CN103736457B - The preparation method of a kind of magnetic active carbon and the magnetic active carbon prepared by the method - Google Patents
The preparation method of a kind of magnetic active carbon and the magnetic active carbon prepared by the method Download PDFInfo
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Abstract
The preparation method of a kind of magnetic active carbon and the magnetic active carbon prepared by the method, the present invention selects abandoned biomass to prepare magnetic active carbon as raw material, this cheaper starting materials is easy to get, greatly reduce the production cost of magnetic active carbon, recovery to activated carbon, it is to avoid cause secondary pollution to have great importance.Additionally, by carbonization, activation and three processes of magnetization are merged, it is achieved that a step prepares magnetic active carbon, and production technology is simple, and cost reduces.It addition, the advantage that magnetic active carbon not only has high-specific surface area, absorption property is good prepared, and its pore structure controllable, there is enough magnetic intensities and stable magnetic property simultaneously.
Description
Technical field
The present invention relates to the preparation method of a kind of magnetic active carbon and the magnetic active carbon prepared by the method.
Background technology
Activated carbon has high-specific surface area, abundant functional group is contained on absorption property regeneration good, easy, surface, catalytic performance is good and the advantage such as stable chemical performance, is obtained in fields such as environmental protection, national defence, chemical industry, food and is widely applied.Activated carbon can be prepared by the material containing carbon rich.China will produce substantial amounts of abandoned biomass every year, and these abandoned biomass phosphorus content are high, are the good raw material preparing activated carbon.
But the recovery after activated carbon use and utilization are activated carbon application fields to be needed to solve a difficult problem.At present, the method for recovered carbon mainly has MF method, sedimentation.Wherein microporous filter can not retain by selectivity, and construction cost, operating cost are also higher;Sedimentation can only reclaim bulky grain activated carbon, and removal process is easily mixed into other impurity.
Magnetic method is a kind of new recovery method of exhibition recently.At present, the method preparing magnetic active carbon mainly has bonding method, infusion process, mixing method, Magnetic reagent method.The shortcomings such as magnetic active carbon prepared by bonding method, infusion process, mixing method has magnetic instability, and magnetic-particle is easy to fall off, and adsorptivity is not strong;And Magnetic reagent method not only solves stability problem, and substantially increasing absorption property, but above-mentioned preparation method is all made up of two key steps, namely the first step prepares activated carbon;Second step composes magnetic activated carbon, and therefore its preparation process complexity and preparation cost are higher.As in patent of invention that application number is 200910077154.X, with coal for raw material, with magnetic metal-oxide for magnetic additive, it is prepared for magnetic active carbon, the magnetic property of magnetic active carbon prepared by the method is relatively stable, but in preparation process, employ bonding agent, it is easy to block the space of this magnetic active carbon, therefore its absorption property is unstable;Meanwhile, in preparation process, first by the carbonization 0.5-2.5h in 400-700 DEG C of the article shaped after bonding forming, then carbide is activated in 700-1000 DEG C 2-40h;The relative additive method of its activation temperature is high, and preparation time is also longer.For another example application number is in the patent of invention of 02149357.X, by finished activated charcoal be raw material and in iron content, copper, manganese solution dipping after, add alkali neutralize, aged, washing, dry or at 400-500 DEG C heat 2h, obtain magnetic active carbon.The inorganic matters such as Organic substance and arsenic, chromium, the cadmium that magnetic active carbon prepared by the method can be used for removing in water;But prepare and the process of magnetic active carbon needs ageing 2h, dry 9-30h, and the specific surface area of the magnetic active carbon of preparation only has 500-600m2/g.For another example application number is in the patent of invention of 03150818.9,1:9(mass fraction is pressed for raw material and ferroferric oxide powder with activated carbon, %) proportioning mixing and ball milling, adds sodium silicate after obtaining the ferrum Carbon composites of primary, obtains parcel ferrosilicon Carbon composites by liquid deposition;The magnetic active carbon of containing metal iron is prepared at 600~640 DEG C of reduction 1-3h.Utilizing magnetic active carbon prepared by the method, grain diameter is little, and in the blood vessel around tumor tissues, permeability is strengthened, hence it is evident that improve its curative effect as medicine.But utilize magnetic active carbon adsorptive value prepared by the method extremely low, and the addition of ferroso-ferric oxide is also very big.
The method of magnetic active carbon processed can not solve the problem of stability and adsorptivity and complex manufacturing simultaneously at present;These problems limit activated carbon and are more widely applied, and reclaiming of activated carbon and the research utilized also are needed further reinforcement.
Summary of the invention
It is an object of the invention to provide one to be not easily blocked, specific surface area is big, and magnetic property is strong, activation, magnetization and preparation method that three processes of carbonization merge, the regulatable magnetic active carbon of pore structure and the magnetic active carbon prepared by the method.The method can substantially reduce the preparation cost of magnetic active carbon, promotes the application of activated carbon, contributes to the development of environmental protection cause.
The present invention is achieved through the following technical solutions:
A kind of method being prepared magnetic active carbon by abandoned biomass, including following preparation process:
1) it is placed in liquor zinci chloridi by the abandoned biomass through including washing, dry, broken, screening early stage processes impregnation process;The abandoned biomass obtaining having impregnated is standby;
Described abandoned biomass is preferably agricultural waste material, timber or timber waste;
2) at Fe3O4The surface of granule obtains required Magnetic reagent after adsorbing lauric acid and dodecyl sodium sulfate two layers of surface activating agent successively from inside to outside;
3) by the described abandoned biomass impregnated and described Magnetic reagent mix homogeneously, dry, obtain article shaped;
4) described article shaped being cracked under inert gas shielding, cracking final temperature is 400-500 DEG C;Product, through washing, drying, obtains product magnetic active carbon.
Wherein,
1st) in step, it is preferable that be that 1:1-1:4 impregnates according to the mass ratio of zinc chloride in abandoned biomass and liquor zinci chloridi.
Dip time is preferably 12h-36h.
Preferably the 2nd) Fe in step3O4Quality be the 1st) 5%-10% of abandoned biomass quality in step.
2nd) lauric acid, dodecyl sodium sulfate and Fe in step3O4Mass ratio be both preferably 1:1-4:1.
2nd) the concrete preparation process of step Magnetic reagent is: by Fe3O4It is added to the water with lauric acid, in the basic conditions, water-bath 0.5-1h at 60-100 DEG C;Acid adding, to pH=4~5, is collected and has been adsorbed one layer of lauric Fe3O4Granule, after washing, then adds dodecyl sodium sulfate and water, water-bath 0.5-2h at 50-70 DEG C, prepares Magnetic reagent.
Described alkali condition can drip 3-6mol/LNaOH solution and realize, and described washing should be washed to pH=7 and be advisable.
Lauric acid, dodecyl sodium sulfate and Fe3O4Mass ratio be both preferably 1:1-4:1.
4th) heating rate when cracking in step is preferably 5-10 DEG C/min, and temperature retention time is preferably 0.5-2h.
And by magnetic active carbon prepared by said method.
Currently preferred preparation method is as follows:
1. wood material is washed, dry, broken, screening, dried again, be placed in liquor zinci chloridi dipping 20-30h in the ratio that raw material and zinc chloride mass ratio are 1:2;
2. with Fe3O4For magnetic additive, first by Fe3O4It is added to the water with lauric acid, drips 3-6mol/LNaOH solution to making solution alkaline, water-bath 0.5-1h at 60-100 DEG C;It is added thereto to dilute hydrochloric acid to pH=4~5, collects and adsorbed one layer of lauric Fe3O4Granule, is washed to pH=7, then adds dodecyl sodium sulfate and water, water-bath 0.5-2h at 50-70 DEG C, prepares Magnetic reagent.
3. the cedar sawdust impregnated is mixed with the Magnetic reagent prepared, stir, put in baking oven dry.
4. dried article shaped being cracked under argon shield, cracking final temperature is 400-500 DEG C, and heating rate is 5-10 DEG C/min, and temperature retention time is 0.5-2h.Product, through washing, dry, grinding, obtains product magnetic active carbon.
The wood material that heretofore described abandoned biomass adopts is preferably cedar sawdust.
In experimentation, inventor have found that if by Fe3O4Directly mix with the cedar sawdust impregnated, dry, heat up after cracking, the product obtained is dipped in water, then this water can present dispersed particle and the Fe of crimson color3O4, this phenomenon shows, Fe3O4Separate with cedar sawdust.Inventor, by constantly experiment and exploration discovery, by adding surfactant, utilizes surfactant by Fe3O4Loading to cedar sawdust, after the cracking that heats up, when being dipped in water by the product obtained, water is clarification, and Fe is described3O4With wood flour already in connection with.
The beneficial effect of the invention
Compared with prior art, preparation technology of the present invention is simple, will activate, magnetize and three processes combinations of carbonization, it is achieved a step prepares magnetic active carbon;Simultaneously, it is possible to regulate the pore structure of magnetic active carbon by controlling the consumption of magnetic additive, the various products needed are obtained.It addition, the activation temperature of this preparation process is low, energy consumption is low, and preparation process clean environment firendly;The cheaper starting materials that the present invention uses is easy to get, and reduces the production cost of magnetic active carbon, the recovery to activated carbon, it is to avoid cause secondary pollution to be significant.The magnetic active carbon prepared by the present invention has high specific surface area, good absorption property, enough magnetic intensities 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 carbon;
As shown in Figure 2, Fe3O4When addition is 10%, occur in that Fe3O4Six diffraction maximums, respectively (220), (311), (400), (422), (511), (440).In collection of illustrative plates, have also appeared three new peaks, wherein 2 θ=27.042 ° are probably Fe3O4The peak of hydrolyzate FeOOH, 2 θ=28.70 ° and 2 θ=47.59 ° are probably ZnCl2The peak of hydrolyzate 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 that SEM figure, figure are amplification 500 times of 100 times;
In Fig. 4, Fig. 4 a-c is the SEM figure of embodiment 2 gained magnetic active carbon, and wherein Fig. 4 a is the SEM figure of amplification 100 times, and Fig. 4 b, Fig. 4 c are the SEM figure of amplification 1000 times;
Being compared can be obtained by Fig. 3 a-b and 4a-c, when magnetic additive is 0%, activated carbon surface is smooth, it does not have loaded article exists;And magnetic additive is when being 10%, there is one layer of uniform loaded article on its surface, in conjunction with XRD testing result, can show that the activated carbon prepared by the method is 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 Fe3O4The increase of addition, also increases as than saturated magnetic intensity, all has certain coercivity and remanent magnetism, and the initial susceptibility of embodiment 1 and embodiment 2 all reaches needed for magnetic separation.
Fig. 6 a-b respectively comparative example 1, the nitrogen adsorption figure of embodiment 1-2 gained magnetic active carbon and graph of pore diameter distribution.
It will be appreciated from fig. 6 that specific surface area is along with Fe3O4The increase of addition and reduce, mesoporous and aperture are at Fe3O4Addition is maximum when being 6%.
The a-g figure of Fig. 7 is embodiments of the invention 1Fe3O4On be adsorbed with the preparation process figure of the Magnetic reagent after lauric acid and dodecyl sodium sulfate two layers of surface activating agent successively.Wherein 7a is ferroso-ferric oxide and lauric acid is added to the water, and not being heated water-bath, ferroso-ferric oxide and lauric acid is separate, and upper strata is lauric acid, and beaker bottom is ferroso-ferric oxide;7b is after adding sodium hydroxide, together with ferroso-ferric oxide is set in lauric acid;7c is after 90 DEG C of water-bath 1h, and substantially, bottom is for having adsorbed lauric ferroso-ferric oxide in layering;7d is for after adding dilute hydrochloric acid, and cohesion occurs in ferroso-ferric oxide;7e is for, after washing, adding dodecyl sodium sulfate, and in thick, dodecyl sodium sulfate is insoluble;7f is after 60 DEG C of water-baths, and dodecyl sodium sulfate dissolves;7g is for after adding cedar sawdust, and cedar sawdust and Magnetic reagent are uniformly distributed.
Specific embodiment
Comparative example 1
Weighing 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is hydrolyzed preventing zinc chloride.Weighing 5g cedar sawdust, cedar sawdust impregnates 24h in liquor zinci chloridi, wherein, the mass ratio of wood flour and zinc chloride is 1:2, dries 24h.Weigh the sample after drying and be put in reacting furnace, argon shield, crack under 450 DEG C of final temperatures, 5 DEG C/min of heating rate, the magnetic active carbon of preparation when insulation 1h, BET specific surface area is 1307.64m after tested2/ g, total pore volume is 0.749cm3/ g, iodine sorption value is 814mg/g, and methylene blue adsorption value is 200mg/g, the saturated magnetic intensity 0.63856emu/g of ratio, and coercivity is 95.20Oe, and remanent magnetism is 0.05861emu/g.
Wherein, the specific surface area of activated carbon and pore-size distribution Quadrasorb automatic absorbing instrument measure (N2 adsorption when 77.35K).The specific surface area of activated carbon is calculated according to Brunauer-Emmett-Teller (BET) equation;Mesopore pore volume according to Density-Functional-Theory, (applied many by DFT, density functional method at present in the world by the method and HK method.) Equation for Calculating;Pore-size distribution is according to Barrett, JoynerandHalenda(BJH) model calculating.(following example measure by same method)
Embodiment 1
Weighing 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is hydrolyzed preventing zinc chloride.Weighing 5g cedar sawdust, cedar sawdust impregnates 24h in liquor zinci chloridi, wherein, the mass ratio of wood flour and zinc chloride is 1:2, weighs 0.3gFe3O4, and 0.3g lauric acid, first by Fe3O4Add in 15mL water with lauric acid, add 2mL5mol/LNaOH solution, water-bath 0.5h at 90 DEG C;It is added thereto to dilute hydrochloric acid to pH=4~5, collects and adsorbed one layer of lauric Fe3O4Granule, is washed to pH=7, then adds 0.6g dodecyl sodium sulfate and 20mL water, water-bath 1h at 60 DEG C, prepares Magnetic reagent.The cedar sawdust impregnated is mixed with Magnetic reagent, stirs, dry.Weigh the sample after drying and be put in reacting furnace, argon shield, crack under 450 DEG C of final temperatures, 5 DEG C/min of heating rate, the magnetic active carbon of preparation when insulation 1h, BET specific surface area is 896.07m after tested2/ g, total pore volume is 0.567cm3/ g, iodine sorption value is 817.98mg/g, and methylene blue adsorption value is 266mg/g, the saturated magnetic intensity 1.548emu/g of ratio, and coercivity is 77.72Oe, and remanent magnetism is 0.123emu/g, and initial susceptibility is 1.752 × 10-5。
Embodiment 2
Weighing 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is hydrolyzed preventing zinc chloride.Weighing 5g cedar sawdust, cedar sawdust impregnates 24h in liquor zinci chloridi, wherein, the mass ratio of wood flour and zinc chloride is 1:2, weighs 0.5gFe3O4, and 1.0g lauric acid, first by Fe3O4Add in 15mL water with lauric acid, add 2mL5mol/LNaOH solution, water-bath 0.5h at 90 DEG C;It is added thereto to dilute hydrochloric acid to pH=4~5, collects and adsorbed one layer of lauric Fe3O4Granule, is washed to pH=7, then adds 1.0g dodecyl sodium sulfate and 20mL water, water-bath 1h at 60 DEG C, prepares Magnetic reagent.The cedar sawdust impregnated is mixed with Magnetic reagent, stirs, dry.Weigh the sample after drying and be put in reacting furnace, argon shield, crack under 450 DEG C of final temperatures, 5 DEG C/min of heating rate, the magnetic active carbon of preparation when insulation 1h, BET specific surface area is 774.28m after tested2/ 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, the saturated magnetic intensity 8.881emu/g of ratio, and coercivity is 97.25Oe, and remanent magnetism is 0.851emu/g, and initial susceptibility is 9.306 × 10-5。
Embodiment 3
Weighing 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is hydrolyzed preventing zinc chloride.Weighing 5g cedar sawdust, cedar sawdust impregnates 24h in liquor zinci chloridi, wherein, the mass ratio of wood flour and zinc chloride is 1:2, weighs 0.5gFe3O4, and 1.0g lauric acid, first by Fe3O4Add in 15mL water with lauric acid, add 2mL5mol/LNaOH solution, water-bath 0.5h at 90 DEG C;It is added thereto to dilute hydrochloric acid to pH=4~5, collects and adsorbed one layer of lauric Fe3O4Granule, is washed to pH=7, then adds 1.0g dodecyl sodium sulfate and 20mL water, water-bath 1h at 60 DEG C, prepares Magnetic reagent.The cedar sawdust impregnated is mixed with Magnetic reagent, stirs, dry.Weigh the sample after drying and be put in reacting furnace, argon shield, crack under 400 DEG C of final temperatures, 5 DEG C/min of heating rate, the magnetic active carbon of preparation when insulation 1h, BET specific surface area is 112.753m after tested2/ g, total pore volume is 0.594cm3/ g, iodine sorption value is 756.77mg/g, and methylene blue adsorption value is 324.23mg/g, the saturated magnetic intensity 2.567emu/g of ratio, and coercivity is 38.29Oe, and remanent magnetism is 0.139emu/g, and initial susceptibility is 3.143 × 10-5。
Embodiment 4
Weighing 10g zinc chloride, add 40mL water, 2mL concentrated hydrochloric acid is hydrolyzed preventing zinc chloride.Weigh 5g cedar sawdust, cedar sawdust is impregnated in liquor zinci chloridi 24h;Wherein, the mass ratio of wood flour and zinc chloride is 1:2, weighs 0.5gFe3O4, and 1.0g lauric acid, first by Fe3O4Add in 15mL water with lauric acid, add 2mL5mol/LNaOH solution, water-bath 0.5h at 90 DEG C;It is added thereto to dilute hydrochloric acid to pH=4~5, collects and adsorbed one layer of lauric Fe3O4Granule, is washed to pH=7, then adds 1.0g dodecyl sodium sulfate and 20mL water, water-bath 1h at 60 DEG C, prepares Magnetic reagent.The cedar sawdust impregnated is mixed with Magnetic reagent, stirs, dry.Weigh the sample after drying and be put in reacting furnace, argon shield, crack under 500 DEG C of final temperatures, 5 DEG C/min of heating rate, the magnetic active carbon of preparation when insulation 1h, BET specific surface area is 1818.143m after tested2/ g, total pore volume is 1.026cm3/ g, iodine sorption value is 926.61mg/g, and methylene blue adsorption value is 327.51mg/g, the saturated magnetic intensity 2.217emu/g of ratio, and coercivity is 6.17Oe, and remanent magnetism is 0.0145emu/g, and initial susceptibility is 5.389 × 10-5。
Claims (6)
1. the method being prepared magnetic active carbon by abandoned biomass, it is characterised in that comprise the following steps:
1) being placed in liquor zinci chloridi by the abandoned biomass through including washing, dry, broken, screening early stage processes impregnation process, the abandoned biomass obtaining having impregnated is standby;
Wherein, described abandoned biomass is timber waste;
2) at Fe3O4The surface of granule obtains required Magnetic reagent after adsorbing lauric acid and dodecyl sodium sulfate two layers of surface activating agent successively from inside to outside;
3) by the described 1st) abandoned biomass and the 2nd that impregnated of step) Magnetic reagent mix homogeneously described in step, dry, obtain article shaped;
4) described article shaped being cracked under inert gas shielding, cracking final temperature is 400-500 DEG C, by pyrolysis product through washing, drying, obtains product magnetic active carbon;
2nd) Fe in step3O4Quality be the 1st) 5%-10% of the quality of abandoned biomass in step;
2nd) lauric acid and Fe in step3O4Mass ratio, dodecyl sodium sulfate and Fe3O4Mass ratio be 1:1-4:1;
The preparation process of described Magnetic reagent is: by Fe3O4It is added to the water with lauric acid, at alkali condition, water-bath 0.5-1h at 60-100 DEG C;Acid adding, to pH=4~5, is collected and has been adsorbed with lauric Fe wherein again3O4Granule, after washing, adds dodecyl sodium sulfate and water, water-bath 0.5-2h at 50-70 DEG C, prepares.
2. method according to claim 1, it is characterised in that the 1st) step is that 1:1~4 impregnate according to abandoned biomass with the mass ratio of zinc chloride in liquor zinci chloridi.
3. method according to claim 2, it is characterised in that the 1st) dip time is 24h-30h in step.
4. method according to claim 1, it is characterised in that the 2nd) Fe in step3O4Quality be the 1st) in step the 6% or 10% of abandoned biomass.
5. method according to claim 1, it is characterised in that the 4th) heating rate when cracking in step is 5-10 DEG C/min, temperature retention time is 0.5-2h.
6. the magnetic active carbon that prepared by the method described in any one of claim 1-5.
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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 |
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 |
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