CN104028214B - A kind of preparation method of agricultural biomass carbon back magnetic adsorptive material - Google Patents
A kind of preparation method of agricultural biomass carbon back magnetic adsorptive material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of agricultural biomass carbon back magnetic adsorptive material. The method be the agricultural biomass that derives from plant organism be raw material, adopt ferric ion and load process, alkali precipitation and the low-temperature hydrothermal carbonization of the ultrasonic blend of living beings to compose magnetic technique, the magnetic biological carbon adsorbing material of acquisition tool. The present invention not only can realize the preparation of carbon adsorbing material simultaneously and compose magnetic process, and raw material sources are extensive, cheap and easy to get, are that a kind of highly versatile, controllability are good, the simple preparation method of technique. The magnetism of material of preparing with the method is stable, and absorption property is strong, is easy to separate, and can be used for the organic pollutant removals such as water treatment decolouring, dyestuff, has broad application prospects in environmental improvement field.
Description
Technical field
The technical field that under the present invention prepared by sustainable regeneration and advanced material. Relate to biomass resource, material supply sectionThe correlation technique in multiple subject crossing fields such as, environmental science and environmental protection, relating generally to one can utilize on a large scaleAgricultural biomass resource is prepared the method for the magnetic biological carbon adsorbing material of tool.
Technical background
Along with science and technology and economic fast development, a large amount of discharges of agro-industry factory effluent make water environment pollution problem dayBenefit is outstanding. Particularly dyeing waste water, its contained dyestuff mostly is artificial synthetic chemical dye, has complicated aromatic ring structure, propertyMatter is stable, difficult degradation, have potential toxicity, and directly discharge meeting causes severe contamination to environment, and by food chain directly orIndirectly threaten human health. Biological carbon is to utilize in recent years a kind of New Type of Carbon sorbing material of absorption method treatment of dyeing and printing, canObtain by resourceful living beings imperfect combustion, the carbonaceous products producing has stronger to the pollutant in water bodySurface adsorption property. But the complexity of Pollutants in Wastewater kind and quantity has determined that the adsorption rate of biological carbon has much room for improvement,It is difficult to reclaim after processing dyestuff simultaneously, easily causes the wasting of resources and secondary pollution. Therefore, improve biological carbon adsorption rate and giveThe magnetic that it is stable, can solve an above-mentioned difficult problem, realizes the quick separation of pollutant and the recovery of adsorbent.
Utilize the biomass-making cheap and easy to get magnetic sorbing material of getting everything ready to attract wide attention in recent years. China speciallyProfit CN103316640A, name is called " a kind of preparation of magnetic green material adsorbent and the method for removal heavy metal ", by inciting somebody to actionLiving beings-acetic acid solution adds Fe after mixing with shitosan-acetic acid solution3O4The method of solid magnetic, prepares the magnetic of non-carbonizationProperty biomass absorbent material. Chinese patent CN103316636A, name is called " a kind of preparation side of biomass-based magnetic active carbonMethod ", employing is first prepared active carbon and with the method for magnetic mixing and absorption, magnetisable material is loaded on active carbon. Chinese patent CN101642699A, name is called " a kind of preparation method and its usage of magnetic biological carbon adsorbing material ", taking abandoned biomass as carbonSource, by ferrous iron and ferric iron mixed liquor as presoma, through precipitation, filter, adopt again the charing of limit oxygen after dry, compactingMethod prepare magnetic adsorptive material. Chinese patent CN101847481A, name is called that " abandoned biomass is prepared C-Fe shell nuclear-magnetismProperty active carbon new technology ", stalk or wood chip are mixed with zinc chloride and iron chloride mixed liquor, then logical in pyrolysis furnaceEnter 700 DEG C of nitrogen and carry out cracking. Chinese patent CN101564677B, name is called " a kind of superparamagnetism porous carbon absorption materialSynthetic method ", also adopted the method for 600 ~ 900 DEG C of roastings in nitrogen atmosphere to prepare magnetic adsorptive material. Although theseResearch all obtains certain effect, but still has following problem: (1) preparation process poor controllability. Particularly by active carbon or lifeThe fill process that material directly mixes with magnetic, easily causes magnetic medium to come off, and material structure is unstable, charcoal absorption energyThe problems such as power reduction. (2) magnetic presoma mostly is ferrous iron and ferric mixed liquor, molysite and inorganic salts mixed liquor or ironThe mixed liquor of salt, inorganic salts and ethanol, preparation process is loaded down with trivial details. (3) carbonization or tax magnetic process all adopt in limit oxygen or nitrogen atmosphereThe method of Pintsch process, on the one hand severe reaction conditions, increased energy consumption and cost, need on the other hand by reactant filter,Could Pintsch process processing after dry, compacting, process is loaded down with trivial details and the cycle is longer. Hydro-thermal method is a kind of using water as reaction mediumHeat chemistry transformation technology, the green synthetic important method of material with carbon element that Ye Shi material circle is generally acknowledged. But, utilize Hydrothermal Synthesis legal systemThe correlative study of magnetic agricultural wastes carbon back sorbing material of getting everything ready is not also reported at present.
China is the country of agricultural wastes quantum of output maximum in the world, wherein only the annual production of agricultural crop straw just up to7.5 hundred million tons and of a great variety, but because its Processes For Effective Conversion is few, comprehensive utilization ratio is low, cause the same of a large amount of wastes of resourceShi Yi causes environmental pollution, and the environmental problem of particularly bringing because of crop straw burning seems particularly outstanding in recent years. Therefore, forDifferent types of agricultural biomass is set up comparatively general, the simple treatment process of one and recycling approach, will be agriculture wasteMultiple stage circulation and the utilization in goods and materials source provide new approaches.
Summary of the invention
The present invention, from the angle of biomass resource utilization and water environment protection, for the deficiency in existing research, carriesSupply a kind of method of utilizing cheap agricultural wastes to prepare biological carbon back magnetic adsorptive material. Feature of the present invention is: (1)Be different from traditional co-precipitation method ferrous iron and ferric mixed liquor or molysite and inorganic salts mixed liquor or molysite, inorganic salts andThe mixed liquor of ethanol, the present invention only utilizes single trivalent iron salt as magnetic precursor liquid; (2) adopt hydrothermal reaction at low temperature synchronously completeBecome the preparation of biological carbon adsorbing material and compose magnetic process; (3) raw material sources are extensive, lignocellulose-like biomass or sourceStarch based living beings in plant all can be used as biological carbon raw material. The inventive method highly versatile, controllability is good, technique is simple,Mould material wide material sources and with low cost.
Below by technical scheme, the present invention is described in detail:
The first step, ultrasonic blend load process:
Described ultrasonic blend load process, refers to: the lignocellulose-like biomass after drying and pulverizing and plant are formed sedimentAfter one or more in powder mix, joining concentration is in the ferric trichloride precursor liquid of 0.1 ~ 1mol/L, living beings additionFor the above-mentioned liquor ferri trichloridi of 1g ~ 10g/100mL, mix rear ultrasonic power 500W and process 0.5h ~ 2h.
Described lignocellulose-like biomass be corncob, rice husk, wood chip, bagasse, rice straw, broomcorn straw,One or more mixtures in cotton stalk, soybean stalk and maize straw; Described plant amylum be conventional corn starch,One or more mixtures in waxy corn starch, amylomaize, farina, wheaten starch, tapioca.
The lignocellulose-like biomass such as described corncob, agricultural stalk, rice husk, wood chip, bagasse are 60 ~ 105After DEG C oven dry, pulverize, after pulverizing, cross 100 mesh sieves.
Described ferric trichloride precursor liquid is by FeCl3·6H2O is water-soluble to be made.
Second step, alkali precipitation:
Described alkali precipitation, refers to: be that the mixture that the first step is obtained adds a certain amount of NaOH solid and acutely stirsMix and mix, the quality of the NaOH adding is the above-mentioned living beings dispersion liquid of 0.02 ~ 0.05g/mL.
The 3rd step, magnetic technique is composed in low-temperature hydrothermal carbonization:
Magnetic technique is composed in described low-temperature hydrothermal carbonization, refers to the mixture obtaining through second step alkali precipitation is all transferred toIn stainless steel autoclave, carry out sealed reaction, reaction temperature 150-250 DEG C, reaction time 5-10h, dries after filtration washingThe dry carbon back magnetic adsorptive material that obtains.
Principle of the present invention and foundation are as follows: increase the accessibility of biomass material by the method for ultrasonic processing, promoteInfiltration and the deposition of ferric ion in living beings structure, shortens dip time, improves follow-up carbonization and composes magnetic efficiency. Pass throughThe method of low-temperature hydrothermal carbonization, becomes amorphous carbon as reaction medium by biomass conversion using water at low temperatures, simultaneously unformedThe formation of carbon is again by Fe3+Partial reduction, forms the magnetic Fe of tool3O4And be embedded in the frame structure of biological carbon, finally obtainObtain the magnetic sorbing material of tool.
The present invention is directed to the agricultural biomass (lignocellulose and starch based) that two classes derive from plant, one is providedHighly versatile, the preparation method that technique is simple, consuming time less, controllability is good. The material of preparing with the inventive method has goodMagnetic and absorption property, particularly have good adsorption effect for dyestuff of different nature, can be used for water treatment decolouring, hasThe removal of organic pollutants, has before wide application in the environmental improvement such as advanced treatment of waste water and toxic gas, automatically cleaning fieldScape.
Brief description of the drawings:
Fig. 1 is the preparation flow figure of agricultural biomass carbon back magnetic adsorptive material of the present invention
Fig. 2 is the design sketch that the corncob carbon back magnetic adsorptive material prepared of the present invention is processed methylene blue waste water.
Fig. 3 is that the XRD collection of illustrative plates of the magnetic adsorptive material that in embodiment 1 prepared by corncob (shows adsorbent " carbon back " with thisAnd Fe3O4Combination, Δ: carbon back (indefinite form carbon); Ο: Fe3O4）。
Fig. 4 is that the XRD collection of illustrative plates of the magnetic adsorptive material that in embodiment 15 prepared by conventional corn starch (shows adsorbent with this" carbon back " and Fe3O4Combination, Δ: carbon back (indefinite form carbon); Ο: Fe3O4）。
Fig. 5 is that the XRD collection of illustrative plates of the magnetic adsorptive material that in embodiment 14 prepared by rice husk, wood chip and broomcorn straw (is shown with thisBright adsorbent " carbon back " and Fe3O4Combination, Δ: carbon back (indefinite form carbon); Ο: Fe3O4）。
Fig. 6 is magnetic adsorptive material that in embodiment 22 prepared by amylomaize, wheaten starch and tapiocaXRD collection of illustrative plates (shows adsorbent " carbon back " and Fe with this3O4Combination, Δ: carbon back (indefinite form carbon); Ο: Fe3O4）。
Fig. 7 is that the XRD collection of illustrative plates that corncob is not composed the hydrothermal carbonization product of magnetic at 220 DEG C (shows not compose magnetic with thisIn product, only have " carbon back ", Δ: carbon back (indefinite form carbon))
Fig. 8 is the EDX collection of illustrative plates of the corncob carbon back magnetic adsorptive material prepared of the embodiment of the present invention 1.
Fig. 9 is the corncob prepared of the embodiment of the present invention 21 and the EDX collection of illustrative plates of starch mixing carbon back magnetic adsorptive material.
Detailed description of the invention
The present invention provides embodiment selectively, has provided detailed embodiment and specific operation process, only for this is describedThe part important value of invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1 prepares carbon back magnetic adsorptive material taking corncob as living beings
Collect the corncob that large Tanaka tests in this seminar, after cleaning, dry and pulverize, rear 100 mesh sieves of crossing of pulverizing in 90 DEG CAnd collect the maize cob meal that sieves, get 4g corncob powder and join the FeCl of 100mL0.1mol/L3In solution, 400After stirring, rmp rotating speed obtained disperseing the FeCl of maize cob meal in the ultrasonic 1h of 500W3Solution. Ultrasonic afterwards to having disperseedThe FeCl of maize cob meal3In solution, add the NaOH of 4g, continue 500rmp rotating speed vigorous stirring, be then transferred to hydro-thermal reactionIn still and seal hydrothermal reaction kettle, in 220 DEG C of reaction 6h, reaction finishes rear filtration and obtains magnetic with deionized water cyclic washingProperty carbon back sorbing material 2.5g.
Embodiment 2 prepares carbon back magnetic adsorptive material taking rice husk as living beings
Collect this seminar and test large Tanaka and gather in rice husk after treatment, after cleaning, dry and pulverize in 100 DEG C, after pulverizingCross 100 mesh sieves and collect the powdered rice hulls that sieves, getting 6g rice husk powder and join the FeCl of 100mL0.5mol/L3In solution,After stirring, 400rmp rotating speed obtained disperseing the FeCl of powdered rice hulls in the ultrasonic 1.5h of 500W3Solution. Ultrasonic afterwards to dividingThe FeCl of powdered rice hulls has fallen apart3In solution, add the NaOH of 5g, continue 500rmp rotating speed vigorous stirring, be then transferred to hydro-thermal anti-Answer in still and seal hydrothermal reaction kettle, in 200 DEG C of reaction 10h, reaction finishes rear filtration and obtains with deionized water cyclic washingMagnetic carbon adsorbing material 3.2g.
Embodiment 3 prepares carbon back magnetic adsorptive material taking wheat stalk as living beings
Collect the wheat stalk that large Tanaka tests in this seminar, after cleaning, dry and pulverize, mistake 100 after pulverizing in 105 DEG CMesh sieve is also collected the wheat stalk powder that sieves, gets 5g wheat stalk powder and join the FeCl of 100mL0.6mol/L3SolutionIn, after stirring, 400rmp rotating speed obtained disperseing the FeCl of wheat stalk powder in the ultrasonic 2h of 500W3Dispersion soln. SuperSound is afterwards to the FeCl that has disperseed wheat stalk powder3In solution, add the NaOH of 4g, continue 500rmp rotating speed vigorous stirring, soAfter be transferred in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 240 DEG C reaction 8h, reaction finish rear filtration and use deionizationWater cyclic washing obtains magnetic carbon adsorbing material 2.3g.
Embodiment 4 prepares carbon back magnetic adsorptive material taking wood chip as living beings
To after the wood chip cleaning of collection, dry and pulverize, the rear 100 mesh sieves wood chip that also collection is sieved of crossing of pulverizing in 100 DEG CPowder, gets 3g wood chip powder and joins the FeCl of 100mL1.0mol/L3In solution, after 400rmp rotating speed stirs inThe ultrasonic 2h of 500W has obtained disperseing the FeCl of wood dust3Solution. Ultrasonic afterwards to the FeCl that has disperseed wood dust3In solution, addEnter the NaOH of 2g, continue 500rmp rotating speed vigorous stirring, be then transferred in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in200 DEG C of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.8g with deionized water cyclic washing.
Embodiment 5 prepares carbon back magnetic adsorptive material taking maize leaves as living beings
Collect this seminar and test large Tanaka's maize leaves, after cleaning, dry and pulverize, rear 100 orders of crossing of pulverizing in 90 DEG CSieve and collect the maize leaves powder sieving, get 3g maize leaves powder and join the FeCl of 100mL0.3mol/L3In solution, 400After stirring, rmp rotating speed obtained disperseing the FeCl of maize leaves powder in the ultrasonic 1h of 500W3Solution. Ultrasonic afterwards to having disperseedThe FeCl of maize leaves powder3In solution, add the NaOH of 4g, continue 500rmp rotating speed vigorous stirring, be then transferred to hydro-thermal reactionIn still and seal hydrothermal reaction kettle, in 200 DEG C of reaction 10h, reaction finishes rear filtration and obtains magnetic with deionized water cyclic washingProperty carbon back sorbing material 1.5g.
Embodiment 6 prepares carbon back magnetic adsorptive material taking bagasse as living beings
Collect the bagasse that large Tanaka tests in this seminar, after cleaning, dry and pulverize, rear 100 mesh sieves of crossing of pulverizing in 90 DEG CAnd collect the bagasse powder that sieves, get 3g bagasse powder and join the FeCl of 100mL0.5mol/L3In solution, 400After stirring, rmp rotating speed obtained disperseing the FeCl of bagasse powder in the ultrasonic 1.5h of 500W3Solution. Ultrasonic afterwards to dispersionThe FeCl of bagasse powder3In solution, add the NaOH of 3g, continue 500rmp rotating speed vigorous stirring, be then transferred to hydro-thermal anti-Answer in still and seal hydrothermal reaction kettle, in 220 DEG C of reaction 10h, reaction finishes rear filtration and obtains with deionized water cyclic washingMagnetic carbon adsorbing material 1.37g.
Embodiment 7 prepares carbon back magnetic adsorptive material taking rice straw as living beings
Collect the rice straw that large Tanaka tests in this seminar, after cleaning, dry and pulverize, mistake 100 after pulverizing in 80 DEG CMesh sieve is also collected the rice straw powder that sieves, gets 10g rice straw powder and join the FeCl of 100mL0.2mol/L3MoltenIn liquid, after stirring, 400rmp rotating speed obtains disperseing the FeCl of rice straw powder in the ultrasonic 0.5h of 500W3Solution. SuperSound is afterwards to the FeCl that has disperseed rice straw powder3In solution, add the NaOH of 5g, continue 500rmp rotating speed vigorous stirring, soAfter be transferred in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 240 DEG C reaction 5h, reaction finish rear filtration and use deionizationWater cyclic washing obtains magnetic carbon adsorbing material 4.86g.
Embodiment 8 prepares carbon back magnetic adsorptive material taking broomcorn straw as living beings
Collect the broomcorn straw that large Tanaka tests in this seminar, after cleaning, dry and pulverize, rear 100 orders of crossing of pulverizing in 80 DEG CSieve and collect the broomcorn straw powder sieving, get 8g broomcorn straw powder and join the FeCl of 100mL0.6mol/L3SolutionIn, after stirring, 400rmp rotating speed obtained disperseing the FeCl of broomcorn straw powder in the ultrasonic 2h of 500W3Solution. Ultrasonic itThe backward FeCl that disperses broomcorn straw powder3In solution, add the NaOH of 4g, continue 500rmp rotating speed vigorous stirring, then turnMove in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 220 DEG C of reaction 10h, reaction finishes rear filtration anti-by deionized waterAfter backwashing is washed and is obtained magnetic carbon adsorbing material 4.39g.
Embodiment 9 prepares carbon back magnetic adsorptive material taking cotton stalk as living beings
Collect the cotton stalk that large Tanaka tests in this seminar, after cleaning, dry and pulverize, mistake 100 after pulverizing in 90 DEG CMesh sieve is also collected the cotton stalk powder that sieves, gets 6g cotton stalk powder and join the FeCl of 100mL0.8mol/L3SolutionAfter stirring, middle 400rmp rotating speed obtained disperseing the FeCl of cotton stalk powder in the ultrasonic 1h of 500W3Solution. After ultrasonicTo the FeCl that has disperseed cotton stalk powder3In solution, add the NaOH of 4g, continue 500rmp rotating speed vigorous stirring, then turnMove in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 250 DEG C of reaction 5h, reaction finishes rear filtration anti-by deionized waterAfter backwashing is washed and is obtained magnetic carbon adsorbing material 3.27g.
Embodiment 10 prepares carbon back magnetic adsorptive material taking soybean stalk as living beings
Collect the soybean stalk that large Tanaka tests in this seminar, after cleaning, dry and pulverize, mistake 100 after pulverizing in 100 DEG CMesh sieve is also collected the soybean stalk powder that sieves, gets 3g soybean stalk powder and join the FeCl of 100mL0.3mol/L3SolutionIn, after stirring, 400rmp rotating speed obtained disperseing the FeCl of soybean stalk powder in the ultrasonic 2h of 500W3Solution. Ultrasonic itThe backward FeCl that disperses soybean stalk powder3In solution, add the NaOH of 2g, continue 500rmp rotating speed vigorous stirring, then turnMove in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 240 DEG C of reaction 6h, reaction finishes rear filtration anti-by deionized waterAfter backwashing is washed and is obtained magnetic carbon adsorbing material 1.39g.
Embodiment 11 prepares carbon back magnetic adsorptive material taking maize straw as living beings
Collect the maize straw that large Tanaka tests in this seminar, after cleaning, dry and pulverize, rear 100 orders of crossing of pulverizing in 90 DEG CSieve and collect the corn stalk powder sieving, get 5g maize straw powder and join the FeCl of 100mL0.4mol/L3SolutionIn, after stirring, 400rmp rotating speed obtained disperseing the FeCl of corn stalk powder in the ultrasonic 2h of 500W3Solution. Ultrasonic itThe backward FeCl that disperses corn stalk powder3In solution, add the NaOH of 4g, continue 500rmp rotating speed vigorous stirring, then turnMove in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 220 DEG C of reaction 6h, reaction finishes rear filtration anti-by deionized waterAfter backwashing is washed and is obtained magnetic carbon adsorbing material 2.37g.
Embodiment 12 prepares carbon back magnetic adsorptive material taking corncob and rice husk as living beings
Collect the corncob that large Tanaka tests in this seminar, after cleaning, dry and pulverize, rear 100 orders of crossing of pulverizing in 105 DEG CSieve and collect the maize cob meal sieving. Collect the rice husk that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 105 DEG C,After pulverizing, cross 100 mesh sieves and collect the powdered rice hulls sieving. Get 2g corncob powder and 2g rice husk powder joins 100mLThe FeCl of 0.5mol/L3In solution, after stirring, 400rmp rotating speed obtains having disperseed mixed-powder in the ultrasonic 1h of 500WFeCl3Solution. Ultrasonic afterwards to the FeCl that has disperseed mixed-powder3In solution, add the NaOH of 4g, continue 500rmp rotating speedVigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 220 DEG C of reaction 8h, reaction finishes rear filtrationAnd obtain magnetic carbon adsorbing material 2.06g with deionized water cyclic washing.
Embodiment 13 prepares carbon back magnetic adsorptive material taking the mixture of bagasse and maize straw as living beings
Collect the bagasse that large Tanaka tests in this seminar, clean latter 90 DEG C and dry and pulverize, after pulverizing, cross 100 mesh sievesAnd collect the bagasse powder that sieves. Collect the maize straw that large Tanaka tests in this seminar, after cleaning, dry and powder in 90 DEG CBroken, after pulverizing, cross 100 mesh sieves and collect the corn stalk powder sieving. Get 4g bagasse powder and 2g maize straw powder addsTo the FeCl of 100mL0.3mol/L3In solution, after stirring, 400rmp rotating speed obtains having disperseed in the ultrasonic 2h of 500WThe FeCl of mixed-powder3Solution. Ultrasonic afterwards to the FeCl that has disperseed mixed-powder3In solution, add the NaOH of 4g, continue 500Rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, in 240 DEG C of reaction 6h, reaction knotAfter bundle, filter and use deionized water cyclic washing to obtain magnetic carbon adsorbing material 2.89g.
Embodiment 14 prepares carbon back magnetic adsorptive material taking the mixture of rice husk, wood chip and broomcorn straw as living beings
Collect this seminar and test large Tanaka and gather in rice husk after treatment, after cleaning, dry and pulverize in 100 DEG C, pulverizeRear mistake 100 mesh sieves are also collected the powdered rice hulls sieving. After the wood chip of collecting is cleaned, dry and pulverize, mistake after pulverizing in 100 DEG C100 mesh sieves are also collected the wood dust sieving. Collect the broomcorn straw that large Tanaka tests in this seminar, after cleaning in 100 DEG C of oven dryAnd pulverize, after pulverizing, cross 100 mesh sieves and collect the broomcorn straw powder sieving. Get 2g powdered rice hulls, 1g wood dust and 3g sorghum stalksStalk powder joins the FeCl of 100mL0.3mol/L3In solution, after stirring, 400rmp rotating speed obtains in the ultrasonic 2h of 500WTo the FeCl that has disperseed mixed-powder3Solution. Ultrasonic afterwards to the FeCl that has disperseed mixed-powder3In solution, add 4g'sNaOH, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, anti-in 240 DEG CAnswer 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.95g with deionized water cyclic washing.
Embodiment 15 prepares carbon back magnetic adsorptive material taking conventional corn starch as living beings
The conventional corn starch of drying at 60 DEG C is added to the FeCl of 100mL0.2mol/L with the amount of 5g3SolutionIn, after stirring, 400rmp rotating speed obtained disperseing the FeCl of conventional corn starch in the ultrasonic 1h of 500W3Solution. UltrasonicAfterwards to the FeCl that has disperseed conventional corn starch3In solution, add the NaOH of 3g, continue 500rmp rotating speed vigorous stirring, soAfter be transferred in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 150 DEG C reaction 10h, reaction finish rear filtration and use deionizationWater cyclic washing obtains magnetic carbon adsorbing material 2.29g.
Embodiment 16 prepares carbon back magnetic adsorptive material taking waxy corn starch as living beings
The waxy corn starch of drying at 60 DEG C is added to the FeCl of 100mL0.3mol/L with the amount of 4g3SolutionIn, after stirring, 400rmp rotating speed obtained disperseing the FeCl of waxy corn starch in the ultrasonic 2h of 500W3Solution. UltrasonicAfterwards to the FeCl that has disperseed waxy corn starch3In solution, add the NaOH of 4g, continue 500rmp rotating speed vigorous stirring, soAfter be transferred in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 180 DEG C reaction 6h, reaction finish rear filtration and use deionizationWater cyclic washing obtains magnetic carbon adsorbing material 1.86g.
Embodiment 17 prepares carbon back magnetic adsorptive material taking amylomaize as living beings
The amylomaize of drying at 60 DEG C is added to the FeCl of 100mL0.5mol/L with the amount of 6g3MoltenIn liquid, after stirring, 400rmp rotating speed obtains disperseing the FeCl of amylomaize in the ultrasonic 1.5h of 500W3MoltenLiquid. Ultrasonic afterwards to the FeCl that has disperseed amylomaize3In solution, add the NaOH of 5g, continue the play of 500rmp rotating speedStrong stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 DEG C of reaction 6h, reaction finishes rear filtration alsoObtain magnetic carbon adsorbing material 2.57g with deionized water cyclic washing.
Embodiment 18 prepares carbon back magnetic adsorptive material taking farina as living beings
The farina of drying at 60 DEG C is added to the FeCl of 100mL0.1mol/L with the amount of 3g3In solution,After stirring, 400rmp rotating speed obtained disperseing the FeCl of farina in the ultrasonic 0.5h of 500W3Solution. After ultrasonicTo the FeCl that has disperseed farina3In solution, add the NaOH of 3g, continue 500rmp rotating speed vigorous stirring, then shiftTo hydrothermal reaction kettle and seal hydrothermal reaction kettle, in 150 DEG C of reaction 6h, reaction finish rear filtration and with deionized water repeatedlyWashing obtains magnetic carbon adsorbing material 1.28g.
Embodiment 19 prepares carbon back magnetic adsorptive material taking wheaten starch as living beings
The wheaten starch of drying at 60 DEG C is added to the FeCl of 100mL0.6mol/L with the amount of 5g3In solution, 400After stirring, rmp rotating speed obtained disperseing the FeCl of wheaten starch in the ultrasonic 2h of 500W3Solution. Ultrasonic afterwards to having disperseedThe FeCl of wheaten starch3In solution, add the NaOH of 4g, continue 500rmp rotating speed vigorous stirring, be then transferred to hydro-thermal reactionIn still and seal hydrothermal reaction kettle, in 180 DEG C of reaction 6h, reaction finishes rear filtration and obtains magnetic with deionized water cyclic washingProperty carbon back sorbing material 2.35g.
Embodiment 20 prepares carbon back magnetic adsorptive material taking tapioca as living beings
The tapioca of drying at 60 DEG C is added to the FeCl of 100mL0.5mol/L with the amount of 4g3In solution, 400After stirring, rmp rotating speed obtained disperseing the FeCl of tapioca in the ultrasonic 2h of 500W3Solution. Ultrasonic afterwards to having disperseedThe FeCl of tapioca3In solution, add the NaOH of 3g, continue 500rmp rotating speed vigorous stirring, be then transferred to hydro-thermal reactionIn still and seal hydrothermal reaction kettle, in 200 DEG C of reaction 6h, reaction finishes rear filtration and obtains magnetic with deionized water cyclic washingProperty carbon back sorbing material 1.83g.
Embodiment 21 prepares carbon back magnetic adsorptive material taking the mixture of conventional corn starch and corncob as living beings
Dry maize cob meal 2g and add 100mL at the conventional corn starch 2g of drying at 60 DEG C and 105 DEG CThe FeCl of 0.3mol/L3In solution, after stirring, 400rmp rotating speed obtains disperseing mixed-powder in 500W ultrasonic 1hFeCl3Solution. Ultrasonic afterwards to the FeCl that has disperseed mixed-powder3In solution, add the NaOH of 5g, continue the play of 500rmp rotating speedStrong stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 DEG C of reaction 6h, reaction finishes rear filtration alsoObtain magnetic carbon adsorbing material 1.72g with deionized water cyclic washing.
Embodiment 22 prepares carbon back taking the mixture of amylomaize, wheaten starch and tapioca as living beingsMagnetic adsorptive material
By what dry at the wheaten starch 3g of drying at the amylomaize 1g, 60 DEG C of drying at 60 DEG C and 60 DEG CTapioca 2g adds the FeCl of 100mL0.2mol/L to3In solution, super in 500W after 400rmp rotating speed stirsSound 2h has obtained disperseing the FeCl of mixed-powder3Solution. Ultrasonic afterwards to the FeCl that has disperseed mixed-powder3In solution, add 4The NaOH of g, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, in 200DEG C reaction 8h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.56g with deionized water cyclic washing.
Embodiment 23 prepares carbon back magnetic taking the mixture of cotton stalk, wood chip and amylomaize as living beingsSorbing material
Collect the cotton stalk that large Tanaka tests in this seminar, after cleaning, dry and pulverize, rear 100 orders of crossing of pulverizing in 90 DEG CSieve and collect the cotton stalk powder sieving; After the wood chip of collecting is cleaned, dries and pulverizes in 90 DEG C, pulverize rear 100 mesh sieves alsoThe wood dust that collection is sieved. The high straight-chain maize that above-mentioned 1g cotton stalk powder, the above-mentioned wood dust of 1g and 6g are dried at 60 DEG CStarch fully mixes, and then adds the FeCl of 100mL1mol/L to3In solution, after 400rmp rotating speed stirs in 500The ultrasonic 2h of W has obtained disperseing the FeCl of mixed-powder3Solution. Ultrasonic afterwards to the FeCl that has disperseed mixed-powder3In solution, addEnter the NaOH of 5g, continue 500rmp rotating speed vigorous stirring, be then transferred in hydrothermal reaction kettle and seal hydrothermal reaction kettle, in220 DEG C of reaction 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 3.98g with deionized water cyclic washing.
Embodiment 24 prepares carbon back taking the mixture of rice husk, broomcorn straw, farina and tapioca as living beingsMagnetic adsorptive material
Collect this seminar and test large Tanaka and gather in rice husk after treatment, after cleaning, dry and pulverize in 105 DEG C, after pulverizingCross 100 mesh sieves and collect the powdered rice hulls sieving. Collect the broomcorn straw that large Tanaka tests in this seminar, after cleaning in 105 DEG C of bakingsDry doubling is pulverized, and crosses 100 mesh sieves and collect the broomcorn straw powder sieving after pulverizing. By above-mentioned 1g powdered rice hulls, the above-mentioned broomcorn straw of 1gThe tapioca that the farina that powder, 2g are dried at 60 DEG C and 2g are dried at 60 DEG C fully mixes, and then adds toThe FeCl of 100mL0.5mol/L3In solution, after 400rmp rotating speed stirs, obtain having disperseed mixed in the ultrasonic 2h of 500WClose the FeCl of powder3Solution. Ultrasonic afterwards to the FeCl that has disperseed mixed-powder3In solution, add the NaOH of 4g, continue 500Rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, in 240 DEG C of reaction 6h, reaction knotAfter bundle, filter and use deionized water cyclic washing to obtain magnetic carbon adsorbing material 2.85g.
The embodiment 25 absorption property evaluations of living beings magnetic carbon back sorbing material to dyestuff
Adsorption test concrete steps:
1. get respectively magnetic adsorbent prepared by 0.02g above-described embodiment and add the methylene that 10mL concentration is 120mg/L toIn the blue solution of base.
2. the above-mentioned dye solution that has added magnetic adsorbent is placed in to oscillator and shakes 30min, after concussion finishes, useMagnetic field separating adsorbent, gets supernatant and measures absorbance in spectrophotometer 664nm, calculates dyestuff according to calibration curveResidual quantity.
3. magnetic adsorptive material absorption property is evaluated:
Adsorption rate=
C0For methylene blue initial concentration, C1For the methylene blue concentration of magnetic adsorptive material after 30min absorption.
Choosing typical difficult degradation organic dyestuff methylene blue in dyeing waste water is representative, to what prepare with the inventive methodThe performance of agricultural biomass carbon back magnetic adsorptive material is evaluated and illustrates. Magnetic adsorbent consumption in embodiment is 2G/L, methylene blue dye concentration is 120mg/L, adsorption time is 30min. Concrete outcome is in table 1:
The absorption property of table 1 living beings magnetic carbon back sorbing material to methylene blue dye
Choose in dyeing waste water the Congo red and methyl orange of typical difficult degradation organic dyestuff, to what prepare with the inventive methodThe performance of agricultural biomass carbon back magnetic adsorptive material is evaluated and illustrates. Magnetic adsorbent consumption in embodiment is 2G/L, dye strength is 100mg/L, adsorption time is 60min. Concrete outcome is in table 2:
Table 2 living beings magnetic carbon back sorbing material is to Congo red and absorption property methyl orange dye
Claims (8)
1. a preparation method for living beings carbon back magnetic adsorptive material, is characterized in that: living beings are joined to ferric trichlorideIn solution and fully mix, mix rear ultrasonic processing and obtained disperseing the liquor ferri trichloridi of living beings; Then to having disperseed lifeIn the liquor ferri trichloridi of material, add NaOH abundant stirring and dissolving to obtain the living beings dispersion liquid of processing through NaOH; FinallyThe living beings dispersion liquid of processing through NaOH is transferred in stainless steel autoclave, close under 150-250 DEG C of temperature conditionsEnvelope reaction, after reaction, washing and drying obtains living beings carbon back magnetic adsorptive material, and described powdered biomass is lignocellulosicThe mixture of one or several in the middle of biolobic material powder and plant amylum powdered biomass.
2. the preparation method of a kind of living beings carbon back magnetic adsorptive material as claimed in claim 1, it is characterized in that comprising withLower step:
1) ultrasonic blend load: it is three of 0.1～1mol/L that the dry powdered biomass of 1～10g is joined to 100mL concentrationIn ferric chloride solution, fully mix rear ultrasonic processing 0.5h～2h and obtained disperseing the liquor ferri trichloridi of powdered biomass;
2) alkali precipitation: to step 1) gained dispersion in the liquor ferri trichloridi of powdered biomass, add a certain amount of NaOH solidBody vigorous stirring mix the living beings dispersion liquid obtaining through NaOH processing, the NaOH solid masses adding and above-mentioned biologyThe ratio of matter dispersion liquid is 0.02～0.05g/mL;
3) magnetic technique is composed in low-temperature hydrothermal carbonization: by step 2) the living beings dispersion liquid of processing through NaOH of gained is all transferred toIn stainless steel autoclave, also sealing is reacted, and reaction temperature is 150-250 DEG C, reaction time 5-10h, mistake after reactionFilter fully washing post-drying obtain living beings carbon back magnetic adsorptive material;
Described powdered biomass be a kind of in the middle of lignocellulose-like biomass powder and plant amylum powdered biomass orSeveral mixtures.
3. the preparation method of a kind of living beings carbon back magnetic adsorptive material as claimed in claim 2, is characterized in that: step 1)Described powdered biomass is the central one of lignocellulose-like biomass powder and plant amylum powdered biomass or severalThe mixture of planting; And lignocellulose-like biomass powder is that lignocellulose-like biomass is through 60～105 DEG C of dry, pulverizingAnd the powder that sieves of mistake 100 mesh sieves; Plant amylum powdered biomass is the powder of plant amylum living beings after super-dry.
4. the preparation method of a kind of living beings carbon back magnetic adsorptive material as claimed in claim 3, is characterized in that: described woodMatter cellulose series biomass comprises corncob, rice husk, wheat stalk, wood chip, maize leaves, bagasse, rice straw, sorghum stalksStalk, cotton stalk, soybean stalk and maize straw; Described plant amylum living beings are that conventional corn starch, waxy corn form sedimentPowder, amylomaize, farina, wheaten starch, tapioca.
5. the preparation method of a kind of living beings carbon back magnetic adsorptive material according to claim 2, is characterized in that: step1) liquor ferri trichloridi of 0.1 described～1mol/L is by FeCl3·6H2O is water-soluble to be made.
6. the preparation method of a kind of living beings carbon back magnetic adsorptive material according to claim 2, is characterized in that: step1) the ultrasonic processing described in, ultrasonic power is 500W.
7. a living beings carbon back magnetic adsorptive material, is characterized in that by the one described in claim 1-6 any one rawThe preparation method of material carbon back magnetic adsorptive material prepares.
8. the application of a kind of living beings carbon back magnetic adsorptive material claimed in claim 7 in Adsorption of Organic, is characterized by:The difficult degradating organic dye of described organic matter, described difficult degradation organic dyestuff is methylene blue, Congo red and methyl orange.
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