CN103551113A - Preparation method of rice-hull-based carbon-supported ferroferric oxide nanoparticle (RC-Fe3O4) and method for treating lead-contained wastewater by using RC-Fe3O4 - Google Patents
Preparation method of rice-hull-based carbon-supported ferroferric oxide nanoparticle (RC-Fe3O4) and method for treating lead-contained wastewater by using RC-Fe3O4 Download PDFInfo
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- CN103551113A CN103551113A CN201310580963.9A CN201310580963A CN103551113A CN 103551113 A CN103551113 A CN 103551113A CN 201310580963 A CN201310580963 A CN 201310580963A CN 103551113 A CN103551113 A CN 103551113A
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Abstract
The invention discloses a preparation method of a rice-hull-based carbon-supported ferroferric oxide nanoparticle (RC-Fe3O4) and a method for treating lead-contained wastewater by using the RC-Fe3O4. RC-Fe3O4 powder is prepared by taking rice hulls and ferric salt as raw materials by using an impregnation and carbon thermal method with simple processes to absorb heavy metal lead ions in the wastewater. By using the material, a great number of lead ions in the wastewater can be adsorbed and can be separated under the action of an external magnetic field, so that the aims of efficiently removing the lead ions and purifying the wastewater are achieved, the removal rate of the metal ions can be up to 97%, and the RC-Fe3O4 material can be regenerated and reused.
Description
Technical field
The present invention relates to a kind of rice husk base charcoal loaded with nano ferriferrous oxide particles (RC-Fe
3o
4) preparation and with it, process the method for lead waste water, particular content is raw material for take rice husk and molysite, employing process simply flood-carbon hot preparation legal system obtains RC-Fe
3o
4powder, the heavy metal lead ion in absorption waste water.
Background technology
Heavy metal is a class noxious material that causes environmental pollution.China is the large mining powers in third place in the world, and the processes such as the exploitation of mineral products, smelting and processing have been brought a large amount of heavy metals into environment.Lead and compound thereof are the very large environmental contaminants of a class toxicity, and main infringement bone, hemopoietic system and nervous system after being absorbed by the body, cause anaemia, peripheral nerve inflammation, also can flow into brain tissue with blood, disturbs metabolic activity, causes brain damage.Once the most fearful harm of lead contamination is that it enters water body or soil, is just difficult to remove and even causes permanent pollution.Therefore, lead waste water is effectively treated as in environmental improvement to more and more distinct issues.At present, the processing method of lead waste water mainly contains chemical precipitation method, ion-exchange, hyperfiltration, electrolysis, membrane separation process etc.And absorption method is one of processing method of tool prospect.
Since fullerene and CNT are found, worldwide just started the research boom of material with carbon element.Material with carbon element, with advantages such as its stable chemical property, unique physics and electromagnetic properties, is widely used in the fields such as chemical industry, machinery, metallurgy, electronics, environmental protection.Yet along with we constantly increase the demand of the energy, the supply growing tension of fossil fuel, has caused considerable restraint to the development of material with carbon element and application, thereby supplementing and substituting in the urgent need to other energy.Living beings are unique reproducible carbon sources, and source is abundant, price is cheap, becomes the optimal selection that replaces petrochemical industry carbon source to prepare material with carbon element.Wherein, utilizing agricultural wastes biomass-making is a kind ofly both can reduce environmental pollution for active carbon, can widen again the new model of energy access.China is Rice Cropping big country, and current total output occupies first place in the world.Rice husk is the main byproduct in rice process, and the annual rice husk output of China can reach tens million of tons.The main component of rice husk is cellulose, hemicellulose, lignin and a small amount of mineral salt, and essential element is carbon, hydrogen, oxygen, silicon, and phosphorus content is high, is very good active carbon raw materials.
Active carbon is owing to having larger specific area, can be in its surface or duct load various metals or nonmetal, to prepare new function composite.This composite can be taken into account the advantage of every kind of material simultaneously, and the performance of material is optimized.The composite that active carbon and metal composite obtain is usually used in the preparation of adsorbent in environmental pollution reparation field or catalyst.This method can improve the reason of charcoal absorption, utilizes metallic to have good binding ability to some pollutant (comprising lead) on the one hand; To utilize homodisperse metallic can effectively increase the site that contacts of composite and pollutant on the other hand.
Summary of the invention
The object of the invention is to provide a kind of preparation method of rice husk base charcoal loaded with nano ferriferrous oxide particles and utilizes it to process the method for lead waste water, nano ferriferrous oxide granule in the prepared rice husk base charcoal loaded with nano ferriferrous oxide particles of the present invention is disperseed and difficult drop-off, be stored under normal temperature and pressure, and high to plumbous adsorption rate.
For achieving the above object, the preparation method of rice husk base charcoal loaded with nano ferriferrous oxide particles of the present invention, comprises the following steps:
(A) by pure water rinsing 3-5 time for rice husk, dry 24 hours for 105 ℃, pulverized 80 mesh sieves, obtain powdered rice hulls;
(B) FeCl that preparation molar concentration is 0.5～5mol/L
36H
2o solution, fully stirs until FeCl
36H
2o dissolves completely, obtains FeCl3 solution;
(C) by 1:5～20 mass volume ratio, powdered rice hulls is immersed to above-mentioned FeCl
3in solution, 50-70 ℃ is stirred 12 hours, and after centrifugation, 80-100 ℃ of oven dry, obtains the powdered rice hulls of dipping;
(D) powdered rice hulls that must flood is that the lasting nitrogen of 30-50mL/min flows down pyrolysis at flow velocity, heating schedule is: from room temperature, with 10-20 ℃/min, rise to 800 ℃, keep 60-120min, obtain rice husk base charcoal loaded with nano ferriferrous oxide particles after cooling, i.e. RC-Fe
3o
4material.
For reaching above-mentioned purpose, the present invention also provides a kind of method of utilizing above-mentioned rice husk base charcoal loaded with nano ferriferrous oxide particles to process lead waste water, and it comprises:
(A) in mass concentration, be in 1-1000mg/L lead waste water, to add rice husk base charcoal loaded with nano ferriferrous oxide particles, and to make its mass concentration in lead waste water be 0.1-2.0g/L;
(B) 60-120min that vibrates under the condition that is 250rmp by the mixed solution of step (A) gained in room temperature and rotating speed, can remove the lead ion in lead waste water.
The above-mentioned method of utilizing rice husk base charcoal loaded with nano tri-iron tetroxide to process lead waste water, also can be further by the rice husk base charcoal loaded with nano ferriferrous oxide particles magnet adsorption after step (B) is processed, after putting together, with after washed with de-ionized water, again drop into the processing of lead waste water.
Compared with the prior art, beneficial effect of the present invention is embodied in:
(1) the present invention's modified magnetic tri-iron tetroxide particle on rice husk, and can be applied to the processing of lead waste water, not only raw material is cheap and easy to get, reduced production cost, really realized " treatment of wastes with processes of wastes against one another ", and preparation process of the present invention is simple, is easy to operate and control, be convenient to produce in a large number.
(2) the rice husk base charcoal loaded with nano ferriferrous oxide particles surface area that the present invention uses is large, high adsorption capacity, and to plumbous obvious processing effect, can reach balance within a short period of time, and clearance is up to more than 90%.
(3) the rice husk base charcoal loaded with nano ferriferrous oxide particles that prepared by the present invention can effectively improve active carbon to plumbous adsorption capacity, and the material after absorption carries out Separation of Solid and Liquid by externally-applied magnetic field, not only absorption after material can through regeneration after reuse, realize the recycling of resource, and can effectively shorten the Separation of Solid and Liquid time after absorption, whole process is fast, efficiently.
Accompanying drawing explanation
Fig. 1 is RC-Fe
3o
4observation by light microscope result;
Fig. 2 is RC-Fe
3o
4tem observation result;
Fig. 3 is RC-Fe
3o
4xRD characterization result;
Fig. 4 is the kinetic curve that this method is removed lead ion in lead waste water, RC-Fe
3o
4addition is 0.1g, and lead ion mass concentration is 500mg/L.
The specific embodiment
Below in conjunction with example, further illustrate feasibility of the present invention and stability.
Example one:
(1) get appropriate pure water rinsing 3 times for 2g rice husk, dry 24 hours for 105 ℃, pulverized 80 mesh sieves, obtain powdered rice hulls; Take 5.4g FeCl
36H
2o joins in 20mL distilled water, and fully stirring and dissolving obtains 1mol/L FeCl
3solution; Then above-mentioned powdered rice hulls is immersed to FeCl
3in solution, 60 ℃ of 300r/min stir 12 hours, 80 ℃ of oven dry after centrifugation; Powdered rice hulls after dipping is ground, continue nitrogen flow down pyrolysis at 30mL/min, heating schedule is: from room temperature, with 10 ℃/min, rise to 800 ℃, keep 60min; Cooling rear taking-up in tube furnace, obtains rice husk base charcoal loaded with nano ferriferrous oxide particles, is also RC-Fe
3o
4particle.
(2) take the PVC bottle that 0.03g rice husk base charcoal loaded with nano tri-iron tetroxide is placed in 100mL, add the lead waste water that 100mL, lead ion mass concentration are 100mg/L.Cover tightly after bottle cap, sample bottle is placed in oscillator, in the lower 250 revs/min of vibrations of room temperature 60 minutes, then cross leaching filtrate and measure residual lead ion concentration, calculating clearance is 100%, RC-Fe
3o
4to the extracted amount of lead ion, be 333.3mg/g.By the RC-Fe after absorption
3o
4material puts together by externally-applied magnetic field, by deionized water, washes one time, again adds the lead waste water of 100mL, 100mg/L, repeats above-mentioned steps, and lead ion clearance is 95.3%.
Example two:
(1) get appropriate pure water rinsing 4 times for 2g rice husk, dry 24 hours for 105 ℃, pulverized 80 mesh sieves, obtain powdered rice hulls; Take 5.4g FeCl
36H
2o joins in 10mL distilled water, and fully stirring and dissolving obtains 2mol/L FeCl
3solution; Then above-mentioned powdered rice hulls is immersed to FeCl
3in solution, 50 ℃ of 300r/min stir 12 hours, 90 ℃ of oven dry after centrifugation; Powdered rice hulls after dipping is ground, continue nitrogen flow down pyrolysis at 40mL/min, heating schedule is: from room temperature, with 15 ℃/min, rise to 800 ℃, keep 60min; In tube furnace, cooling rear taking-up, obtains RC-Fe
3o
4particle.
(2) take 0.05g RC-Fe
3o
4be placed in the PVC bottle of 100mL, add the lead waste water that 100mL, lead ion mass concentration are 200mg/L.Cover tightly after bottle cap, sample bottle is placed in oscillator, in the lower 250 revs/min of vibrations of room temperature 80 minutes, then cross leaching filtrate and measure residual lead ion concentration, calculating clearance is 97%, RC-Fe
3o
4to the extracted amount of lead ion, be that 388mg/g(specific experiment result is referring to Fig. 4).
Example three:
(1) get appropriate pure water rinsing 5 times for 3g rice husk, dry 24 hours for 105 ℃, pulverized 80 mesh sieves, obtain powdered rice hulls; Take 10.8g FeCl
36H
2o joins in 40mL distilled water, and fully stirring and dissolving obtains 1mol/L FeCl
3solution; Then above-mentioned powdered rice hulls is immersed to FeCl
3in solution, 70 ℃ of 300r/min stir 12 hours, 100 ℃ of oven dry after centrifugation; Powdered rice hulls after dipping is ground, continue nitrogen flow down pyrolysis at 50mL/min, heating schedule is: from room temperature, with 20 ℃/min, rise to 800 ℃, keep 80min; In tube furnace, cooling rear taking-up, obtains RC-Fe
3o
4particle.
(2) take 0.1g RC-Fe
3o
4be placed in the PVC bottle of 100mL, add the simulation lead waste water that 100mL, lead ion mass concentration are 500mg/L.Cover tightly after bottle cap, sample bottle is placed in oscillator, in the lower 250 revs/min of vibrations of room temperature 90 minutes, then cross leaching filtrate and measure residual lead ion concentration, calculating clearance is 92.6%, RC-Fe
3o
4to the extracted amount of lead ion, be 463mg/g.
Example four:
(1) get appropriate pure water rinsing 3 times for 4g rice husk, dry 24 hours for 105 ℃, pulverized 80 mesh sieves, obtain powdered rice hulls; Take 20.25g FeCl
36H
2o joins in 50mL distilled water, and fully stirring and dissolving obtains 1.5mol/L FeCl
3solution; Then above-mentioned powdered rice hulls is immersed to FeCl
3in solution, 60 ℃ of 300r/min stir 12 hours, 80 ℃ of oven dry after centrifugation; Powdered rice hulls after dipping is ground, continue nitrogen flow down pyrolysis at 45mL/min, heating schedule is: from room temperature, with 10 ℃/min, rise to 800 ℃, keep 120min; In tube furnace, cooling rear taking-up, obtains RC-Fe
3o
4particle.
(2) take 0.15g RC-Fe
3o
4be placed in the PVC bottle of 100mL, add the simulation lead waste water that 100mL, lead ion mass concentration are 700mg/L.Cover tightly after bottle cap, sample bottle is placed in oscillator, in the lower 250 revs/min of vibrations of room temperature 120 minutes, then cross leaching filtrate and measure residual lead ion concentration, calculating clearance is 94.1%, RC-Fe
3o
4to the extracted amount of lead ion, be 439.1mg/g.Material after absorption is put together, by deionized water, wash one time, again add the simulation lead waste water of 100mL, 700mg/L, repeat above-mentioned steps, lead ion clearance is 85.2%.
Example five:
(1) get appropriate pure water rinsing 3 times for 2g rice husk, dry 24 hours for 105 ℃, pulverized 80 mesh sieves, obtain powdered rice hulls; Take 5.4g FeCl
36H
2o joins in 40mL distilled water, and fully stirring and dissolving obtains 0.5mol/L FeCl
3solution; Then above-mentioned powdered rice hulls is immersed to FeCl
3in solution, 70 ℃ of 300r/min stir 12 hours, 80 ℃ of oven dry after centrifugation; Powdered rice hulls after dipping is ground, continue nitrogen flow down pyrolysis at 30mL/min, heating schedule is: from room temperature, with 12 ℃/min, rise to 800 ℃, keep 60min; In tube furnace, cooling rear taking-up, obtains RC-Fe
3o
4particle.
(2) take 0.2g RC-Fe
3o
4be placed in the PVC bottle of 100mL, add the simulation lead waste water that 100mL, lead ion mass concentration are 1000mg/L.Cover tightly after bottle cap, sample bottle is placed in oscillator, in the lower 250 revs/min of vibrations of room temperature 70 minutes, then cross leaching filtrate and measure residual lead ion concentration, calculating clearance is 90.8%, RC-Fe
3o
4to the extracted amount of lead ion, be 454mg/g.
The present invention is not limited to above specific embodiment.
Claims (3)
1. a preparation method for rice husk base charcoal loaded with nano ferriferrous oxide particles, is characterized in that comprising the following steps:
(A) by pure water rinsing 3-5 time for rice husk, dry 24 hours for 105 ℃, pulverized 80 mesh sieves, obtain powdered rice hulls;
(B) FeCl that preparation molar concentration is 0.5～5mol/L
36H
2o solution, fully stirs until FeCl
36H
2o dissolves completely, obtains FeCl
3solution;
(C) by 1:5～20 mass volume ratio, powdered rice hulls is immersed to above-mentioned FeCl
3in solution, 50-70 ℃ is stirred 12 hours, and after centrifugation, 80-100 ℃ of oven dry, obtains the powdered rice hulls of dipping;
(D) by the powdered rice hulls of dipping, at flow velocity, be that 30-50mL/min continues nitrogen and flows down pyrolysis, heating schedule is: from room temperature, with 10-20 ℃/min, rise to 800 ℃, keep 60-120min, obtain rice husk base charcoal loaded with nano ferriferrous oxide particles after cooling, i.e. RC-Fe
3o
4material.
2. utilize rice husk base charcoal loaded with nano ferriferrous oxide particles described in claim 1 to process a method for lead waste water, it is characterized in that comprising:
(A) in mass concentration, be in 1-1000mg/L lead waste water, to add rice husk base charcoal loaded with nano ferriferrous oxide particles, and to make its mass concentration in lead waste water be 0.1-2.0g/L;
(B) 60-120min that vibrates under the condition that is 250rpm by the mixed solution of step (A) gained in room temperature and rotating speed, can remove the lead ion in lead waste water.
3. the method for utilizing rice husk base charcoal loaded with nano tri-iron tetroxide to process lead waste water according to claim 2, it is characterized in that: by the rice husk base charcoal loaded with nano ferriferrous oxide particles magnet adsorption after step (B) is processed, after putting together, with after washed with de-ionized water, again drop into the processing of lead waste water.
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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 |
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| CN104437361A (en) * | 2014-10-24 | 2015-03-25 | 东华大学 | Method for preparing functional biological carbon by in-situ impregnation |
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| JP2017031025A (en) * | 2015-08-04 | 2017-02-09 | 公立大学法人首都大学東京 | Process for producing magnetically activated carbon |
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Application publication date: 20140205 |