CN103736457A - Preparation method and magnetic activated carbon prepared by same - Google Patents
Preparation method and magnetic activated carbon prepared by same Download PDFInfo
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- CN103736457A CN103736457A CN201310705320.2A CN201310705320A CN103736457A CN 103736457 A CN103736457 A CN 103736457A CN 201310705320 A CN201310705320 A CN 201310705320A CN 103736457 A CN103736457 A CN 103736457A
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Abstract
The invention relates to a preparation method and magnetic activated carbon prepared by the same. According to the invention, waste biomass is used as a raw material to prepare the magnetic activated carbon, and the raw material is low in price and easily available, so that the production cost of the magnetic activated carbon is greatly lowered. The activated carbon is recycled so as to avoid secondary pollution, and the preparation method has important meaning on the elimination of secondary pollution. In addition, the magnetic activated carbon is prepared by one step by combining three processes including carbonization, activation and magnetization. The production process is simple and the cost is lowered. Furthermore, the magnetic activated carbon not only has the advantages of high specific surface area and good adsorptive property, but also has an adjustable pore structure and has enough magnetic intensity and stable magnetic property.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic active carbon and the magnetic active carbon of being prepared by the method.
Background technology
Active carbon have high-specific surface area, good, the easy regeneration of absorption property, surface contain enrich functional group, catalytic performance is good and the advantage such as stable chemical performance, in fields such as environmental protection, national defence, chemical industry, food, be all widely used.Active carbon can be made by the material containing carbon rich.China all will produce a large amount of abandoned biomass every year, and these abandoned biomass phosphorus content are high, is the good raw material of preparing active carbon.
But recovery and utilization after active carbon is used are that activated carbon application field need to solve a difficult problem.At present, the method for recovered carbon mainly contains MF method, sedimentation.Wherein micro porous filtration can not selectively be held back, and construction cost, operating cost are also higher; Sedimentation can only reclaim bulky grain active carbon, and removal process is easily sneaked into other impurity.
Magnetic method is a kind of new recovery method of opening up recently.At present, the method for preparing magnetic active carbon mainly contains bonding method, infusion process, mixing method, magnetization agent method.The shortcomings such as it is unstable that magnetic active carbon prepared by bonding method, infusion process, mixing method has magnetic, and magnetic-particle easily comes off, and adsorptivity is not strong; And magnetization agent method has not only solved stability problem, and greatly improved absorption property, but above-mentioned preparation method is comprised of two key steps, the first step is prepared active carbon; Second step is composed magnetic active carbon, thus its preparation process complexity and preparation cost higher.In the application number patent of invention that is 200910077154.X, take coal as raw material, take magnetic metal oxide as magnetic additive, prepared magnetic active carbon, the magnetic property of magnetic active carbon prepared by the method is relatively stable, but in preparation process, used bonding agent, easily stopped up the space of this magnetic active carbon, therefore its absorption property is unstable; Meanwhile, in preparation process, first by the charing 0.5-2.5h in 400-700 ℃ of the article shaped after bonding forming, then carbide is activated to 2-40h in 700-1000 ℃; The relative additive method of its activation temperature is high, and preparation time is also longer.For another example in the patent of invention that application number is 02149357.X, by finished product active carbon, be raw material and after dipping, add alkali neutralization in iron content, copper, manganese solution, through ageing, washing, oven dry or heat 2h at 400-500 ℃, obtain magnetic active carbon.Magnetic active carbon prepared by the method can be used for removing the inorganic matters such as organic matter in water and arsenic, chromium, cadmium; But prepare in the process of magnetic active carbon and need ageing 2h, dry 9-30h, and the specific area of the magnetic active carbon of preparation only has 500-600m
2/ g.For another example in the patent of invention that application number is 03150818.9, take active carbon as raw material and ferroferric oxide powder are by 1:9(mass fraction, %) proportioning mixing and ball milling, obtains adding sodium metasilicate after elementary iron Carbon composites again, by liquid deposition, obtains wrapping up ferrosilicon Carbon composites; At 600～640 ℃ of reduction 1-3h, prepare the magnetic active carbon of containing metal iron.The magnetic active carbon that utilizes the method to prepare, grain diameter is little, and in tumor tissues blood vessel around, permeability is enhanced, and has obviously improved its curative effect as medicine.But the magnetic active carbon adsorptive value that utilizes the method to prepare is extremely low, and the addition of tri-iron tetroxide is also very large.
The method of magnetic active carbon processed can not solve the problem of stability and adsorptivity simultaneously at present, and complex manufacturing; These problems have limited active carbon and have applied more widely, and the research of the recovery of active carbon and utilization is also needed to further reinforcement.
Summary of the invention
The object of this invention is to provide a kind of difficult obstruction, specific area is large, and magnetic property is strong, that three processes of activation, magnetization and charing merge, the preparation method of the regulatable magnetic active carbon of pore structure and the magnetic active carbon of being prepared by the method.The method can obviously reduce the preparation cost of magnetic active carbon, promotes the application of active carbon, contributes to the development of environmental protection cause.
The present invention is achieved through the following technical solutions:
A method of being prepared magnetic active carbon by abandoned biomass, comprises following preparation process:
1) process is comprised to washing, abandoned biomass dry, broken, screening processing in early stage are placed in liquor zinci chloridi impregnation process; The abandoned biomass that obtains having flooded is standby;
Described abandoned biomass is preferably agricultural waste material, timber or timber waste;
2) at Fe
3o
4adsorb after laurate and dodecyl sodium sulfate two layers of surface activating agent from inside to outside successively on the surface of particle, obtains required magnetization agent;
3) the good abandoned biomass of described dipping and described magnetization agent are mixed, dry, obtain article shaped;
4), by the cracking under inert gas shielding of described article shaped, cracking final temperature is 400-500 ℃; Product, through washing, dry, obtains product magnetic active carbon.
Wherein,
The 1st), in step, according to the mass ratio of zinc chloride in abandoned biomass and liquor zinci chloridi, be preferably that 1:1-1:4 floods.
Dip time is preferably 12h-36h.
Preferably the 2nd) Fe in step
3o
4quality be the 1st) 5%-10% of abandoned biomass quality in step.
The 2nd) laurate, dodecyl sodium sulfate and Fe in step
3o
4mass ratio be all preferably 1:1-4:1.
The 2nd) the concrete preparation process of step magnetization agent is: by Fe
3o
4be added to the water with laurate, under alkali condition, water-bath 0.5-1h at 60-100 ℃; Acid adding, to pH=4～5, is collected and has been adsorbed the lauric Fe of one deck
3o
4particle, after washing, adds dodecyl sodium sulfate and water then, and water-bath 0.5-2h at 50-70 ℃, makes magnetization agent.
Described alkali condition can drip 3-6mol/LNaOH solution and realize, and described washing should be washed to pH=7 and be advisable.
Laurate, dodecyl sodium sulfate and Fe
3o
4mass ratio be all preferably 1:1-4:1.
The 4th) in step, heating rate during cracking is preferably 5-10 ℃/min, and temperature retention time is preferably 0.5-2h.
And the magnetic active carbon of preparing by said method.
The preferred preparation method of the present invention is as follows:
By wood material washing, dry, broken, screening, dry again after, the ratio that is 1:2 in raw material and zinc chloride mass ratio is placed in liquor zinci chloridi and floods 20-30h;
2. with Fe
3o
4for magnetic additive, first by Fe
3o
4be added to the water with laurate, drip 3-6mol/L NaOH solution to making solution be alkalescence, water-bath 0.5-1h at 60-100 ℃; Add wherein watery hydrochloric acid to pH=4～5, collect and adsorbed the lauric Fe of one deck
3o
4particle, is washed to pH=7, then adds dodecyl sodium sulfate and water, and water-bath 0.5-2h at 50-70 ℃, makes magnetization agent.
3. the cedar sawdust having flooded is mixed with the magnetization agent preparing, stir, put into baking oven dry.
4. by the cracking under argon shield of dried article shaped, cracking final temperature is 400-500 ℃, and heating rate is 5-10 ℃/min, and temperature retention time is 0.5-2h.Product, through washing, dry, grinding, obtains product magnetic active carbon.
The wood material that abandoned biomass described in the present invention adopts is preferably cedar sawdust.
In experimentation, if inventor finds Fe
3o
4directly mix with the cedar sawdust having flooded, dry, after intensification cracking, the product obtaining is dipped in water, the dispersed particle that can present crimson look in this water is Fe
3o
4, this phenomenon shows, Fe
3o
4separate with cedar sawdust.Inventor, by constantly testing and exploration discovery, by adding surfactant, utilizes surfactant by Fe
3o
4load to cedar sawdust, after intensification cracking, when the product obtaining is dipped in water, water is clarified, and Fe is described
3o
4be combined with wood chip.
The beneficial effect of the invention
Compared with prior art, preparation technology of the present invention is simple, by activation, magnetization and three process combinations of charing, realizes a step and makes magnetic active carbon; Meanwhile, can by controlling the consumption of magnetic additive, regulate the pore structure of magnetic active carbon, obtain the various products that need.In addition, the activation temperature of this preparation process is low, and energy consumption is low, and preparation process clean environment firendly; The raw material that the present invention uses is cheap and easy to get, has reduced the production cost of magnetic active carbon, and the recovery to active carbon, avoids causing secondary pollution to be significant.The magnetic active carbon of preparing by the present invention has high specific area, good absorption property, enough magnetic intensity and stable magnetic property.
Accompanying drawing explanation
Fig. 1 is the flow chart of the inventive method;
Fig. 2 is the XRD comparison diagram of comparative example 1 and embodiment 2 gained magnetic active carbons;
As shown in Figure 2, Fe
3o
4when addition is 10%, there is Fe
3o
4six diffraction maximums, be respectively (220), (311), (400), (422), (511), (440).In collection of illustrative plates, also there are three new peaks, wherein 2 θ=27.042 ° may be Fe
3o
4the peak of hydrolysate FeOOH, 2 θ=28.70 ° and 2 θ=47.59 ° may be ZnCl
2the peak of hydrolysate ZnO.
Fig. 3 a-b is the SEM figure of comparative example 1 gained magnetic active carbon, and wherein Fig. 3 a amplifies the SEM figure of 100 times, and figure amplifies the SEM figure of 500 times;
In Fig. 4, Fig. 4 a-c is the SEM figure of embodiment 2 gained magnetic active carbons, and wherein Fig. 4 a is for amplifying the SEM figure of 100 times, and Fig. 4 b, Fig. 4 c are for amplifying the SEM figure of 1000 times;
By Fig. 3 a-b and 4a-c, relatively can be obtained, when magnetic additive is 0%, activated carbon surface is smooth, there is no loaded article; And magnetic additive is while being 10%, there is the uniform loaded article of one deck on its surface, in conjunction with XRD testing result, can show that the active carbon of preparing by the method composed magnetic.
Fig. 5 is the comparison diagram of the hysteresis curve of comparative example 1, embodiment 1-2 gained magnetic active carbon.
As shown in Figure 5, along with Fe
3o
4the increase of addition, also along with increase, all has certain coercivity and remanent magnetism than saturated magnetic intensity, and the initial susceptibility of embodiment 1 and embodiment 2 all to reach magnetic separation required.
Fig. 6 a-b is respectively nitrogen adsorption figure and the graph of pore diameter distribution of comparative example 1, embodiment 1-2 gained magnetic active carbon.
As shown in Figure 6, specific area is along with Fe
3o
4the increase of addition and reducing, mesoporous and aperture are at Fe
3o
4it is maximum when addition is 6%.
The a-g figure of Fig. 7 is embodiments of the invention 1Fe
3o
4on successively absorption have the preparation process figure of the magnetization agent after laurate and dodecyl sodium sulfate two layers of surface activating agent.Wherein 7a is that tri-iron tetroxide and laurate are added to the water, and does not carry out heated water bath, and tri-iron tetroxide is separated with laurate, and upper strata is laurate, and beaker bottom is tri-iron tetroxide; 7b is for adding after NaOH, together with tri-iron tetroxide is set in laurate; After 7c is 90 ℃ of water-bath 1h, layering is obvious, and bottom is for having adsorbed lauric tri-iron tetroxide; 7d is for adding after watery hydrochloric acid, and cohesion appears in tri-iron tetroxide; 7e, for after washing, adds dodecyl sodium sulfate, is thick, and dodecyl sodium sulfate does not dissolve; After 7f is 60 ℃ of water-baths, dodecyl sodium sulfate dissolves; 7g is for adding after cedar sawdust, and cedar sawdust is uniformly distributed with magnetization agent.
Specific embodiment
Comparative example 1
Take 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is to prevent zinc chloride hydrolysis.Take 5g cedar sawdust, cedar sawdust is flooded in liquor zinci chloridi to 24h, wherein, the mass ratio of wood chip and zinc chloride is 1:2, dries 24h.The sample taking after oven dry is put in reacting furnace, argon shield, and cracking under 450 ℃ of final temperatures, 5 ℃/min of heating rate, the magnetic active carbon of preparing under insulation 1h condition, BET specific area is 1307.64m after tested
2/ g, total pore volume is 0.749cm
3/ g, iodine sorption value is 814mg/g, and methylene blue adsorption value is 200mg/g, and than saturated magnetic intensity 0.63856emu/g, coercivity is 95.20Oe, and remanent magnetism is 0.05861emu/g.
Wherein, the specific area of active carbon and pore-size distribution are measured (the nitrogen absorption when 77.35K) with Quadrasorb automatic absorbing instrument.The specific area of active carbon is calculated according to Brunauer-Emmett-Teller (BET) equation; Mesopore pore volume according to Density-Functional-Theory, (apply many to the method and HK method in the world at present by DFT, density functional method.) equation calculating; Pore-size distribution is according to Barrett, Joyner and Halenda(BJH) model calculates.(following examples use the same method mensuration)
Embodiment 1
Take 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is to prevent zinc chloride hydrolysis.Take 5g cedar sawdust, cedar sawdust is flooded in liquor zinci chloridi to 24h, wherein, the mass ratio of wood chip and zinc chloride is 1:2, takes 0.3gFe
3o
4, and 0.3g laurate, first by Fe
3o
4add in 15mL water with laurate, add 2mL5mol/L NaOH solution, water-bath 0.5h at 90 ℃; Add wherein watery hydrochloric acid to pH=4～5, collect and adsorbed the lauric Fe of one deck
3o
4particle, is washed to pH=7, then adds 0.6g dodecyl sodium sulfate and 20mL water, and water-bath 1h at 60 ℃, makes magnetization agent.The cedar sawdust having flooded is mixed with magnetization agent, stir, dry.The sample taking after oven dry is put in reacting furnace, argon shield, and cracking under 450 ℃ of final temperatures, 5 ℃/min of heating rate, the magnetic active carbon of preparing under insulation 1h condition, BET specific area is 896.07m after tested
2/ g, total pore volume is 0.567cm
3/ g, iodine sorption value is 817.98mg/g, and methylene blue adsorption value is 266mg/g, and than saturated magnetic intensity 1.548emu/g, coercivity is 77.72Oe, and remanent magnetism is 0.123emu/g, initial susceptibility is 1.752 * 10
-5.
Take 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is to prevent zinc chloride hydrolysis.Take 5g cedar sawdust, cedar sawdust is flooded in liquor zinci chloridi to 24h, wherein, the mass ratio of wood chip and zinc chloride is 1:2, takes 0.5gFe
3o
4, and 1.0g laurate, first by Fe
3o
4add in 15mL water with laurate, add 2mL5mol/L NaOH solution, water-bath 0.5h at 90 ℃; Add wherein watery hydrochloric acid to pH=4～5, collect and adsorbed the lauric Fe of one deck
3o
4particle, is washed to pH=7, then adds 1.0g dodecyl sodium sulfate and 20mL water, and water-bath 1h at 60 ℃, makes magnetization agent.The cedar sawdust having flooded is mixed with magnetization agent, stir, dry.The sample taking after oven dry is put in reacting furnace, argon shield, and cracking under 450 ℃ of final temperatures, 5 ℃/min of heating rate, the magnetic active carbon of preparing under insulation 1h condition, BET specific area is 774.28m after tested
2/ g, total pore volume is 0.423cm3/g, and iodine sorption value is 863.02mg/g, and methylene blue adsorption value is 327.23mg/g, and than saturated magnetic intensity 8.881emu/g, coercivity is 97.25Oe, and remanent magnetism is 0.851emu/g, and initial susceptibility is 9.306 * 10
-5.
Embodiment 3
Take 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is to prevent zinc chloride hydrolysis.Take 5g cedar sawdust, cedar sawdust is flooded in liquor zinci chloridi to 24h, wherein, the mass ratio of wood chip and zinc chloride is 1:2, takes 0.5gFe
3o
4, and 1.0g laurate, first by Fe
3o
4add in 15mL water with laurate, add 2mL5mol/L NaOH solution, water-bath 0.5h at 90 ℃; Add wherein watery hydrochloric acid to pH=4～5, collect and adsorbed the lauric Fe of one deck
3o
4particle, is washed to pH=7, then adds 1.0g dodecyl sodium sulfate and 20mL water, and water-bath 1h at 60 ℃, makes magnetization agent.The cedar sawdust having flooded is mixed with magnetization agent, stir, dry.The sample taking after oven dry is put in reacting furnace, argon shield, and cracking under 400 ℃ of final temperatures, 5 ℃/min of heating rate, the magnetic active carbon of preparing under insulation 1h condition, BET specific area is 112.753m after tested
2/ g, total pore volume is 0.594cm
3/ g, iodine sorption value is 756.77mg/g, and methylene blue adsorption value is 324.23mg/g, and than saturated magnetic intensity 2.567emu/g, coercivity is 38.29Oe, and remanent magnetism is 0.139emu/g, initial susceptibility is 3.143 * 10
-5.
Take 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is to prevent zinc chloride hydrolysis.Take 5g cedar sawdust, cedar sawdust is flooded in liquor zinci chloridi to 24h; Wherein, the mass ratio of wood chip and zinc chloride is 1:2, takes 0.5gFe
3o
4, and 1.0g laurate, first by Fe
3o
4add in 15mL water with laurate, add 2mL5mol/L NaOH solution, water-bath 0.5h at 90 ℃; Add wherein watery hydrochloric acid to pH=4～5, collect and adsorbed the lauric Fe of one deck
3o
4particle, is washed to pH=7, then adds 1.0g dodecyl sodium sulfate and 20mL water, and water-bath 1h at 60 ℃, makes magnetization agent.The cedar sawdust having flooded is mixed with magnetization agent, stir, dry.The sample taking after oven dry is put in reacting furnace, argon shield, and cracking under 500 ℃ of final temperatures, 5 ℃/min of heating rate, the magnetic active carbon of preparing under insulation 1h condition, BET specific area is 1818.143m after tested
2/ g, total pore volume is 1.026cm
3/ g, iodine sorption value is 926.61mg/g, and methylene blue adsorption value is 327.51mg/g, and than saturated magnetic intensity 2.217emu/g, coercivity is 6.17Oe, and remanent magnetism is 0.0145emu/g, initial susceptibility is 5.389 * 10
-5.
Claims (9)
1. by abandoned biomass, prepared a method for magnetic active carbon, it is characterized in that, comprise the following steps:
1) process is comprised to washing, abandoned biomass dry, broken, screening processing in early stage are placed in liquor zinci chloridi impregnation process, the abandoned biomass that obtains having flooded is standby;
Wherein, described abandoned biomass is agricultural waste material, timber or timber waste;
2) at Fe
3o
4adsorb after laurate and dodecyl sodium sulfate two layers of surface activating agent from inside to outside successively on the surface of particle, obtains required magnetization agent;
3) by the described the 1st) abandoned biomass and the 2nd that flooded of step) magnetization agent described in step mixes, dry, obtains article shaped;
4) by the cracking under inert gas shielding of described article shaped, cracking final temperature is 400-500 ℃, and pyrolysis product, through washing, dry, is obtained to product magnetic active carbon.
2. in step, according to the mass ratio of zinc chloride in abandoned biomass and liquor zinci chloridi, be method according to claim 1, is characterized in that, the 1st) that 1:1～4 are flooded.
3. method according to claim 2, is characterized in that, the 1st) in step, dip time is 24h-30h.
4. method according to claim 1, is characterized in that, the 2nd) Fe in step
3o
4quality be the 1st) 5%-10% of the quality of abandoned biomass in step.
5. method according to claim 4, is characterized in that, the 2nd) Fe in step
3o
4quality be the 1st) in step abandoned biomass 6% or 10%.
6. method according to claim 1, is characterized in that, the 2nd) laurate and Fe in step
3o
4mass ratio, dodecyl sodium sulfate and Fe
3o
4mass ratio be 1:1-4:1.
7. method according to claim 1, is characterized in that, the preparation process of described magnetization agent is: by Fe
3o
4be added to the water with laurate, at alkali condition, water-bath 0.5-1h at 60-100 ℃; Acid adding is to pH=4～5 wherein again, and collecting to have adsorbed has lauric Fe
3o
4particle, after washing, adds dodecyl sodium sulfate and water, and at 50-70 ℃, water-bath 0.5-2h, makes; Wherein, described Fe
3o
4quality be the 5%-10% of abandoned biomass quality; Laurate and Fe
3o
4mass ratio, dodecyl sodium sulfate and Fe
3o
4mass ratio be 1:1-4:1.
8. method according to claim 1, is characterized in that, the 4th) in step, heating rate during cracking is 5-10 ℃/min, and temperature retention time is 0.5-2h.
9. the magnetic active carbon of being prepared by the method described in claim 1-8 any one.
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Cited By (6)
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|---|---|---|---|---|
| CN104368308A (en) * | 2014-07-03 | 2015-02-25 | 中国科学院西北高原生物研究所 | Compound adsorbent based on hippophae rhamnoides linn branches and trunks and preparation method of compound adsorbent |
| CN105709691A (en) * | 2016-03-04 | 2016-06-29 | 深圳市翔丰华科技有限公司 | Preparation method of magnetic activated carbon |
| CN106824095A (en) * | 2017-03-01 | 2017-06-13 | 中南大学 | A kind of preparation method of biomass magnetic active carbon |
| CN109877143A (en) * | 2019-04-10 | 2019-06-14 | 黑龙江省农业科学院土壤肥料与环境资源研究所 | A kind of straw waste recycling and reusing processing method and adsorbent |
| CN110078177A (en) * | 2019-04-19 | 2019-08-02 | 广西民族大学 | A kind of SnO2- GAC particle and its preparation method and application |
| CN111661943A (en) * | 2020-06-11 | 2020-09-15 | 浙江恒美环保科技有限公司 | Comprehensive utilization method of biogas slurry |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104368308A (en) * | 2014-07-03 | 2015-02-25 | 中国科学院西北高原生物研究所 | Compound adsorbent based on hippophae rhamnoides linn branches and trunks and preparation method of compound adsorbent |
| CN105709691A (en) * | 2016-03-04 | 2016-06-29 | 深圳市翔丰华科技有限公司 | Preparation method of magnetic activated carbon |
| CN105709691B (en) * | 2016-03-04 | 2018-10-02 | 深圳市翔丰华科技股份有限公司 | A kind of preparation method of magnetic active carbon |
| CN106824095A (en) * | 2017-03-01 | 2017-06-13 | 中南大学 | A kind of preparation method of biomass magnetic active carbon |
| CN109877143A (en) * | 2019-04-10 | 2019-06-14 | 黑龙江省农业科学院土壤肥料与环境资源研究所 | A kind of straw waste recycling and reusing processing method and adsorbent |
| CN109877143B (en) * | 2019-04-10 | 2021-11-30 | 黑龙江省农业科学院土壤肥料与环境资源研究所 | Straw waste recycling treatment method and adsorbent |
| CN110078177A (en) * | 2019-04-19 | 2019-08-02 | 广西民族大学 | A kind of SnO2- GAC particle and its preparation method and application |
| CN111661943A (en) * | 2020-06-11 | 2020-09-15 | 浙江恒美环保科技有限公司 | Comprehensive utilization method of biogas slurry |
| CN111661943B (en) * | 2020-06-11 | 2022-08-23 | 浙江恒美环保科技有限公司 | Comprehensive biogas slurry utilization method |
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| CN103736457B (en) | 2016-07-06 |
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