CN104028214A - Preparation method for agriculture biomass carbon-based magnetic adsorption material - Google Patents
Preparation method for agriculture biomass carbon-based magnetic adsorption material Download PDFInfo
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Abstract
The invention discloses a preparation method for an agriculture biomass carbon-based magnetic adsorption material. According to the method, agriculture biomass originated from plant organisms is used as a raw material and a loading process of ultrasonic blending of trivalent iron ions with biomass, alkali precipitation and a low temperature hydro-thermal carbonization magnetization process are adopted so as to prepare the biomass carbon adsorption material with magnetism. The method realizes simultaneous preparation and magnetization of the carbon adsorption material and has the advantages of wide sources, low price and easy availability of the raw material, good versatility and controllability and easy processes. The material prepared by using the method has stable magnetism and strong adsorptivity, is easy to separate, can be used for water treatment decoloring and removal of organic pollutants like dyes and shows wide application prospects in the field of environmental management.
Description
Technical field
The technical field that under the present invention prepared by sustainable regeneration and advanced material.The correlation technique that relates to a plurality of subject crossing fields such as biomass resource, material science, environmental science and environmental protection, relates generally to a kind of agricultural biomass resource of can utilizing on a large scale and prepares 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 become increasingly conspicuous water environment pollution problem.Dyeing waste water particularly, its contained dyestuff mostly is artificial synthetic chemical dye, have complicated aromatic ring structure, stable in properties, difficult degradation, have potential toxicity, directly discharge meeting causes severe contamination to environment, and directly or indirectly threatens human health by food chain.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, can obtain by resourceful living beings imperfect combustion, and the carbonaceous products producing has stronger surface adsorption property to the pollutant in water body.Yet 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 give its stable magnetic, can solve an above-mentioned difficult problem, realizing 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.Chinese patent CN 103316640 A, name is called " a kind of preparation of magnetic green material adsorbent and the method for removal heavy metal ", after living beings-acetic acid solution is mixed with shitosan-acetic acid solution, adds Fe
3o
4the method of solid magnetic, prepares the magnetic green material sorbing material of non-carbonization.Chinese patent CN 103316636 A, name is called " a kind of preparation method of biomass-based magnetic active carbon ", and 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 ", take abandoned biomass as carbon source, by ferrous iron and ferric iron mixed liquor as presoma, through precipitation, filter, adopt again the method for limit oxygen charing to prepare magnetic adsorptive material after dry, compacting.Chinese patent CN 101847481 A, name is called " new technology of preparing C-Fe shell-core magnetic active carbon by utilizing waste biomasses ", and stalk or wood chip are mixed with zinc chloride and iron chloride mixed liquor, then in pyrolysis furnace, passes into 700 ℃ of nitrogen and carries out cracking.Chinese patent CN 101564677 B, name is called " a kind of synthetic method of superparamagnetism porous carbon absorption material ", has also adopted the method for 600～900 ℃ of roastings in nitrogen atmosphere to prepare magnetic adsorptive material.Although these researchs all obtain certain effect, still there is following problem: (1) preparation process poor controllability.Particularly, by active carbon or the direct fill process mixing with magnetic of living beings, easily cause the problems such as magnetic medium comes off, and material structure is unstable, activated carbon adsorptive capacity reduction.(2) magnetic presoma mostly is the mixed liquor of ferrous iron and ferric mixed liquor, molysite and inorganic salts mixed liquor or molysite, inorganic salts and ethanol, and preparation process is loaded down with trivial details.(3) carbonization or tax magnetic process all adopt the method for Pintsch process in limit oxygen or nitrogen atmosphere, on the one hand severe reaction conditions, increased energy consumption and cost, need on the other hand reactant to filter, could process by Pintsch process after dry, compacting, process is loaded down with trivial details and the cycle is longer.Hydro-thermal method is a kind ofly to using water as the heat chemistry transformation technology of reaction medium, the green synthetic important method of material with carbon element that Ye Shi material circle is generally acknowledged.Yet the correlative study that utilizes hydrothermal synthesis method to prepare the magnetic agricultural wastes carbon back of tool sorbing material 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 to 7.5 hundred million tons and of a great variety, but because its Processes For Effective Conversion is few, comprehensive utilization ratio is low, when causing a large amount of waste of resource, easily cause environmental pollution, the environmental problem of particularly bringing because of crop straw burning, seems particularly outstanding in recent years.Therefore, for different types of agricultural biomass, set up a kind of comparatively general, simple treatment process and recycling approach, by the multiple stage circulation for agricultural wastes resource and utilization, 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, provides a kind of method of utilizing cheap agricultural wastes to prepare biological carbon back magnetic adsorptive material.Feature of the present invention is: (1) is different from the mixed liquor of ferrous iron and ferric mixed liquor or molysite and inorganic salts mixed liquor or molysite, inorganic salts and ethanol in traditional co-precipitation method, and the present invention only utilizes single trivalent iron salt as magnetic precursor liquid; (2) adopt hydrothermal reaction at low temperature synchronously complete the preparation of biological carbon adsorbing material and compose magnetic process; (3) raw material sources are extensive, and lignocellulose-like biomass or the starch based living beings that derive from 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, refer to: by after the lignocellulose-like biomass after drying and pulverizing and one or more mixing in plant amylum, joining concentration is in the ferric trichloride precursor liquid of 0.1～1mol/L, living beings addition is the above-mentioned liquor ferri trichloridi of 1g～10g/100mL, mixes rear ultrasonic power 500W and processes 0.5h～2h.
Described lignocellulose-like biomass is one or more mixtures in corncob, rice husk, wood chip, bagasse, rice straw, broomcorn straw, cotton stalk, soybean stalk and maize straw; Described plant amylum is one or more mixtures in conventional corn starch, waxy corn starch, amylomaize, farina, wheaten starch, tapioca.
The lignocellulose-like biomass such as described corncob, agricultural stalk, rice husk, wood chip, bagasse are to pulverize after 60～105 ℃ of oven dry, after pulverizing, cross 100 mesh sieves.
Described ferric trichloride precursor liquid is by FeCl
36H
2o 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 vigorous stirring to 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, refer to the mixture obtaining through second step alkali precipitation is all transferred to and in stainless steel autoclave, carries out sealed reaction, reaction temperature 150-250 ℃, reaction time 5-10h, filtration washing post-drying obtains carbon back magnetic adsorptive material.
Principle of the present invention and foundation are as follows: by the method for ultrasonic processing, increase the accessibility of biomass material, promote infiltration and the deposition of ferric ion in living beings structure, shorten dip time, improve follow-up carbonization and tax magnetic efficiency.By the method for low-temperature hydrothermal carbonization, the water of usining at low temperatures becomes amorphous carbon as reaction medium by biomass conversion, and the formation of agraphitic carbon is again by Fe simultaneously
3+partial reduction, forms the magnetic Fe of tool
3o
4and be embedded in the frame structure of biological carbon, finally obtain 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, a kind of highly versatile, technique is simple, consuming time less, controllability is good preparation method are provided.The material of preparing with the inventive method has good magnetic and absorption property, particularly for dyestuff of different nature, there is good adsorption effect, can be used for the removal of water treatment decolouring, organic pollution, in the environmental improvements such as advanced treatment of waste water and toxic gas, automatically cleaning field, have broad application prospects.
Accompanying drawing explanation
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 " and Fe with this
3o
4combination, Δ: carbon back (indefinite form carbon); Ο: Fe
3o
4).
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 " carbon back " and Fe with this
3o
4combination, Δ: carbon back (indefinite form carbon); Ο: Fe
3o
4).
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 (shows adsorbent " carbon back " and Fe with this
3o
4combination, Δ: carbon back (indefinite form carbon); Ο: Fe
3o
4).
Fig. 6 is that the XRD collection of illustrative plates of the magnetic adsorptive material that in embodiment 22 prepared by amylomaize, wheaten starch and tapioca (shows adsorbent " carbon back " and Fe with this
3o
4combination, Δ: carbon back (indefinite form carbon); Ο: Fe
3o
4).
Fig. 7 is that the corncob XRD collection of illustrative plates of not composing the hydrothermal carbonization product of magnetic at 220 ℃ (shows not compose in the product of magnetic with this and only has " 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 of the embodiment of the present invention 1 preparation.
Fig. 9 is the corncob of the embodiment of the present invention 21 preparations and the EDX collection of illustrative plates of starch mixing carbon back magnetic adsorptive material.
The specific embodiment
The present invention provides embodiment selectively, has provided detailed embodiment and specific operation process, be only explanation part important value of the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1 be take corncob and is prepared carbon back magnetic adsorptive material as living beings
Collect the corncob that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 90 ℃, after pulverizing, cross 100 mesh sieves and collect the maize cob meal sieving, get the FeCl that 4g corncob powder joins 100mL0.1mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of maize cob meal in the ultrasonic 1h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed maize cob meal
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 220 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.5g with deionized water cyclic washing.
Embodiment 2 be take rice husk and is prepared carbon back magnetic adsorptive material as living beings
Collect this seminar and test large Tanaka and gather in the rice husk after processing, after cleaning, dry and pulverize in 100 ℃, after pulverizing, cross 100 mesh sieves and collect the powdered rice hulls sieving, get the FeCl that 6g rice husk powder joins 100mL0.5mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of powdered rice hulls in the ultrasonic 1.5h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed powdered rice hulls
3the NaOH that adds 5g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 ℃ of reaction 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 3.2g with deionized water cyclic washing.
Embodiment 3 be take wheat stalk and is prepared carbon back magnetic adsorptive material as living beings
Collect the wheat stalk that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 105 ℃, after pulverizing, cross 100 mesh sieves and collect the wheat stalk powder sieving, get the FeCl that 5g wheat stalk powder joins 100mL0.6mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of wheat stalk powder in the ultrasonic 2h of 500W
3dispersion soln.Ultrasonic afterwards to the FeCl that has disperseed wheat stalk powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 240 ℃ of reaction 8h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.3g with deionized water cyclic washing.
Embodiment 4 be take wood chip and is prepared carbon back magnetic adsorptive material as living beings
After the wood chip of collecting is cleaned, dries and pulverizes in 100 ℃, after pulverizing, cross the 100 mesh sieves wood dust that also collection is sieved, get the FeCl that 3g wood chip powder joins 100mL1.0mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of wood dust in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed wood dust
3the NaOH that adds 2g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.8g with deionized water cyclic washing.
Embodiment 5 be take maize leaves and is prepared carbon back magnetic adsorptive material as living beings
Collect this seminar and test large Tanaka's maize leaves, after cleaning, dry and pulverize in 90 ℃, after pulverizing, cross 100 mesh sieves and collect the maize leaves powder sieving, get the FeCl that 3g maize leaves powder joins 100mL0.3mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of maize leaves powder in the ultrasonic 1h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed maize leaves powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 ℃ of reaction 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.5g with deionized water cyclic washing.
Embodiment 6 be take bagasse and is prepared carbon back magnetic adsorptive material as living beings
Collect the bagasse that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 90 ℃, after pulverizing, cross 100 mesh sieves and collect the bagasse powder sieving, get the FeCl that 3g bagasse powder joins 100mL0.5mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of bagasse powder in the ultrasonic 1.5h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed bagasse powder
3the NaOH that adds 3g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 220 ℃ of reaction 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.37g with deionized water cyclic washing.
Embodiment 7 be take rice straw and is prepared carbon back magnetic adsorptive material as living beings
Collect the rice straw that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 80 ℃, after pulverizing, cross 100 mesh sieves and collect the rice straw powder sieving, get the FeCl that 10g rice straw powder joins 100mL0.2mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of rice straw powder in the ultrasonic 0.5h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed rice straw powder
3the NaOH that adds 5g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 240 ℃ of reaction 5h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 4.86g with deionized water cyclic washing.
Embodiment 8 be take broomcorn straw and is prepared carbon back magnetic adsorptive material as living beings
Collect the broomcorn straw that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 80 ℃, after pulverizing, cross 100 mesh sieves and collect the broomcorn straw powder sieving, get the FeCl that 8g broomcorn straw powder joins 100mL0.6mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of broomcorn straw powder in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed broomcorn straw powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 220 ℃ of reaction 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 4.39g with deionized water cyclic washing.
Embodiment 9 be take cotton stalk and is prepared carbon back magnetic adsorptive material as living beings
Collect the cotton stalk that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 90 ℃, after pulverizing, cross 100 mesh sieves and collect the cotton stalk powder sieving, get the FeCl that 6g cotton stalk powder joins 100mL0.8mol/L
3in solution, 400rmp rotating speed has obtained disperseing the FeCl of cotton stalk powder in the ultrasonic 1h of 500W after stirring
3solution.Ultrasonic afterwards to the FeCl that has disperseed cotton stalk powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 250 ℃ of reaction 5h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 3.27g with deionized water cyclic washing.
Embodiment 10 be take soybean stalk and is prepared carbon back magnetic adsorptive material as living beings
Collect the soybean stalk that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 100 ℃, after pulverizing, cross 100 mesh sieves and collect the soybean stalk powder sieving, get the FeCl that 3g soybean stalk powder joins 100mL0.3mol/L
3in solution, after stirring, 400 rmp rotating speeds obtained disperseing the FeCl of soybean stalk powder in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed soybean stalk powder
3the NaOH that adds 2g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 240 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.39g with deionized water cyclic washing.
Embodiment 11 be take maize straw and is prepared carbon back magnetic adsorptive material as living beings
Collect the maize straw that large Tanaka tests in this seminar, after cleaning, dry and pulverize in 90 ℃, after pulverizing, cross 100 mesh sieves and collect the corn stalk powder sieving, get the FeCl that 5g maize straw powder joins 100mL0.4mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of corn stalk powder in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed corn stalk powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 220 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.37g with deionized water cyclic washing.
Embodiment 12 be take corncob and rice husk and is prepared carbon back magnetic adsorptive material as living beings
Collect the corncob that large Tanaka tests in this seminar, after cleaning, in 105 ℃, dry and pulverize, the rear 100 mesh sieves maize cob meal that also collection is sieved of crossing of pulverizing.Collect the rice husk that large Tanaka tests in this seminar, after cleaning, in 105 ℃, dry and pulverize, the rear 100 mesh sieves powdered rice hulls that also collection is sieved of crossing of pulverizing.Get the FeCl that 2g corncob powder and 2g rice husk powder join 100mL0.5mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of mixed-powder in the ultrasonic 1h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed mixed-powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 220 ℃ of reaction 8h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.06g with deionized water cyclic washing.Embodiment 13 be take the mixture of bagasse and maize straw and is prepared carbon back magnetic adsorptive material as living beings
Collect the bagasse that large Tanaka tests in this seminar, clean latter 90 ℃ and dry and pulverize, after pulverizing, cross 100 mesh sieves and collect the bagasse powder sieving.Collect the maize straw that large Tanaka tests in this seminar, after cleaning, in 90 ℃, dry and pulverize, the rear 100 mesh sieves corn stalk powder that also collection is sieved of crossing of pulverizing.Get the FeCl that 4g bagasse powder and 2g maize straw powder join 100mL0.3mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of mixed-powder in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed mixed-powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 240 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.89g with deionized water cyclic washing.
Embodiment 14 be take the mixture of rice husk, wood chip and broomcorn straw and is prepared carbon back magnetic adsorptive material as living beings
Collect this seminar and test large Tanaka and gather in the rice husk after processing, after cleaning, dry and pulverize in 100 ℃, after pulverizing, cross 100 mesh sieves and collect the powdered rice hulls sieving.To after the wood chip cleaning of collection, in 100 ℃, dry and pulverize, the rear 100 mesh sieves wood dust that also collection is sieved of crossing of pulverizing.Collect the broomcorn straw that large Tanaka tests in this seminar, after cleaning, in 100 ℃, dry and pulverize, the rear 100 mesh sieves broomcorn straw powder that also collection is sieved of crossing of pulverizing.Get the FeCl that 2g powdered rice hulls, 1g wood dust and 3g broomcorn straw powder join 100mL0.3mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of mixed-powder in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed mixed-powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 240 ℃ of reaction 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.95g with deionized water cyclic washing.
Embodiment 15 be take conventional corn starch and is prepared carbon back magnetic adsorptive material as living beings
With the amount of 5g, add the conventional corn starch of drying at 60 ℃ the FeCl of 100mL0.2mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of conventional corn starch in the ultrasonic 1h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed conventional corn starch
3the NaOH that adds 3g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 150 ℃ of reaction 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.29g with deionized water cyclic washing.
Embodiment 16 be take waxy corn starch and is prepared carbon back magnetic adsorptive material as living beings
With the amount of 4g, add the waxy corn starch of drying at 60 ℃ the FeCl of 100mL0.3mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of waxy corn starch in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed waxy corn starch
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 180 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.86g with deionized water cyclic washing.
Embodiment 17 be take amylomaize and is prepared carbon back magnetic adsorptive material as living beings
With the amount of 6g, add the amylomaize of drying at 60 ℃ the FeCl of 100mL0.5mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of amylomaize in the ultrasonic 1.5h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed amylomaize
3the NaOH that adds 5g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.57g with deionized water cyclic washing.
Embodiment 18 be take farina and is prepared carbon back magnetic adsorptive material as living beings
With the amount of 3g, add the farina of drying at 60 ℃ the FeCl of 100mL0.1mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of farina in the ultrasonic 0.5h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed farina
3the NaOH that adds 3g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 150 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.28g with deionized water cyclic washing.
Embodiment 19 be take wheaten starch and is prepared carbon back magnetic adsorptive material as living beings
With the amount of 5g, add the wheaten starch of drying at 60 ℃ the FeCl of 100mL0.6mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of wheaten starch in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed wheaten starch
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 180 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.35g with deionized water cyclic washing.
Embodiment 20 be take tapioca and is prepared carbon back magnetic adsorptive material as living beings
With the amount of 4g, add the tapioca of drying at 60 ℃ the FeCl of 100mL0.5mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of tapioca in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed tapioca
3the NaOH that adds 3g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.83g with deionized water cyclic washing.
Embodiment 21 be take the mixture of conventional corn starch and corncob and is prepared carbon back magnetic adsorptive material as living beings
By at the conventional corn starch 2g of drying at 60 ℃ and 105 ℃, dry the FeCl that maize cob meal 2g adds 100mL0.3mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of mixed-powder in the ultrasonic 1h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed mixed-powder
3the NaOH that adds 5g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 1.72g with deionized water cyclic washing.
Embodiment 22 be take the mixture of amylomaize, wheaten starch and tapioca and is prepared carbon back magnetic adsorptive material as living beings
The tapioca 2g of drying at the wheaten starch 3g of drying at the amylomaize 1g of drying at 60 ℃, 60 ℃ and 60 ℃ is added to the FeCl of 100mL0.2mol/L
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of mixed-powder in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed mixed-powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 200 ℃ of reaction 8h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.56g with deionized water cyclic washing.
Embodiment 23 be take the mixture of cotton stalk, wood chip and amylomaize and is prepared carbon back magnetic adsorptive material as living beings
Collect the cotton stalk that large Tanaka tests in this seminar, after cleaning, in 90 ℃, dry and pulverize, the rear 100 mesh sieves cotton stalk powder that also collection is sieved of crossing of pulverizing; To after the wood chip cleaning of collection, in 90 ℃, dry and pulverize, the rear 100 mesh sieves wood dust that also collection is sieved of crossing of pulverizing.The amylomaize that the above-mentioned cotton stalk powder of 1g, the above-mentioned wood dust of 1g and 6g are dried at 60 ℃ fully mixes, and then adds the FeCl of 100mL1mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of mixed-powder in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed mixed-powder
3the NaOH that adds 5g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 220 ℃ of reaction 10h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 3.98g with deionized water cyclic washing.
Embodiment 24 be take the mixture of rice husk, broomcorn straw, farina and tapioca and is prepared carbon back magnetic adsorptive material as living beings
Collect this seminar and test large Tanaka and gather in the rice husk after processing, after cleaning, dry and pulverize in 105 ℃, after pulverizing, cross 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 ℃, dry and pulverize, the rear 100 mesh sieves broomcorn straw powder that also collection is sieved of crossing of pulverizing.The tapioca that the farina that the above-mentioned powdered rice hulls of 1g, the above-mentioned broomcorn straw powder of 1g, 2g are dried at 60 ℃ and 2g are dried at 60 ℃ fully mixes, and then adds the FeCl of 100mL0.5mol/L to
3in solution, after stirring, 400rmp rotating speed obtained disperseing the FeCl of mixed-powder in the ultrasonic 2h of 500W
3solution.Ultrasonic afterwards to the FeCl that has disperseed mixed-powder
3the NaOH that adds 4g in solution, continues 500rmp rotating speed vigorous stirring, is then transferred in hydrothermal reaction kettle and seals hydrothermal reaction kettle, and in 240 ℃ of reaction 6h, reaction finishes rear filtration and obtains magnetic carbon adsorbing material 2.85g with deionized water cyclic washing.
The embodiment 25 absorption property evaluations of living beings magnetic carbon back sorbing material to dyestuff
Adsorption test concrete steps:
1. getting respectively magnetic adsorbent prepared by 0.02g above-described embodiment adds in the methylene blue solution that 10mL concentration is 120mg/L.
2. the above-mentioned dye solution that has added magnetic adsorbent is placed in to oscillator and shakes 30min, after concussion finishes, use magnetic field separating adsorbent, get supernatant and measure absorbance in spectrophotometer 664nm, according to calibration curve, calculate the residual quantity of dyestuff.
3. magnetic adsorptive material absorption property is evaluated:
C
0for methylene blue initial concentration, C
1for 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, and the performance of the agricultural biomass carbon back magnetic adsorptive material of preparing with the inventive method is evaluated and illustrated.Magnetic adsorbent consumption in embodiment is 2g/L, and methylene blue dye concentration is 120mg/L, and 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, the performance of the agricultural biomass carbon back magnetic adsorptive material of preparing with the inventive method is evaluated and illustrated.Magnetic adsorbent consumption in embodiment is 2g/L, and dye strength is 100mg/L, and 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 (10)
1. a preparation method for living beings carbon back magnetic adsorptive material, is characterized in that: living beings are joined in liquor ferri trichloridi and fully mixed, mix the liquor ferri trichloridi that rear ultrasonic processing has obtained disperseing living beings; Then to disperseed to add in the liquor ferri trichloridi of living beings NaOH and fully stirring and dissolving obtain the living beings dispersion liquid of processing through NaOH; Finally the living beings dispersion liquid of processing through NaOH is transferred in stainless steel autoclave, 150-250 ℃ of temperature conditions lower seal reaction, after reaction, washing and drying obtains living beings carbon back magnetic adsorptive material.
2. the preparation method of a kind of living beings carbon back magnetic adsorptive material as claimed in claim 1, is characterized in that comprising the following steps:
1) ultrasonic blend load: it is in the liquor ferri trichloridi of 0.1 ~ 1 mol/L that the dry powdered biomass of 1 ~ 10 g is joined to 100 mL concentration, fully mixes the liquor ferri trichloridi that rear ultrasonic processing 0.5 h ~ 2 h has obtained disperseing powdered biomass;
2) alkali precipitation: to the dispersion of step 1) gained in the liquor ferri trichloridi of powdered biomass, add a certain amount of NaOH solid vigorous stirring to mix to obtain the living beings dispersion liquid of processing through NaOH, the NaOH solid masses adding and the ratio of above-mentioned living beings dispersion liquid are 0.02 ~ 0.05 g/mL;
3) low-temperature hydrothermal carbonization tax magnetic technique: by step 2) the living beings dispersion liquid of processing through NaOH of gained is all transferred in stainless steel autoclave and seals and reacts, reaction temperature is 150-250 ℃, reaction time 5-10 h, filters after reaction and abundant washing post-drying obtains living beings carbon back magnetic adsorptive material.
3. the preparation method of a kind of living beings carbon back magnetic adsorptive material as claimed in claim 2, is characterized in that: the powdered biomass described in step 1) is one or several the mixture in the middle of lignocellulose-like biomass powder and plant amylum powdered biomass; And lignocellulose-like biomass powder is that lignocellulose-like biomass is through 60 ~ 105 ℃ of dry, to pulverize and cross 100 mesh sieves powder that sieve; 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 lignocellulose-like biomass comprises corncob, rice husk, wheat stalk, wood chip, maize leaves, bagasse, rice straw, broomcorn straw, cotton stalk, soybean stalk and maize straw; Described plant amylum living beings are conventional corn starch, waxy corn starch, 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: the liquor ferri trichloridi of 0.1 ~ 1 mol/L described in step 1) is by FeCl
36H
2o 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: the ultrasonic processing described in step 1), ultrasonic power is 500 W.
7. a living beings carbon back magnetic adsorptive material, is characterized in that being prepared by the preparation method of a kind of living beings carbon back magnetic adsorptive material described in claim 1-6 any one.
8. the application of a kind of living beings carbon back magnetic adsorptive material claimed in claim 7 in Adsorption of Organic.
9. the application of a kind of living beings carbon back magnetic adsorptive material as claimed in claim 8 in Adsorption of Organic, is characterized by: the difficult degradating organic dye of described organic matter.
10. the application of a kind of living beings carbon back magnetic adsorptive material as claimed in claim 9 in Adsorption of Organic, is characterized by: described difficult degradation organic dyestuff is methylene blue, Congo red and methyl orange.
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