CN105903459B - A kind of charcoal carried magnetic gelatin composite material and preparation method thereof and purposes - Google Patents
A kind of charcoal carried magnetic gelatin composite material and preparation method thereof and purposes Download PDFInfo
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- CN105903459B CN105903459B CN201610471568.0A CN201610471568A CN105903459B CN 105903459 B CN105903459 B CN 105903459B CN 201610471568 A CN201610471568 A CN 201610471568A CN 105903459 B CN105903459 B CN 105903459B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/027—Compounds of F, Cl, Br, I
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
Abstract
The present invention relates to a kind of charcoal carried magnetic gelatin composite material and preparation method thereof and purposes, the composite material is using charcoal as matrix, matrix surface carried magnetic gelatin.What is prepared concretely comprises the following steps:The order of preparation is that powdered biomass first is placed in pyrolysis in tube furnace to obtain charcoal, then gelatin is loaded Fe3O4Magnetic gelatine is obtained, then charcoal is loaded into this upper compound and obtains the product.In the preparation process of the charcoal carried magnetic gelatin composite material of the present invention, it is only necessary to which a pyrolytic process and a water-bath heating process, preparation expense is few, and the used time is also shorter, facilitates easy to operate.The product has good degradation effect to the arsenic in waste water.
Description
Technical field
The invention belongs to environment functional materials and water process new technical field, and in particular to a kind of charcoal carried magnetic is bright
The preparation method and purposes of glue composite material.
Background technology
Arsenic is widely distributed in nature, has metalloid characteristic, and product is mainly used for timber preservative, glass enamel
The fields such as industry, pesticide, alloy material, medicine, feed chemical industry particularly have specific use in terms of medicine, alloy material.
But arsenic mostly exists with other mineral (such as Non-ferrous minerals) associations, due to Spontaneous release and artificial exploitation, especially to poor
The a large amount of of ore deposit exploit and use, and a large amount of arsenic are developed with host element into environment in production process.Mining, non-ferrous metal smelting
For the waste water of the industrial circles discharges such as refining, sulfuric acid preparation, chemical dyestuff and pesticide producing often containing a large amount of arsenic, it is a kind of carcinogenic
Substance, and also there is genetoxic, belong to the World Health Organization (WHO) priority pollutants.Therefore economical and efficient is explored
The treatment technology for waste water arsenic removal it is very necessary.Arsenic removal technology mainly has the precipitation method, ion-exchange, film both at home and abroad at present
Partition method, bioanalysis and absorption method etc., and the precipitation method and absorption method application are most.
Charcoal is that the biomass such as agricultural wastes, solid waste, sludge are pyrolyzed generation under conditions of anaerobic or anoxic
The higher solid material of phosphorus content.Charcoal stability height, large specific surface area, pore structure are good and structure of functional groups enriches.
Therefore, charcoal is as a kind of new adsorbent, prepares simple, and easy to operate, raw material are easy to get, environment friendly and pollution-free and have
The advantages that nontoxic.But simple biological carbon materials are small and powdered biologies for the adsorption capacity of arsenic
There is the problems such as separation and difficult recycling in the treatment of waste water in charcoal.Therefore research and develop new other substances of load has height
The composite material of effect absorption property is the key matter of science and technology in current charcoal waste water treatment applications.Gelatin is a kind of
Environment-friendly type substance containing a large amount of amino and carboxyl, functional group enriches, and has extremely strong hydrophily, will by appropriate method
Combined with charcoal, it can be enhanced and be enriched with target contaminant, the ability for capturing intermediate product, and by magnetic loading to gelatin
On, it can be so that gelatine microsphere be more stable, increase specific surface area enhances adsorption capacity, on the other hand so that composite material can be more preferable
Separated with waste water, help to recycle and reuse.
The content of the invention
The technical problems to be solved by the invention are:For technical problem existing in the prior art, a kind of low price, height are developed
The composite material of the charcoal carried magnetic gelatin of the removal available for arsenic in waste water of effect.
A kind of preparation method of charcoal carried magnetic gelatin composite material proposed by the present invention, is to gelatin by charcoal
Functionalization is carried out, the adsorbent being prepared can be assembled in biological carbon surface by magnetic gelatine, increase biological carbon surface
Adsorption site quantity, be as follows:
(1) biomass raw material (selection is chestnut shell) are cleaned with deionized water, then drying 24 is small at 80 DEG C
When, the biomass after drying is crushed, obtains powdered biomass;It is put into be pyrolyzed in tube-type atmosphere furnace and fire, protected in pyrolytic process
The quartzy seal of tube of atmosphere furnace is held, while N is passed through with the flow velocity of 400mL/min into pipe2, entire pyrolytic process is kept with this
Anaerobic condition, the temperature program of tube furnace is set as:450 DEG C are risen to from room temperature with the heating of the heating rate of 7 DEG C/min, and
Persistently be pyrolyzed under this temperature conditions 2 it is small when, then start Temperature fall process, N kept in temperature-fall period2With identical flow velocity
It is continually fed into, the charcoal solid then fired.
(2) 2g gelatin is weighed with assay balance, adds in the 500ml beakers for filling 100ml water, be placed in 55 DEG C of water-baths
Gelatin solution is formed with 275 rpms of speed stirring half an hour, obtains solution A.
(3) iron chloride of 0.02mol is weighed, the frerrous chloride of 0.01mol is dissolved in respectively in 200ml water, both are molten
Liquid is poured into solution A simultaneously, and water-bath pot temperature is adjusted to 80 DEG C, and rotating speed is constant, lasting to stir, and then adds in 120ml ammonium hydroxide,
Stirring.
(4) after 5min, the 2g charcoals weighed are added in this mixed liquor, rotating speed water temperature is all constant, and is added dropwise
Three drop Tween 80s so that gelatin disperses, and solution mixes evenly, stops after magnetic mixed solution is stirred 1h, obtains suspension.
(5) solid in the obtained suspension in step 4 has magnetism, and rapid subsidence can be allowed to magnet, is used repeatedly
Deionization is washed, until the solid with a small amount of water is placed in drying in 60 DEG C of vacuum drying chambers, probably needed by suspension into neutrality
It to depend on the circumstances for 24 hours, treats to take out it after solid drying, be placed in mortar and grind it, cross 200nm sieves to get to described
Final composite material.
In above-mentioned preparation method, the order of preparation is first to be pyrolyzed powdered biomass in tube furnace to obtain charcoal, so
Afterwards again on charcoal by above-mentioned steps carried magnetic gelatin, the product is obtained finally by washing drying.Above-mentioned preparation side
In method, the biomass such as the raw material selection agricultural wastes of charcoal, solid waste, sludge.
In above-mentioned preparation method, the mass ratio of the gelatin and charcoal is 1:1, the concentration ratio of frerrous chloride and iron chloride
For 1:2.
In above-mentioned preparation method, containing powdered biomass must drying 24 is small at 80 DEG C in an oven when, to ensure to enter
Drying regime before being pyrolyzed in tube furnace.
In above-mentioned preparation method, the heating rate of tube furnace is 7 DEG C/min, and maximum temperature is 450 DEG C, and in this temperature strip
Persistently be pyrolyzed under part 2 it is small when.
Pentavalent arsenic in the charcoal carried magnetic gelatin composite material removal waste water being prepared using the method for the present invention.
Compared with prior art, the advantage of the invention is that:
1. the raw material sources of charcoal are extensive, and cheap, primary raw material is agricultural wastes, solid waste, sludge
Etc. biomass;Chemicals gelatin, ammonium hydroxide, iron chloride and frerrous chloride for using etc. are common chemical products.
2. the preparation process of charcoal carried magnetic gelatin composite material of the present invention and easy to operate, prepare it is quick, it is raw
The production cycle is short, and product recovery rate is high, special chemical industry equipment is not required, it is easy to accomplish industrialized production.
3. in the preparation process of the charcoal carried magnetic gelatin composite material of the present invention, only need a heat treatment and water-bath
Pot heating and drying course, prepare expense and the time is all shorter.
4. product is nontoxic, environmentally friendly.
5. the charcoal carried magnetic gelatin composite material of the present invention is high to the removal efficiency of arsenic.
Description of the drawings
Fig. 1 is the scanning electron microscope schematic diagram of the charcoal carried magnetic gelatin composite material of the embodiment of the present invention 1;
Surface illustrates that gelatin has been loaded to above charcoal there are many irregular white spheres as seen from the figure.
Fig. 2 is the infrared spectrum schematic diagram of the charcoal carried magnetic gelatin composite material of the embodiment of the present invention 1;
Occur the peak of ferro element in figure, illustrate that magnetic gelatine has been loaded to above charcoal.
Specific embodiment
The present invention is described in further details below with reference to Figure of description and specific embodiment.
Embodiment 1:
A kind of preparation of charcoal carried magnetic gelatin composite material of the present invention, charcoal raw material selection life plate
Chestnut shell, specific preparation method are as follows:
Biomass raw material (selection is chestnut shell) are cleaned with deionized water, when then drying 24 is small at 80 DEG C,
Biomass after drying is crushed, obtains powdered biomass;It is put into be pyrolyzed in tube-type atmosphere furnace and fire, gas is kept in pyrolytic process
The quartzy seal of tube of atmosphere stove, while N is passed through with the flow velocity of 400mL/min into pipe2, detesting for entire pyrolytic process is kept with this
Oxygen condition, the temperature program of tube furnace are set as:450 DEG C are risen to from room temperature with the heating rate heating of 7 DEG C/min, and herein
Persistently be pyrolyzed under temperature conditionss 2 it is small when, then start Temperature fall process, N kept in temperature-fall period2Continued with identical flow velocity
It is passed through, the charcoal solid then fired;2g gelatin is weighed with assay balance, adds in the 500ml beakers for filling 100ml water
In, it is placed in 55 DEG C of water-baths and gelatin solution is formed with 275 rpms of speed stirring half an hour, obtain solution A;It weighs
The iron chloride of 0.02mol, the frerrous chloride of 0.01mol are dissolved in respectively in 200ml water, both solution are poured into solution A simultaneously
In, water-bath pot temperature is adjusted to 80 DEG C, rotating speed is constant, lasting to stir, and then adds in 120ml ammonium hydroxide, stirring;It, will after 5min
The 2g charcoals weighed are added in this mixed liquor, and rotating speed water temperature is all constant, and three drop Tween 80s are added dropwise so that gelatin point
It dissipates, solution mixes evenly, stops after magnetic mixed solution is stirred 1h, obtains suspension;In obtained suspension in step 4
Solid there is magnetism, rapid subsidence can be allowed to magnet, is washed with deionized water repeatedly, until suspension is into neutrality, will be carried
The solid of water is placed in 60 DEG C of vacuum drying chambers dry on a small quantity, probably needs for 24 hours, to depend on the circumstances, and treats that solid drying afterwards will
Taking-up, be placed in mortar and grind it, cross 200nm sieves to get to the final composite material.
Charcoal carried magnetic gelatin composite material appearance obtained above is in black, places it under scanning electron microscope and sees
It examines, surface texture is as shown in Figure 1, it can be seen that its surface is uniformly distributed a large amount of gelatine microspheres.Fig. 2 is charcoal carried magnetic
The hysteresis graph of gelatin shows that adsorbent possesses good superparamagnetism.
Embodiment 2:
Pentavalent arsenic in the charcoal carried magnetic gelatin composite material processing waste water of the present invention, comprises the following steps:
50ml is taken to adjust pentavalent arsenic solutions of the pH in 3-11 scopes, it is bright to add in charcoal carried magnetic made from embodiment 1
Glue composite material, the dosage of the adsorbent are 0.02g, are reacted in 25 DEG C of isothermal vibration incubators, 6 it is small when after passed through
Filter separates adsorbent from waste water, is measured with atomic fluorescence spectrum under the instrument condition that negative pressure is 280V in waste water
The content for the arsenic not being degraded, the results are shown in Table 1 for the degradation amount of calculating:
Table 1:The degradation amount data of pentavalent arsenic solution adsorbent at different temperatures
As shown in Table 1, under identical initial concentration, adsorbance increases with the rising of temperature, this illustrates this adsorption process
For the endothermic reaction.
Embodiment 3:
Pentavalent arsenic in the charcoal carried magnetic gelatin composite material processing waste water of the present invention, comprises the following steps:
The pentavalent arsenic solution that 50mL initial concentrations are 0.2-50mg/L is taken, adds in charcoal load magnetic made from embodiment 1
Property gelatin composite material, the dosage of the adsorbent is 0.02g, is reacted in 25 DEG C of isothermal vibration incubators, 6 it is small when after lead to
Filtering separates adsorbent from waste water, is measured and given up under the instrument condition that negative pressure is 280V with atomic fluorescence spectrum
The content for the arsenic not being degraded in water, the results are shown in Table 1 for the degradation amount of calculating:
Table 2:Under room temperature under the conditions of pentavalent arsenic difference initial concentration adsorbent degradation amount data
As shown in Table 1, degradation amount of the adsorbent with 0.4708mg/g under conditions of initial concentration is 0.2mg/L,
And increase with initial concentration and increase, to 20mg/L under conditions of the degradation amount of the adsorbent reach 42.32mg/g, afterwards with
The increase degradation amount of concentration is reduced and tended to be steady, and the maximal absorptive capacity reached is 42.675mg/g.
Embodiment 4:
The charcoal load TiO of the present invention2Pentavalent arsenic in composite material processing waste water, comprises the following steps:
The arsenic solution that 50mL initial concentrations are 20mg/L is taken, charcoal carried magnetic gelatin made from addition embodiment 1 is answered
Condensation material, the dosage of the catalyst are 0.02g, and light-catalyzed reaction is carried out in 25 DEG C of constant incubators, and the reaction time is respectively
3min, 6min, 10min, 15min, 20min, 40min, 1h, 3h, 6h, 10h, for 24 hours.By filtering by adsorbent from waste water point
From, the content of the arsenic not being degraded in waste water is measured under the instrument condition that negative pressure is 280V with atomic fluorescence spectrum,
The results are shown in Table 3 for the degradation amount of calculating:
Table:3:To the degradation amount data of pentavalent arsenic under the differential responses time
As shown in Table 2, the catalyst degradation amount is in the increase in reaction time under conditions of initial concentration is 20mg/L
First increase the trend to tend to be steady afterwards, adsorb and basically reach balance when the reaction time is 4h, this case study on implementation is molten
It is carried out under the conditions of the original pH of liquid, i.e. pH is 7.42, and the maximal absorptive capacity that when balance reaches is 28.7mg/g.
The above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
With various process programs of the present inventive concept without substantial differences in protection scope of the present invention.
Claims (3)
1. a kind of charcoal carried magnetic gelatin composite material, which is characterized in that the composite material includes biological carbon matrix, base
The gelatin that is magnetic is loaded on body;
The preparation order of the charcoal carried magnetic gelatin composite material is first that gelatin is compound with magnetic material, then is loaded
Onto biological carbon matrix, following steps are specifically included:
(1) biomass raw material-chestnut shell is cleaned with deionized water, when then drying 24 is small at 80 DEG C, after drying
Biomass crushes, and obtains powdered biomass;It is put into be pyrolyzed in tube-type atmosphere furnace and fire, the quartz of atmosphere furnace is kept in pyrolytic process
The seal of tube, while N is passed through with the flow velocity of 400mL/min into pipe2, the anaerobic condition of entire pyrolytic process is kept with this, is managed
The temperature program of formula stove is set as:450 DEG C are risen to from room temperature with the heating rate heating of 7 DEG C/min, and in this temperature conditions
When persistently pyrolysis 2 is small down, then starts Temperature fall process, N is kept in temperature-fall period2It is continually fed into identical flow velocity, so
The charcoal solid fired afterwards;
(2) weigh 2g gelatin with assay balance, add in the 500mL beakers for filling 100mL water, be placed in 55 DEG C of water-baths with
275 rpms of speed stirring half an hour forms gelatin solution, obtains solution A;
(3) iron chloride of 0.02mol is weighed, the frerrous chloride of 0.01mol is dissolved in respectively in 200mL water, both solution are same
When pour into solution A, water-bath pot temperature is adjusted to 80 DEG C, rotating speed is constant, lasting to stir, and then adds in 120mL ammonium hydroxide, stirs
It mixes;
(4) after 5min, the 2g charcoals weighed are added in this mixed liquor, rotating speed water temperature is all constant, and three drops are added dropwise
Tween 80 so that gelatin disperses, and solution mixes evenly, stops after magnetic mixed solution is stirred 1h, obtains suspension;
(5) solid in the obtained suspension in step 4 have magnetism, rapid subsidence can be allowed to magnet, spend repeatedly from
Son washing, until the solid with a small amount of water is placed in drying in 60 DEG C of vacuum drying chambers, probably needed by suspension into neutrality
For 24 hours, depend on the circumstances, treat to take out it after solid drying, be placed in mortar and grind it, cross 200nm sieves to get to described
Final composite material.
2. a kind of charcoal carried magnetic gelatin composite material as described in claim 1 is applied to the pentavalent arsenic in removal waste water
Method, comprise the following steps:The charcoal carried magnetic gelatin composite material is added in into the solution of the arsenic ion containing pentavalent,
It is then placed in isothermal vibration case to be allowed to fully react, is separated charcoal carried magnetic gelatin composite material with the mode of filtering,
Complete the removal to pentavalent arsenic ion.
3. according to the method described in claim 2, it is characterized in that, composite material dosage in waste water is 20mg/L.
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CN109019699B (en) * | 2018-09-30 | 2020-08-18 | 东北农业大学 | Preparation method of rod-like ferroferric oxide particle-loaded biochar composite material |
CN112624405B (en) * | 2020-12-17 | 2023-06-20 | 鄂尔多斯市永胜污水处理有限公司 | Water purification capsule for oily wastewater treatment |
CN112808234B (en) * | 2020-12-31 | 2023-04-25 | 徐州工程学院 | Method for preparing multi-layer structure biochar bag by using biological resources and prepared biochar bag |
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CN104587958A (en) * | 2015-01-23 | 2015-05-06 | 中国科学院生态环境研究中心 | Composite biological carbon material loading iron oxide as well as preparation method and application of composite biological carbon material |
CN104787831A (en) * | 2015-03-23 | 2015-07-22 | 湖南大学 | Method for removing hexavalent chromium in wastewater through magnetic adsorbent compounded by chitosan and magnetic biological carbon |
CN104998620A (en) * | 2015-06-30 | 2015-10-28 | 南京工业大学 | Modified peanut shell biochar / poly aluminium chloride sludge composite adsorbent material |
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CN104587958A (en) * | 2015-01-23 | 2015-05-06 | 中国科学院生态环境研究中心 | Composite biological carbon material loading iron oxide as well as preparation method and application of composite biological carbon material |
CN104787831A (en) * | 2015-03-23 | 2015-07-22 | 湖南大学 | Method for removing hexavalent chromium in wastewater through magnetic adsorbent compounded by chitosan and magnetic biological carbon |
CN104998620A (en) * | 2015-06-30 | 2015-10-28 | 南京工业大学 | Modified peanut shell biochar / poly aluminium chloride sludge composite adsorbent material |
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