CN105536703A - Preparation method for magnetic biological carbon by one-step synthesis - Google Patents
Preparation method for magnetic biological carbon by one-step synthesis Download PDFInfo
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- CN105536703A CN105536703A CN201510995847.2A CN201510995847A CN105536703A CN 105536703 A CN105536703 A CN 105536703A CN 201510995847 A CN201510995847 A CN 201510995847A CN 105536703 A CN105536703 A CN 105536703A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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Abstract
The invention discloses a preparation method for magnetic biological carbon by one-step synthesis. The preparation method comprises the following steps: air-drying a biomass raw material under a natural condition and then storing for later use, and adding a dried and crushed biomass raw material into a ferric salt solution; slowly stirring a mixed solution, then, regulating a pH (potential of hydrogen) value with an NaOH solution, then, continuously stirring, then, standing until the biomass raw material absorbs the ferric salt solution to reach a saturation state, performing suction filtration to remove free water in the biomass raw material, pyrolyzing a suction filtration-treated biomass raw material in a pyrolyzing furnace to make carbon, and introducing an inert shielding gas into the pyrolyzing furnace to obtain the magnetic biological carbon. According to the preparation method disclosed by the invention, carbonization and magnetization are combined together to synthetize the magnetic biological carbon by one-step pyrolysis; meanwhile, different magnetic biological carbon materials can be obtained by changing the shielding gas (nitrogen or carbon dioxide); an effect of removing typical heavy metal pollutants in a water body is obvious, and moreover, the typical heavy metal pollutants can be separated and recovered from the water body as well so as to protect the environment from secondary pollution.
Description
Technical field
The present invention relates to heavy metal pollution control field.Be specifically related to a kind of preparation method of one-step synthesis magnetic bio charcoal.Be applicable to agricultural wastes resource secondary utilize.
Background technology
Due to a large amount of containing heavy metal containing sewage discharge in the industrial activity such as exploitation of mineral resources, smelting, water, native environmental pollution are day by day serious, greatly threaten health, and the water body that therefore heavy metal is polluted effectively repairs the focus having become China's prevention and cure of pollution.Charcoal causes extensive concern as a class novel environmental functional material, charcoal raw material sources are extensive, and there is larger porosity and specific area, the structure of height aromatization, containing advantages such as a large amount of phenolic hydroxyl group, carboxyl and carbonyls, charcoal heavy metal is made to have good absorption and stabilization.But the Collection and utilization after charcoal uses is that charcoal utilizes field to need solution difficult problem, and magnetic method is a kind of new recovery method found at present, successfully solves the recycle and reuse problem of the charcoal after absorption.But the method for magnetic bio charcoal synthesis at present completes in two steps, and the first step is that agriculture waste living beings are made common charcoal; Charcoal is synthesized the magnetic charcoal of tool by second step more again, and its preparation process complexity is time-consuming as seen, and cost is also relatively high.In order to reduce preparation cost, the present invention is by merging pyrolysis charring and magnetization two processes, pyrolysis preparation is carried out in biomass pyrolysis furnace, the novel magnetic charcoal synthesized by this kind of method not only reduces preparation cost, and effectively can remove Heavy Metals in Waters, finally can also realize separation and recovery.
Summary of the invention
The object of the invention is, for the problems referred to above existed at present, to provide a kind of preparation method of one-step synthesis magnetic bio charcoal.In order to the loaded down with trivial details cost of technique overcoming at present synthesizing magnetic charcoal is in two steps relatively high, take pyrolysis charring process and magnetic history to merge, one-step synthesis magnetic bio charcoal.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
Deposit for subsequent use after natural conditions are air-dry by living beings raw material, living beings raw material are crushed into and are about 2 ~ 4cm, are joined by the living beings raw material after dry fragmentation and comprise Fe
2+and Fe
3+iron salt solutions in, in iron salt solutions, Fe
2 +molar concentration be 0.4 ~ 0.6mol/L, Fe
3+molar concentration be 0.04 ~ 0.06mol/L, obtain mixed liquor after living beings raw material are added iron salt solutions, living beings raw material are 0.03 ~ 0.05% at the weight percentage of mixed liquor;
Iron salt solutions is mixed by divalent iron salt solution and ferric salt solution,
Divalent iron salt solution obtains by with under type: by FeSO
4be dissolved in deionized water.
Ferric salt solution obtains by with under type: by Fe
2(SO
4)
3-nH
2o is dissolved in deionized water.
Divalent iron salt solution and ferric salt solution mixing are obtained iron salt solutions.
Mixed liquor is slowly stirred 0.5 ~ 1h at 25 ~ 30 DEG C, then pH value to 10 ~ 11 of mixed liquor are regulated by the NaOH solution of 10mol/L, the mixed liquor regulating pH value continues stirring 0.5 ~ 1h, 1 ~ 2h is placed afterwards, the state until biomass material absorption iron salt solutions reaches capacity under 25 ~ 30 DEG C of temperature conditions.
By vacuumfilter, suction filtration is carried out to mixed liquor; Free water in filtering process living beings raw material; by the pyrolysis charcoal processing in pyrolysis oven of the living beings raw material after suction filtration process; inert protective gas is passed in pyrolysis oven; in pyrolysis oven, heating rate is 20 ~ 30 DEG C/min, pyrolysis temperature is 400 ~ 500 DEG C, pyrolysis time is 40 ~ 50min, obtains magnetic bio charcoal.
Its manufacturing process is as shown in Fig. 1 process.Wherein at CO
2under atmosphere, pyrolysis temperature is that 400 DEG C of magnetic bio charcoals prepared are labeled as MC400; At N
2under atmosphere, pyrolysis temperature is that 400 DEG C of magnetic bio charcoals prepared are labeled as MN400.
Described living beings raw material are all kinds of stalk materials such as rice straw.
Described inert protective gas is nitrogen or carbon dioxide.
Described one-step synthesis magnetic bio Carbon Materials is for removing representative heavy metal pollutant in water body, and representative heavy metal pollutant comprises lead, cadmium, mercury, chromium, copper, zinc etc.
Described magnetic magnetic bio charcoal add quality and sewage volume ratio is 1:500g/mL to 1:2000g/mL.
The present invention compared with prior art has following beneficial effect:
Compared with existing charcoal technology of preparing, preparation technology of the present invention is simple, charing and magnetization two processes is united two into one, realizes a step pyrolysis synthesizing magnetic biological carbon materials; By changing protective gas (nitrogen or carbon dioxide), different magnetic bio Carbon Materials can be obtained simultaneously; In addition, by the magnetic bio charcoal of pyrolysis one-step synthesis method, remove typical heavy metal contaminants (as heavy metal cadmium etc.) Be very effective in water body, and separation and recovery from water body can be realized equally, avoid causing secondary pollution to environment.Therefore, the preparation method of pyrolysis one-step synthesis magnetic bio charcoal, not only reaches the excellent results of magnetic bio charcoal, and this preparation method prepares charcoal than traditional first pyrolysis, and then regulates and controls the two-step method that charcoal gives magnetic, and technique simplifies conveniently greatly.
Accompanying drawing explanation
Fig. 1 is the process chart of the inventive method;
The scanning electron microscope (SEM) photograph of the magnetic bio charcoal MC400 that Fig. 2 (a) obtains for embodiment during amplification 2500 times 1, the scanning electron microscope (SEM) photograph of the magnetic bio charcoal MN400 that Fig. 2 (b) obtains for embodiment during amplification 5000 times 2, and Fig. 2 (a ') for rice straw during amplification 5000 times is at CO
2the scanning electron microscope (SEM) photograph of the charcoal BC400 adopting conventional two-step method to obtain under atmosphere, and Fig. 2 (b ') for rice straw during amplification 5000 times is at N
2the scanning electron microscope (SEM) photograph of the charcoal BN400 adopting conventional two-step method to obtain under atmosphere;
Fig. 3 is the hysteresis curve figure of magnetic bio charcoal prepared by the embodiment of the present invention 1 and embodiment 2;
Fig. 4 is the comparative effectiveness figure that the embodiment of the present invention 1 carbon dioxide atmosphere magnetic charcoal and standard biologic charcoal remove Heavy Metals in Waters cadmium.
Fig. 5 is the comparative effectiveness figure that the embodiment of the present invention 2 nitrogen atmosphere magnetic charcoal and standard biologic charcoal remove Heavy Metals in Waters cadmium.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is described further.
Embodiment 1:
Deposit for subsequent use after natural conditions are air-dry by living beings raw material, living beings raw material are crushed into and are about 2cm, are joined by the living beings raw material after dry fragmentation and comprise Fe
2+and Fe
3+iron salt solutions in, in iron salt solutions, Fe
2+molar concentration be 0.4mol/L, Fe
3+molar concentration be 0.04mol/L, obtain mixed liquor after living beings raw material are added iron salt solutions, living beings raw material are 0.03% at the weight percentage of mixed liquor.
Iron salt solutions is mixed by divalent iron salt solution and ferric salt solution,
Divalent iron salt solution obtains by with under type: by FeSO
4be dissolved in deionized water.
Ferric salt solution obtains by with under type: by Fe
2(SO
4)
3-nH
2o is dissolved in deionized water.
Divalent iron salt solution and ferric salt solution mixing are obtained iron salt solutions.
Mixed liquor is slowly stirred 0.5h at 25 DEG C, then the pH value to 10 of mixed liquor is regulated by the NaOH solution of 10mol/L, the mixed liquor regulating pH value continues to stir 0.5h, places 1h afterwards under 25 DEG C of temperature conditions, the state until biomass material absorption iron salt solutions reaches capacity.
Carry out suction filtration followed by vacuumfilter to mixed liquor, Free water in filtering process artifact matter raw material, by the pyrolysis charcoal processing in pyrolysis oven of the living beings raw material after suction filtration process, passes into CO in pyrolysis oven
2for protective gas, in pyrolysis oven, heating rate is 20 DEG C/min, pyrolysis temperature is 400 DEG C, pyrolysis time is 40min, obtains the magnetic bio charcoal of this embodiment.
The raw material selected in the present embodiment are rice straw.
The magnetic bio charcoal prepared in the present embodiment is labeled as MC400.
Embodiment 2:
Deposit for subsequent use after natural conditions are air-dry by living beings raw material, living beings raw material are crushed into and are about 4cm, and the living beings raw material after just dry fragmentation join and comprise Fe
2+and Fe
3+iron salt solutions in, in iron salt solutions, Fe
2+molar concentration be 0.6mol/L, Fe
3+molar concentration be 0.06mol/L, obtain mixed liquor after living beings raw material are added iron salt solutions, living beings raw material are 0.05% at the weight percentage of mixed liquor.
Iron salt solutions is mixed by divalent iron salt solution and ferric salt solution,
Divalent iron salt solution obtains by with under type: by FeSO
4be dissolved in deionized water.
Ferric salt solution obtains by with under type: by Fe
2(SO
4)
3-nH
2o is dissolved in deionized water.
Divalent iron salt solution and ferric salt solution mixing are obtained iron salt solutions.
Mixed liquor is slowly stirred 1h at 30 DEG C, then the pH value to 11 of mixed liquor is regulated by the NaOH solution of 10mol/L, the mixed liquor regulating pH value continues to stir 1h, places 2h afterwards under 30 DEG C of temperature conditions, the state until biomass material absorption iron salt solutions reaches capacity.
Carry out suction filtration followed by vacuumfilter to mixed liquor, Free water in filtering process artifact matter raw material, by the pyrolysis charcoal processing in pyrolysis oven of the living beings raw material after suction filtration process, passes into CO in pyrolysis oven
2or N
2for protective gas, in pyrolysis oven, heating rate is 20 DEG C/min, pyrolysis temperature is 400 DEG C, pyrolysis time is 50min, obtains the magnetic bio charcoal of this embodiment,
Obtain magnetic bio charcoal in the present embodiment and be labeled as MN400.
Living beings raw material are rice straw in the present embodiment.
The scanning electron microscope (SEM) photograph of the magnetic bio charcoal MC400 that Fig. 2 (a) obtains for embodiment during amplification 2500 times 1, the scanning electron microscope (SEM) photograph of the magnetic bio charcoal MN400 that Fig. 2 (b) obtains for embodiment during amplification 5000 times 2, and Fig. 2 (a ') for rice straw during amplification 5000 times is at CO
2the scanning electron microscope (SEM) photograph of the charcoal BC400 adopting conventional two-step method to obtain under atmosphere, and Fig. 2 (b ') for rice straw during amplification 5000 times is at N
2the scanning electron microscope (SEM) photograph of the charcoal BN400 adopting conventional two-step method to obtain under atmosphere.It is surperficial by maghemite γ-Fe by MC400 and MN400 can be observed clearly in comparison diagram 2 (a) and Fig. 2 (a ') and Fig. 2 (b) and Fig. 2 (b ')
2o
3nano material covered, and find the maghemite γ-Fe on MN400 surface
2o
3the more crypto set covered, and the primitive organism charcoal BC400 that traditional approach obtains and BN400 smooth surface and pore structure is pure and fresh complete.
Strong and weak in order to judge the magnetic of magnetic bio charcoal prepared by one-step synthesis method, the hysteresis curve having done the magnetic bio charcoal under two kinds of atmosphere is shown in Fig. 3, and magnetic bio charcoal can well be attracted separation and recovery from water body by magnet simultaneously.When applied field strengths is 6000Oe, the magnetic saturation intensity of MN400 sample is 10.93emu/g; And the magnetic saturation intensity of MC400 sample is 8.72emu/g.Therefore, the magnetic bio charcoal magnetic prepared of the present invention is better.
0.25g magnetic bio charcoal MC400 obtained for embodiment 1 is put in 50mL tool plug bottle, adds heavy metal Cd (II) solution of 50mL different quality concentration (5-500mg/L), containing 0.01mol/LNaNO in the mixed solution in tool plug bottle
3electrolyte as a setting, and regulate mixed solution pH to 6.0 ± 0.05 in tool plug bottle, the mixed solution in tool plug bottle, at normal temperature 25-30 DEG C, after the speed of 200 turns/min shakes 48 hours on shaking table, sampled 0.22 μm of water system filter membrane, the heavy metal Cd of filtrate
2+concentration Flame Atomic Absorption Spectrometry Determination, calculates the adsorbance of cadmium ion in table 1.
Table 1 magnetic bio charcoal MC400 is to the test result of cadmium sorption amount
As shown in Table 1, the initial concentration along with cadmium-ion solution becomes large gradually, and the adsorbance of magnetic bio charcoal MC400 and MN400 finally reaches capacity and tends towards stability.
0.25g magnetic bio charcoal MN400 obtained for embodiment 2 is put in 50mL tool plug bottle, adds heavy metal Cd (II) solution of 50mL different quality concentration (5-500mg/L), containing 0.01mol/LNaNO in the mixed solution in tool plug bottle
3electrolyte as a setting, and regulate mixed solution pH to 6.0 ± 0.05 in tool plug bottle, the mixed solution in tool plug bottle, at normal temperature 25-30 DEG C, after the speed of 200 turns/min shakes 48 hours on shaking table, sampled 0.22 μm of water system filter membrane, the heavy metal Cd of filtrate
2+concentration Flame Atomic Absorption Spectrometry Determination, calculates the adsorbance of cadmium ion in table 2.
Table 2 magnetic bio charcoal MN400 is to the test result of cadmium sorption amount
As shown in Table 2, the initial concentration along with cadmium-ion solution becomes large gradually, and the adsorbance of magnetic bio charcoal MN400 finally reaches capacity and tends towards stability.
In addition, the charcoal sample of 0.1g magnetic bio charcoal MC400 obtained under carbon dioxide atmosphere in embodiment 1 and conventional preparation is also put in 50mL tool plug bottle by respectively, adds the heavy metal Cd of 20mg/L
2+solution, containing 0.01mol/LNaNO in the mixed solution in tool plug bottle
3electrolyte as a setting, and regulate mixed solution pH to 6.0 ± 0.05 in tool plug bottle, the mixed solution in tool plug bottle is normal temperature 25 DEG C, and the speed of 200 turns/min shakes 48 hours, after 48h on shaking table, samples 0.22 μm of water system filter membrane, the heavy metal Cd of filtrate
2+concentration Flame Atomic Absorption Spectrometry Determination, compare magnetic bio charcoal and standard biologic charcoal Heavy Metals in Waters Cd clearance prepared by one-step method, its heavy metal Cd removal effect is shown in Fig. 4.
The charcoal sample of 0.1g magnetic bio charcoal MN400 obtained in a nitrogen atmosphere in embodiment 2 and conventional preparation is put into respectively in 50mL tool plug bottle, adds the heavy metal Cd of 20mg/L
2+solution, containing 0.01mol/LNaNO in the mixed solution in tool plug bottle
3electrolyte as a setting, and regulate mixed solution pH to 6.0 ± 0.05 in tool plug bottle, the mixed solution in tool plug bottle is normal temperature 25 DEG C, and the speed of 200 turns/min shakes 48 hours, after 48h on shaking table, samples 0.22 μm of water system filter membrane, the heavy metal Cd of filtrate
2+concentration Flame Atomic Absorption Spectrometry Determination, compare magnetic bio charcoal and standard biologic charcoal Heavy Metals in Waters Cd clearance prepared by one-step method, its heavy metal Cd removal effect is shown in Fig. 5.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or optimize or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Claims (4)
1. a preparation method for one-step synthesis magnetic bio charcoal, is characterized in that, comprises the following steps:
Deposit for subsequent use after natural conditions are air-dry by living beings raw material, living beings raw material are crushed into and are about 2 ~ 4cm, are joined by the living beings raw material after dry fragmentation and comprise Fe
2+and Fe
3+iron salt solutions in, in iron salt solutions, Fe
2+molar concentration be 0.4 ~ 0.6mol/L, Fe
3+molar concentration be 0.04 ~ 0.06mol/L, obtain mixed liquor after living beings raw material are added iron salt solutions, living beings raw material are 0.03 ~ 0.05% at the weight percentage of mixed liquor;
Mixed liquor is slowly stirred 0.5 ~ 1h at 25 ~ 30 DEG C, then pH value to 10 ~ 11 of mixed liquor are regulated by the NaOH solution of 10mol/L, the mixed liquor regulating pH value continues stirring 0.5 ~ 1h, 1 ~ 2h is placed afterwards under 25 ~ 30 DEG C of temperature conditions, the state until biomass material absorption iron salt solutions reaches capacity
By vacuumfilter, suction filtration is carried out to mixed liquor; Free water in filtering process living beings raw material; by the pyrolysis charcoal processing in pyrolysis oven of the living beings raw material after suction filtration process; inert protective gas is passed in pyrolysis oven; in pyrolysis oven, heating rate is 20 ~ 30 DEG C/min, pyrolysis temperature is 400 ~ 500 DEG C, pyrolysis time is 40 ~ 50min, obtains magnetic bio charcoal.
2. the preparation method of a kind of one-step synthesis magnetic bio charcoal according to claim 1, it is characterized in that, described living beings raw material are rice straw.
3. the preparation method of a kind of one-step synthesis magnetic bio charcoal according to claim 1, it is characterized in that, described inert protective gas is nitrogen or carbon dioxide.
4. the preparation method of a kind of one-step synthesis magnetic bio charcoal according to claim 1, it is characterized in that, described iron salt solutions is obtained by following steps:
By FeSO
4be dissolved in deionized water and obtain divalent iron salt solution;
By Fe
2(SO
4)
3-nH
2o is dissolved in deionized water and obtains ferric salt solution;
Divalent iron salt solution and ferric salt solution mixing are obtained iron salt solutions.
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