by the mono-state of the 6-8emu/g(of negative pressure impregnation method, Zhang Guandong, Tian Qing, etc. the UV absorber of magnetic active carbon, engineering and process journal, 2004,4 (2): 141-145) be increased to 34.1emu/g, and magnetic distributing homogeneity is protected, be conducive to the application of magnetic active carbon.
2, the inventive method substantially increases the preparation efficiency of magnetic active carbon, can continuous seepage, through amplifying transformation, can be used for large-scale industrial production.
3, the inventive method reagent consumption is few, pollutes little; Technique is simple, does not need high temperature, application of vacuum, can reduce the production cost of magnetic active carbon.
Four, accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is electrophoretic deposition principle schematic.
Number in the figure: 1 positive plate; 2 charged colloidal particles; 3 silk screens; 4 minus plates; 5 activated carbon granules
Fig. 2 is the scanning electron microscope image of magnetic active carbon in embodiment 2.As can be seen from Figure 2, magnetic active carbon keeps the original sheet of active carbon or block structure, and surface does not find obvious clad, and this illustrates that magnetic components is mainly distributed in the inside of active carbon.
Fig. 3 is the images of transmissive electron microscope of magnetic active carbon in embodiment 1.As can be seen from Figure 3, dense distribution nano level magnetic-particle (stain that contrast is darker) in active carbon (translucent portion), what larger proportion in the microchannel of active carbon was described is filled with magnetic-particle.
Fig. 4 is the hysteresis curve of magnetic active carbon sample, wherein magnetic active carbon sample in the corresponding embodiment 1,2,3 of curve 1,2,3 difference.As can be seen from Figure 4 the magnetic active carbon that prepared by embodiment 1-3 all shows and stronger goes out room temperature superparamagnetism, wherein the specific magnetization of embodiment 1,2,3 product is respectively 34.1,30.0 and 22.6e mu/g, substantially exceeds the specific magnetization of the 6-8emu/g that negative pressure impregnation method obtains; Its coercivity is respectively 81.9,82.3 and 77.4Guass.Magnetic active carbon shows as superparamagnetism, is the characteristic feature of magnetic Nano material, and the magnetic material confirmed in magnetic active carbon is atomic thin nano particle.
Five, detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
1, the preparation of molysite colloidal sol
With FeCl
2and FeCl
3for solute, be solvent with deionized water, according to Fe
3+and Fe
2+the proportions concentration of mol ratio 2:1 is the molysite colloidal sol of about 0.5M, and regulate the pH value of molysite colloidal sol to 3.5-4.0, control the zeta potential 16-20meV of iron content micelle, the zeta potential of iron content micelle passes through electrophoresis technique determining.
2, electrophoretic deposition
Electrophoretic deposition set is configured according to shown in Fig. 1, with described molysite colloidal sol for electrophoretic liquid, take carbon-point as anode, the copper sheet being covered with active carbon with surface constructs electrophoretic apparatus, electrode spacing 6cm for negative electrode, and arranging extra electric field is DC pulse external electric field, voltage 6v, pulse frequency 5.0Hz, effective pulsewidth occupation rate 75%, the electrophoretic deposition time is 360 seconds; The setting direction of extra electric field is the direction at the moving direction sensing negative electrode place of iron content micelle, and iron content micelle is directed and is squeezed in activated carbon capillary hole under electrophoretic action.The copper sheet that wherein surface is covered with active carbon industrial activited carbon (being produced by forest chemical research institute of Chinese forest-science academy) grinding is sized to particle diameter≤0.15mm and is coated and fixed by fine-structure mesh to obtain behind the surface of copper sheet, control active carbon layer thickness≤2.0mm, to make the more all even microchannel entering active carbon fully of charged iron content micelle.
3, post processing
The active carbon that electrophoretic deposition is obtained be placed under electric stirring pH value be 10 NaOH solution flood 8min, namely obtain magnetic active carbon after 110-130 DEG C of drying.
Embodiment 2:
1, the preparation of molysite colloidal sol
With FeCl
2and FeCl
3for solute, be solvent with deionized water, according to Fe
3+and Fe
2+the proportions concentration of mol ratio 2:1 is the molysite colloidal sol of about 0.5M, and regulate the pH value of molysite colloidal sol to 4.0-4.5, control the zeta potential 14-17meV of iron content micelle, the zeta potential of iron content micelle passes through electrophoresis technique determining.
2, electrophoretic deposition
Electrophoretic deposition set is configured according to shown in Fig. 1, with described molysite colloidal sol for electrophoretic liquid, take carbon-point as anode, the copper sheet being covered with active carbon with surface constructs electrophoretic apparatus, electrode spacing 8cm for negative electrode, and arranging extra electric field is DC pulse external electric field, voltage 12v, pulse frequency 2.5Hz, effective pulsewidth occupation rate 60%, the electrophoretic deposition time is 540 seconds; The setting direction of extra electric field is the direction at the moving direction sensing negative electrode place of iron content micelle, and iron content micelle is directed and is squeezed in activated carbon capillary hole under electrophoretic action.The copper sheet that wherein surface is covered with active carbon industrial activited carbon grinding is sized to particle diameter≤0.15mm and is coated and fixed by fine-structure mesh to obtain behind the surface of copper sheet, control active carbon layer thickness≤2.0mm, to make the more all even microchannel entering active carbon fully of charged iron content micelle.
3, post processing
The NaOH solution that active carbon after electrophoretic deposition is under agitation placed in pH value 11 is flooded 6min, after 110-130 DEG C of drying, namely obtains magnetic active carbon.
Embodiment 3:
1, the preparation of molysite colloidal sol
With FeSO
4and FeCl
3for solute, be solvent with deionized water, according to Fe
3+and Fe
2+the proportions concentration of mol ratio 2:1 is the molysite colloidal sol of 0.5M, and regulate the pH value of molysite colloidal sol to 4.5-5.0, control the zeta potential 12-15meV of iron content micelle, the zeta potential of iron content micelle passes through electrophoresis technique determining.
2, electrophoretic deposition
Electrophoretic deposition set is configured according to shown in Fig. 1, with described molysite colloidal sol for electrophoretic liquid, take carbon-point as anode, the copper sheet being covered with active carbon with surface constructs electrophoretic apparatus, electrode spacing 8cm for negative electrode, and arranging extra electric field is DC pulse external electric field, voltage 15v, pulse frequency 2.0Hz, effective pulsewidth occupation rate 60%, the electrophoretic deposition time is 600 seconds; The setting direction of extra electric field is the direction at the moving direction sensing negative electrode place of iron content micelle, and iron content micelle is directed and is squeezed in activated carbon capillary hole under electrophoretic action.The copper sheet that wherein surface is covered with active carbon industrial activited carbon grinding is sized to particle diameter≤0.15mm and is coated and fixed by fine-structure mesh to obtain behind the surface of copper sheet, control active carbon layer thickness≤2.0mm, to make the more all even microchannel entering active carbon fully of charged iron content micelle.
3, post processing
The NaOH solution that active carbon after electrophoretic deposition is under agitation placed in pH value 11 is flooded 6min, after 110-130 DEG C of drying, namely obtains magnetic active carbon.
Claims (3)
1. prepared a method for magnetic active carbon by direct current electrophoretic deposition, comprise each unit process of the preparation of molysite colloidal sol, electrophoretic deposition and post processing, it is characterized in that:
The preparation of described molysite colloidal sol is according to Fe
3+and Fe
2+the proportions molysite colloidal sol of mol ratio 2:1, regulates the concentration of molysite colloidal sol and pH value to make the zeta potential of iron content micelle be 10-30meV;
Described electrophoretic deposition is for electrophoretic liquid with described molysite colloidal sol, take carbon-point as anode, the copper sheet being covered with active carbon with surface constructs electrophoretic apparatus for negative electrode, electrode spacing 5-12cm, arranging extra electric field is DC pulse electric field, and the direction arranging extra electric field is the direction making the moving direction of iron content micelle point to negative electrode place, voltage 6-18v, ripple frequency 0.1-10Hz, effective pulsewidth occupation rate 60-80%, the electrophoretic deposition time is 240-720 second; The copper sheet that described surface is covered with active carbon industrial activited carbon grinding is sized to particle diameter≤0.15mm and is coated and fixed by fine-structure mesh to obtain behind the surface of copper sheet, controls active carbon layer thickness≤2.0mm;
Described post processing is that the alkali lye that the active carbon prepared by electrophoretic deposition is under agitation placed in pH value 10-11 floods 5-10min, namely obtains magnetic active carbon after 110-130 DEG C of drying.
2. preparation method according to claim 1, is characterized in that:
In the preparation process of molysite colloidal sol, the concentration of molysite colloidal sol is 0.5M, and pH value controls at 3.5-5.5.
3. preparation method according to claim 1, is characterized in that:
Described alkali lye is ammoniacal liquor or sodium hydroxide solution.
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| CN109574090B (en) * | 2017-09-28 | 2020-09-15 | 比亚迪股份有限公司 | Nickel cobalt manganese hydroxide, positive electrode material, preparation method of positive electrode material and lithium ion battery |
| CN112295724B (en) * | 2020-09-14 | 2022-03-22 | 杭州电子科技大学 | Flotation method and flotation device for powdered activated carbon with different regeneration degrees |
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| CN101538711A (en) * | 2009-03-20 | 2009-09-23 | 同济大学 | Method for preparing ferroelectricicity-ferromagnetic composite thick film by combination of electrophoretic deposition and sol-gel |
| CN103329221A (en) * | 2011-01-26 | 2013-09-25 | 罗伯特·博世有限公司 | Synthesis of magnetic composites |
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| CN101538711A (en) * | 2009-03-20 | 2009-09-23 | 同济大学 | Method for preparing ferroelectricicity-ferromagnetic composite thick film by combination of electrophoretic deposition and sol-gel |
| CN103329221A (en) * | 2011-01-26 | 2013-09-25 | 罗伯特·博世有限公司 | Synthesis of magnetic composites |
Non-Patent Citations (2)
| Title |
|---|
| zhengyong zhang et al..Novel magnetic Fe3O4C nanoparticles as adsorbents for removal of organic dyes from aqueous solution.《Journal of Hazardous Materials》.2011,第193卷 * |
| 电泳沉积制备功能薄膜材料研究进展;周海佳 等;《材料导报》;20080831;第22卷;第311-315页 * |
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