CN106861624A - A kind of preparation method of the porous carbon of adsorbable organic dyestuff in wastewater - Google Patents
A kind of preparation method of the porous carbon of adsorbable organic dyestuff in wastewater Download PDFInfo
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- CN106861624A CN106861624A CN201710226554.7A CN201710226554A CN106861624A CN 106861624 A CN106861624 A CN 106861624A CN 201710226554 A CN201710226554 A CN 201710226554A CN 106861624 A CN106861624 A CN 106861624A
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- porous carbon
- wastewater
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- organic dyestuff
- carbon materials
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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
- B01J20/28054—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 surface properties or porosity
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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
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention provides a kind of preparation method of the porous carbon of adsorbable organic dyestuff in wastewater, main step includes：After activator and EDTA blendings, the high-temperature activation under inert gas shielding, then obtain porous carbon materials by ultrasound, filtering, washing and drying.Porous carbon materials prepared by the present invention possess the performance of efficiently recyclable absorption organic dyestuff.This method process is simple, advantages of good adsorption effect, cyclic utilization rate is high, with certain application value.
Description
Technical field
The present invention relates to technical field of waste water processing, it particularly relates to a kind of adsorbable organic dyestuff in wastewater is more
The preparation method of hole carbon.
Background technology
Organic dyestuff is the important chemical products of a class, and the kind of dyes that industry is applied at present there are about more than 100,000 kinds, greatly
Most dyestuffs are artificial synthesized and with extremely complex structure, and organic dye waste water is universally acknowledged key industry pollution sources
One of, its gas chromatography and noxious material for containing causes high risks to ecological environment and drinking water.It is usually used at present
Process organic dye waste water method mainly have chemical precipitation method, oxidation-reduction method, membrane separation process, photochemical method, bioanalysis and
Absorption method etc., wherein, absorption method because its is simple and easy to do, with low cost, it is efficiently quick receive much concern.With absorption property
Carbon material has CNT, porous carbon, graphene sponge etc., and CNT, graphene sponge are relatively costly, therefore using many
Hole carbon material has certain social effect as the adsorbent of Cheap highly effective.
The present invention is, with EDTA as raw material, it to be sufficiently mixed with a certain amount of activator, is lived under certain condition
Change is processed, and prepares a kind of porous carbon materials of efficiently recyclable absorption organic dyestuff in wastewater, and this kind of material has to organic dyestuff
There is preferable absorption property.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation side of the porous carbon of adsorbable organic dyestuff in wastewater
Method.
A kind of preparation method of the porous carbon of adsorbable organic dyestuff in wastewater, comprises the following steps：
A, activator is fully ground, then it is well mixed with the EDTA of fixed proportion；
B, mixture is activated 1.5-2.5 hours in the atmosphere of inert gases at 550-650 DEG C；
C, solid obtain porous carbon materials by ultrasound, filtering, washing, drying.
Preferably, in described step A, activator is inorganic strong alkali.
Preferably, in described step A, activator is potassium hydroxide.
Preferably, in described step A, the mass ratio of activator and EDTA is 1：（1.5-4）.
The preparation method of the porous carbon of absorption organic dyestuff in wastewater provided by the present invention, main step includes：Will
After activator and EDTA blendings, the high-temperature activation under inert gas shielding, then obtain many by ultrasound, filtering, washing and drying
Hole carbon material.Porous carbon materials prepared by the present invention possess the performance of efficiently recyclable absorption chrysoidine.This method process is simple,
Advantages of good adsorption effect, cyclic utilization rate is high, with certain application value.
Specific embodiment
Embodiment 1
Potassium hydroxide is ground to it is powdered, then by itself and EDTA in mass ratio 1:2（g/g）It is well mixed, by it in nitrogen
In being activated 2 hours at 600 DEG C in atmosphere, solid obtains porous carbon materials after ultrasound, filtering, washing, drying.
Embodiment 2
Potassium hydroxide is ground to it is powdered, then by itself and EDTA in mass ratio 1:4（g/g）It is well mixed, by it in nitrogen
In being activated 1.5 hours at 650 DEG C in atmosphere, solid obtains porous carbon materials after ultrasound, filtering, washing, drying.
Embodiment 3
Potassium hydroxide is ground to it is powdered, then by itself and EDTA in mass ratio 1:1.5（g/g）It is well mixed, by it in nitrogen
Atmosphere obtains porous carbon materials in activation 2.5 hours at 550 DEG C, solid in enclosing after ultrasound, filtering, washing, drying.
Embodiment 4
NaOH is ground to it is powdered, then by itself and EDTA in mass ratio 1:2（g/g）It is well mixed, by it in nitrogen
In being activated 2 hours at 600 DEG C in atmosphere, solid obtains porous carbon materials after ultrasound, filtering, washing, drying.
Embodiment 5
Potassium hydroxide is ground to it is powdered, then by itself and EDTA in mass ratio 1:3（g/g）It is well mixed, by it in nitrogen
In being activated 2 hours at 620 DEG C in atmosphere, solid obtains porous carbon materials after ultrasound, filtering, washing, drying.
Resulting materials are carried out into Fourier's infrared analysis, it is found that O-H stretching vibrations, C=O are primarily present on spectrogram stretches and shake
Dynamic, C-O stretching vibrations, C-N stretching vibrations.
Resulting materials are carried out into XRD analysis, scanning result finds that being 24 ° or so in 2 θ has " short and stout " type diffraction maximum, this
Peak correspondence amorphous carbon；There is faint diffraction maximum for 42 ° or so in 2 θ, this peak shows that material degree of graphitization is relatively low.
Resulting materials are carried out into Raman analyses, amorphous carbon peak and graphitized carbon peak are located at 1353cm respectively-1（ID）、
1586 cm-1 (IG)。
Resulting materials are carried out into TG analyses, as a result shows material in 50 DEG C -200 DEG C main generation H2O loses, at 200 DEG C
It is main above that CO occurs2Loss, contains O-H and C=O in further testimonial material.
Resulting materials are carried out into BET analyses, as a result shows that material is mesoporous material.BET specific surface area is up to 1322 m2g-1, wherein the ratio between micropore and mesopore surface area about 3：2, maximum pore volume is about 0.54 cm3/g.By BJH models
（Barrett-Joyner-Halenda model）And HK models（Horvath-Kawazoe model）Analysis, Jie of material
Hole aperture is main in 2-3nm, and micropore size is mainly in 0.43nm.
Embodiment 6
By a certain amount of porous carbon materials of gained under specified temp and pH with a certain amount of chrysoidine solution mixing certain hour,
Systematically research porous carbon materials are to chrysoidine absorption property in waste water.
0.005g porous carbons prepared by embodiment 1 under 298K, 308K and 318K with 10ml, concentration is 100-500mg/
L, pH value be 6.0 chrysoidine solution mixing, adsorption time be 30 minutes, by langmuir simulation obtain 298K, 308K,
The adsorbance of chrysoidine is respectively 800mg/g, 735mg/g, 725mg/g under 318K.Porous carbon materials are calculated to Ke's clothing
The thermodynamic parameter of fixed absorption（△G0(KJmol-1)、△H0(KJmol-1)、△S0(Jmol-1K-1)）Be respectively under 298K-
16.4 KJmol-1、-12.9 KJmol-1、11.4 Jmol-1K-1。
Fixed adsorption temp is 298K, and porous carbon materials are 0.005g, 0.002g, and chrysoidine solution concentration is 200mg/l,
In the range of 2-12, ibid, research solution ph adsorbs the influence of chrysoidine to porous carbon materials to other conditions to solution ph.It is real
Test result and find that the adsorbance of solution ph chrysoidine in 2-6 rises to 399 by 324 mg/g when porous carbon materials are 0.005g
Mg/g, the adsorbance stabilization of solution ph chrysoidine in 6-12 is in 399 mg/g.When porous carbon materials are 0.002g, pH value of solution
The adsorbance of value chrysoidine in 2-6 rises to 818mg/g by 438 mg/g, the adsorbance of solution ph chrysoidine in 6-12 by
818mg/g rises to 900mg/g.Illustrate material to the absorption of chrysoidine more preferable close to effect in neutral or alkaline solution.
Fixed adsorption temp is 298K, and chrysoidine solution concentration is respectively 100 mg/l, 200 mg/l, 300 mg/l, is inhaled
The attached time is 1 ~ 180 minute, and ibid, research adsorption time adsorbs the influence of chrysoidine to porous carbon materials to other conditions.Experiment
Result finds that absorption reached balance in 2 minutes when chrysoidine concentration is 100mg/l, when chrysoidine concentration is 200mg/l
When, absorption reached balance in 10 minutes, and when chrysoidine concentration is 300mg/l, absorption reached balance in 20 minutes.By
Adsorption dynamics adsorption kinetics analog result under kinetic model Fitting Analysis, all conditions is false second-order kinetics Adsorption Model.
Fixed adsorption temp is 298K, and porous carbon materials are 0.01g, and chrysoidine solution concentration is 200 mg/l, other
Part ibid, porous carbon materials desorption and regeneration is carried out using ethanol, studies the circulation absorption ability of porous carbon materials.Experimental result is sent out
The clearance of chrysoidine is more than 95% during now porous carbon materials are during 7 circulation absorptions to solution.
Fixed adsorption temp is 298K, and porous carbon materials are 0.005g, is matched somebody with somebody with pure water, running water, river as solvent respectively
The chrysoidine solution that concentration is 100 mg/l, 200 mg/l is put, regulation pH value of solution is 8, and research porous carbon materials are really being water rings
To the adsorption capacity of chrysoidine dyestuff in border.Experimental result finds material to the chrysoidine dyestuff in pure water, running water and river
Adsorption capacity is essentially identical, to the clearance of dyestuff more than 95%, illustrates that there is material certain sizable application to be worth.
Embodiment 7
Porous carbon materials 0.005g prepared by embodiment 1 is 50mg/l-500mg/l with concentration, and volume is 10ml, solution ph
Methyl orange solution for 6 mixes, and fixed adsorption temp is 298K, absorption property of the research porous carbon materials to methyl orange dye.
Measuring porous carbon materials are 320mg/l to the adsorption capacity of methyl orange.
Embodiment 8
Methyl orange solution in embodiment 7 is replaced with into the rhodamine B solution that concentration is 50mg/l-500mg/l, other conditions are strictly according to the facts
Apply example 7, absorption property of the research porous carbon materials to rhodamine B.Measuring porous carbon is to the adsorption capacity of rhodamine B
685mg/l。
Embodiment 9
Methyl orange solution in embodiment 7 is replaced with into the crystal violet solution that concentration is 50-450mg/l, other conditions are as implemented
Example 7, absorption property of the research porous carbon materials to crystal violet.Measuring porous carbon materials are to the adsorption capacity of crystal violet
174mg/l。
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of the porous carbon of adsorbable organic dyestuff in wastewater, it is characterised in that carry out as steps described below：
A, activator is fully ground, then it is well mixed with the EDTA of fixed proportion；
B, mixture is activated 1.5-2.5 hours in the atmosphere of inert gases at 550-650 DEG C；
C, solid obtain porous carbon materials by ultrasound, filtering, washing, drying.
2. the preparation method of the porous carbon of organic dyestuff in wastewater is adsorbed as claimed in claim 1, it is characterised in that described
In step A, activator is inorganic strong alkali.
3. the preparation method of the porous carbon of organic dyestuff in wastewater is adsorbed as claimed in claim 2, it is characterised in that described
In step A, activator is potassium hydroxide.
4. the preparation method of the porous carbon of organic dyestuff in wastewater is adsorbed as claimed in claim 1, it is characterised in that described
In step A, the mass ratio of activator and EDTA is 1：（1.5-4）.
5. the preparation method of the porous carbon of organic dyestuff in wastewater is adsorbed as claimed in claim 1, it is characterised in that the activity
Charcoal is used in pH value in the solution of 6-12.
6. the preparation method of the porous carbon of organic dyestuff in wastewater is adsorbed as claimed in claim 1, it is characterised in that the present invention
Porous carbon desorption and regeneration after, the porous carbon of regeneration has circulation absorption ability.
7. the preparation method of the porous carbon of organic dyestuff in wastewater is adsorbed as claimed in claim 1, it is characterised in that described
In step B, mixture is activated 2 hours in the atmosphere of inert gases at 600 DEG C.
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Cited By (2)
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| CN109133051A (en) * | 2018-09-26 | 2019-01-04 | 桂林电子科技大学 | A kind of HEDTA base porous carbon materials and its preparation method and application |
| CN114618529A (en) * | 2022-04-06 | 2022-06-14 | 中国科学院大学 | Magnetic graphene-based photocatalyst GO-Fe3O4@SiO2@ CdS and preparation method and application thereof |
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| CN114618529A (en) * | 2022-04-06 | 2022-06-14 | 中国科学院大学 | Magnetic graphene-based photocatalyst GO-Fe3O4@SiO2@ CdS and preparation method and application thereof |
| CN114618529B (en) * | 2022-04-06 | 2023-09-22 | 中国科学院大学 | Magnetic graphene-based photocatalyst GO-Fe 3 O 4 @SiO 2 @CdS and preparation method and application thereof |
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Application publication date: 20170620 |