CN106540656A - It is a kind of to have magnetic Fe3O4The preparation method of base magnetic crust charcoal new adsorbent - Google Patents
It is a kind of to have magnetic Fe3O4The preparation method of base magnetic crust charcoal new adsorbent Download PDFInfo
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- CN106540656A CN106540656A CN201610841845.2A CN201610841845A CN106540656A CN 106540656 A CN106540656 A CN 106540656A CN 201610841845 A CN201610841845 A CN 201610841845A CN 106540656 A CN106540656 A CN 106540656A
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention prepares magnetic crust charcoal by primary raw material of agriculture and forestry organic waste material walnut shell, solves the problems, such as that existing acticarbon is difficult to recycle.By processed good walnut shell powdered carbon Jing iron chloride and ferrous chloride mixed solution activator are soaked, with sodium hydroxide as precipitant, a kind of new adsorbent is prepared into.Compared with common shell charcoal, the present invention is magnetized to common shell charcoal, is caused the adsorbent promptly carry out solid-liquid separation by the effect of external magnetic field, is eliminated the loaded down with trivial details steps such as centrifugation.
Description
Technical field
The present invention relates to a kind of new adsorbent of wastewater treatment, is belonging to adsorbing material preparation field, more particularly to
Process the sorbent preparation method of the heavy metal wastewater thereby of low concentration.
Background technology
The characteristics of heavy metal wastewater thereby pollution is with toxic effect long duration, biological non-degradable, and can be made by food chain
With entering human body, and accumulate in human body, so as to cause various diseases and disorder, serious danger is finally caused to health
Evil.How to prepare a kind of new adsorbent, can either make rational use of resources, it is also possible to the heavy metal in efficient absorption waste water from
Son realization reuse and the recycling of heavy metal to waste water, have important practical significance.
Agriculture and forestry organic waste material has wide material sources, cheap, regeneration period short, biodegradable and environmental friendliness etc. is many
Advantage, is important biomass resource, and the application in terms of environmental conservation has become the new trend of current research, especially
Become the ideal chose for processing heavy metal wastewater thereby.
Fe3O4The preparation of base magnetic crust charcoal is by Fe using coprecipitation3O4Particle is coated on common shell carbon surface so that
Which gives magnetization and is obtained.Fe3O4Base magnetic crust charcoal has magnetic, and the effect that can pass through external magnetic field after adsorption treatment can
Promptly carry out solid-liquid separation, and adsorption activity is high, adsorption capacity is big, the features such as easily reuse.Therefore, it is dirty in heavy metal chromium
There is in the wastewater treatment of dye preferable application prospect.
The content of the invention
It is contemplated that a kind of new adsorbent can be prepared, which is big to heavy metal ions in wastewater adsorption capacity,
Easily regenerate, with magnetic, solid-liquid separation can be carried out rapidly in the presence of external magnetic field, facilitate looping back for adsorbing material
Receive.
It is a kind of to have magnetic Fe3O4The preparation method of base magnetic crust charcoal new adsorbent,
It is characterized in that its preparation method is comprised the following steps：
Step one, by 3～5g FeCl3·6H2O and 1～2g FeCl2·4H2O is dissolved in beaker, mol ratio n (Fe3 +)：n(Fe2+)=2:1, the common shell charcoal of a certain amount of powder is added afterwards so that mass ratio mFeCl3·6H2O：mCommon shell charcoal=2:1, make
Be sufficiently mixed uniform, under the conditions of 75 DEG C, while mechanical agitation, the sodium hydrate aqueous solution of 40～60mL of Deca is used as heavy
Shallow lake agent causes the pH about 12～13 of mixed liquor, staticly settles beaker, remove supernatant after reaction 1h, and residue obtains suspended
Liquid；
Step 2, the remaining suspension obtained by step one is put in vacuum drying oven and dries 8～12h extremely at 60 DEG C
Resulting materials are rinsed to supernatant in neutrality with distilled water, are preserved in moving into exsiccator at 60 DEG C after drying by constant weight repeatedly,
Prepared adsorbent.
The common shell charcoal is selected from Xinjiang walnut shell shell charcoal.
The sample prepared in step 2 is dried to constant weight at 60 DEG C, the Fe of the too high generation of temperature3O4Granule is easily oxidized.
The adsorbent can parse regeneration, specifically include following steps：By the absorption preserved in exsiccator in step 2
Agent carries out, after adsorption treatment, soaking above-mentioned adsorbent using 0.1mol/L EDTA solution to Cr (VI) waste water of 20mg/L
Adsorbent is subsequently washed till neutrality by bubble 2h, is dried, is repeated the step, carry out parsing regeneration to adsorbent.
Beneficial effect：
(1) Fe of the present invention3O4Base magnetic crust charcoal preparation process is simple, the reaction condition to testing are less demanding, and cost is made
Valency is cheap；
(2) Fe of the present invention3O4The preparation of base magnetic crust charcoal is proportionally：n(Fe3+)：n(Fe2+)=2:1, mFeCl3·6H2O：
mCommon shell charcoal=2:1；Experiment proves that, process 20mg/L reaches 99.3% containing Cr (VI) waste water clearance, and the magnetic crust charcoal has
Magneto separate performance, completes precipitation in 10min under natural gravity setting condition, and only needs under external magnetic field well
45s can just realize sharp separation；
(3) magnetic adsorptive material of the invention is repeatable experiment proves that using adsorption activity is still kept after repeatedly, it
2h is parsed in 0.1mol/L EDTA solution, after reusing 4 times, the clearance of Cr (VI) reaches 97.9%, and residual concentration is
0.42mg/L。
Description of the drawings
Fig. 1 is the Fe prepared by embodiment 13O4Clearance figure of the base magnetic crust charcoal with common shell charcoal to Cr (VI).
Fig. 2 is the Fe prepared by embodiment 13O4Base magnetic crust charcoal regeneration effect figure.
Fig. 3 is the Fe prepared by embodiment 13O4Base magnetic crust charcoal adsorption-desorption isothermal figure.
Fig. 4 is the Fe prepared by embodiment 13O4The X-ray diffractogram of base magnetic crust charcoal new adsorbent.
Fig. 5 is the Fe prepared by embodiment 13O4The scanning electron microscope (SEM) photograph of base magnetic crust charcoal new adsorbent.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention
Limit the present invention.
Embodiment 1：
1st, 3～5g FeCl are weighed3·6H2O and 1～2g FeCl2·4H2O is dissolved in beaker, n (Fe3+)：n(Fe2+)=
2:1, add the common shell charcoal of a certain amount of powder, mFeCl3·6H2O：mCommon shell charcoal=2:1, it is allowed to be sufficiently mixed uniformly, in 75 DEG C of conditions
Under, the sodium hydrate aqueous solution of 40～60mL is slowly added dropwise while mechanical agitation as precipitant, it is beaker is quiet after reaction 1h
Precipitation is put, supernatant is removed；
2nd, above-mentioned remaining suspension is put in vacuum drying oven and is dried to constant weight at 60 DEG C, with distilled water by gained material
Material is rinsed to supernatant repeatedly in neutrality, and magnetic force is preserved during exsiccator is moved into after reclaiming drying.
Below by common shell charcoal, Fe3O4Ejusdem generis Cr (VI) waste water of two kinds of sorbent treatments of base magnetic crust charcoal, together
When its adsorption effect is compared.
(1) by Cr (VI) waste water of 50mL initial concentrations respectively 10,20,30,40,60,80 and 100mg/L in 100mL
In conical flask, the pH value for adjusting water sample is 2.0, adds common shell charcoal 0.8g, is placed in the agitator of 25 DEG C of constant temperature, in 100r/
After adsorbing 180min under min, filtrate is gone to determine the concentration of Cr (VI), its removal effect is as shown in Figure 1.
(2) by Cr (VI) waste water of 50mL initial concentrations respectively 10,20,30,40,60,80 and 100mg/L in 100mL
In conical flask, the pH value for adjusting water sample is 2.0, the Fe prepared in adding embodiment 13O4Base magnetic crust charcoal 0.2g, is placed in constant temperature 25
DEG C agitator in, under 100r/min adsorb 30min after, go filtrate determine Cr (VI) concentration, its removal effect such as Fig. 1 institutes
Show.
(3) by Fe obtained in embodiment 13O4Base magnetic crust charcoal carries out parsing regeneration, and 0.1mol/L EDTA are selected in parsing agent
Adsorbent after immersion 2h, is washed till neutrality, is dried by solution, repeats to carry out adsorption treatment to Cr (VI) waste water of 20mg/L, and which is heavy
Multiple utilizing status are as shown in Figure 2.
In from Fig. 1, common shell charcoal and Fe3O4Base magnetic crust charcoal is for the chromate waste water removal effect for processing low concentration
Preferably, when concentration is 20mg/L, clearance is followed successively by 96%, 99.6%, and Fe3O4The consumption and adsorption time of base magnetic crust charcoal
It is 1/4, the 1/6 of common shell charcoal respectively.In Fig. 2, parsing agent uses 0.1mol/LEDTA, works as Fe3O4Base magnetic crust charcoal repeats
After 4 times, the aqueous concentration of Cr (VI) be 0.42mg/L (<0.50mg/L), when which reuses the 5th, aqueous concentration
For 0.54mg/L, it is seen that its adsorption activity stills remain in higher level, but in order to meet the row of Cr in industrial wastewater (VI)
Put standard, Fe3O4The repeatable utilization selection of times of base magnetic crust charcoal is advisable for 4 times.
From the figure 3, it may be seen that in relatively low nip, Fe3O4Base magnetic crust charcoal is to N2Adsorbance it is less and change little, with
The continuous increase of relative pressure, its adsorbance is also gradually increasing, in p/p0Between 0.18～0.98 when, occur in that significantly
Adsorption desorption hysteresis loop, it is seen that there is substantial amounts of central hole structure in magnetic crust charcoal, belongs to typical micro--mesoporous material.Occur in Fig. 4
Some characteristic peaks, with Fe3O4Peak position it is consistent, show common shell carbon surface generate material be Fe3O4.It is in Fig. 5, general
Logical shell carbon surface is wrapped by many Fe3O4Particle so as to give magnetization, can occur exchange adsorption with chromium ion.
It should be understood that these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that
After the content for having read instruction of the present invention, those skilled in the art can be made various changes or modifications to the present invention, these
The equivalent form of value equally falls within the application appended claims limited range.
Claims (4)
1. it is a kind of to have magnetic Fe3O4The preparation method of base magnetic crust charcoal new adsorbent, it is characterised in that its preparation method bag
Include following steps：
Step one, by 3～5g FeCl3·6H2O and 1～2g FeCl2·4H2O is dissolved in beaker, mol ratio n (Fe3+)：n
(Fe2+)=2:1, the common shell charcoal of a certain amount of powder is added afterwards so that mass ratio mFeCl3·6H2O：mCommon shell charcoal=2:1, it is allowed to fill
Divide mix homogeneously, under the conditions of 75 DEG C, the sodium hydrate aqueous solution of 40～60mL of Deca is used as precipitant while mechanical agitation
So that beaker is staticly settled after reaction 1h, removes supernatant by the pH of mixed liquor about 12～13, residue obtains suspension；
Step 2, the remaining suspension obtained by step one is put in vacuum drying oven 8～12h is dried at 60 DEG C to perseverance
Resulting materials are rinsed to supernatant in neutrality with distilled water, are preserved, system at 60 DEG C after drying in moving into exsiccator by weight repeatedly
Obtain adsorbent.
2. magnetic Fe is had as claimed in claim 13O4The preparation method of base magnetic crust charcoal new adsorbent, its feature exist
In the common shell charcoal is selected from Xinjiang walnut shell shell charcoal.
3. magnetic Fe is had as claimed in claim 13O4The preparation method of base magnetic crust charcoal new adsorbent, its feature exist
In the sample prepared in step 2 is dried to constant weight at 60 DEG C.
4. magnetic Fe is had as claimed in claim 13O4The preparation method of base magnetic crust charcoal new adsorbent, its feature exist
In the adsorbent can parse regeneration, specifically include following steps：By the adsorbent pair preserved in exsiccator in step 2
After Cr (VI) waste water of 20mg/L carries out adsorption treatment, immersion 2h is carried out to above-mentioned adsorbent using 0.1mol/L EDTA solution,
Adsorbent is washed till into neutrality subsequently, is dried, is repeated the step, parsing regeneration is carried out to adsorbent.
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Cited By (7)
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| CN107376838A (en) * | 2017-07-31 | 2017-11-24 | 西安科技大学 | A kind of preparation method and application of magnetic active carbon fiber |
| CN107970890A (en) * | 2017-11-30 | 2018-05-01 | 华南理工大学 | A kind of hydroxyl iron-loaded modified activated carbon composite material and preparation method thereof |
| CN108187619A (en) * | 2018-01-24 | 2018-06-22 | 中冶华天工程技术有限公司 | The preparation method of EDTA modified magnetic activated carbon heavy metal-polluted soil renovation agents |
| CN111097373A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院生态环境研究中心 | Porous adsorption material, oxygen-carrying and adsorption composite functional material and application thereof |
| CN111097374A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院生态环境研究中心 | Preparation method of oxygen-carrying and adsorption composite functional material and application of oxygen-carrying and adsorption composite functional material in water body remediation |
| CN114272897A (en) * | 2021-12-23 | 2022-04-05 | 西安建筑科技大学 | Magnetic charcoal adsorbent based on chia seed gum and preparation method |
| CN115532229A (en) * | 2022-10-18 | 2022-12-30 | 兰州交通大学 | Preparation of magnetic adsorbent material and application of bacterium carrier construction in removing aflatoxin |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376838A (en) * | 2017-07-31 | 2017-11-24 | 西安科技大学 | A kind of preparation method and application of magnetic active carbon fiber |
| CN107970890A (en) * | 2017-11-30 | 2018-05-01 | 华南理工大学 | A kind of hydroxyl iron-loaded modified activated carbon composite material and preparation method thereof |
| CN108187619A (en) * | 2018-01-24 | 2018-06-22 | 中冶华天工程技术有限公司 | The preparation method of EDTA modified magnetic activated carbon heavy metal-polluted soil renovation agents |
| CN111097373A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院生态环境研究中心 | Porous adsorption material, oxygen-carrying and adsorption composite functional material and application thereof |
| CN111097374A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院生态环境研究中心 | Preparation method of oxygen-carrying and adsorption composite functional material and application of oxygen-carrying and adsorption composite functional material in water body remediation |
| CN114272897A (en) * | 2021-12-23 | 2022-04-05 | 西安建筑科技大学 | Magnetic charcoal adsorbent based on chia seed gum and preparation method |
| CN114272897B (en) * | 2021-12-23 | 2023-10-20 | 西安建筑科技大学 | Magnetic biochar adsorbent based on Qiya seed gum and preparation method |
| CN115532229A (en) * | 2022-10-18 | 2022-12-30 | 兰州交通大学 | Preparation of magnetic adsorbent material and application of bacterium carrier construction in removing aflatoxin |
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Application publication date: 20170329 |