CN106925219A - A kind of preparation method of magnetic carbon composite adsorbing material - Google Patents
A kind of preparation method of magnetic carbon composite adsorbing material Download PDFInfo
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- 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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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention provides a kind of preparation method of magnetic carbon composite adsorbing material, it is that nitrogen substance and carbon material ultrasonic disperse are obtained into mixing suspension in solvent, it is added thereto to magnetic material precursor, under ultrasound condition it is fully dispersed after, 30~120 DEG C are heated to, mixing time is 1~8h, is separated, dry, obtain mix powder；It is fully ground after mix powder is processed into 0.5~8h at a high temperature of 120~900 DEG C under inert gas shielding again, crosses 20~300 mesh sieves, obtains final product magnetic carbon composite adsorbing material.The present invention prepare sorbing material there is low cost, absorption property is good, and absorption efficiency is high, recoverable often the features such as, elapsed time is short in the treatment of waste water, be dispersed in water after easily settle；Can decline with repeated application and absorption property again little by simple treatment after recovery, thus there is good economic worth in the treatment of waste water.
Description
Technical field
The present invention relates to a kind of adsorbent for dye wastewater treatment, more particularly to a kind of repeatable magnetic carbon for utilizing
The preparation of composite adsorbing material, belongs to technical field of composite materials and water-treatment technology field.
Background technology
Into after 21st century, with continuing to develop for industry, water pollution problems is increasingly sharpened, heavy metal in waste water
The pollution of the dyestuff of phenols and residual etc. is especially prominent in process of industrialization.Adsorption technology treatment sewage is current environmental pollution
One of common technology of improvement, adsorbent easy, safe and efficient can adsorb impurity and its harmful substance in waste water.Mesh
Preceding the most frequently used adsorbent is activated carbon, molecular sieve etc., but its suspension time in waste water is long, and free settling, does not cause it
Have the shortcomings that to reclaim difficult.
Research shows, if carbon material combined with the Dominant Facies of magnetic material, makes its both adsorptivity with carbon material
Can, but also with the function that magnetic material free settling is easily reclaimed, develop such material and be significant in water process.Especially
Exploitation obtains the economical magnetic adsorbent of NEW TYPE OF COMPOSITE of cheap, efficient, easy recovery, after repeatedly recycling, still can body
Reveal sewage treatment capacity higher.No matter all there is advantage from terms of financial cost, or for environment aspect.
The content of the invention
The purpose of the present invention is directed to the shortcoming that common adsorbents are not easily recycled, there is provided a kind of low cost, absorption efficiency be high,
The preparation method of the magnetic carbon composite adsorbing material that absorption property is good, recuperability is good.
（One）The preparation of magnetic composite adsorbent
Nitrogen substance and carbon material ultrasonic disperse are obtained into mixing suspension in solvent, magnetic material precursor is added thereto to, surpassed
Under the conditions of sound it is fully dispersed after, be heated to 30~120 DEG C, mixing time is 1~8h, is separated, and is dried, and obtains mix powder；Again
It is fully ground after mix powder is processed into 0.5~8h at a high temperature of 120~900 DEG C under inert gas shielding, excessively 20~
300 mesh sieves, obtain final product magnetic carbon composite adsorbing material.
The carbon material is at least one in graphite powder, activated carbon, CNT；Nitrogen substance be urea, ethylenediamine,
At least one in disodium ethylene diamine tetraacetate, ammonium polyphosphate, bipyridyl or melamine；Magnetic material precursor be iron oxide red,
Etal molysite（Such as iron chloride, ferric sulfate, ferric nitrate, high molecular polymerization molysite）, cobalt salt（Such as cobalt chloride, cobaltous sulfate, nitric acid
Cobalt）, rare earth material（NdCo3Or CeCe3）Or rare-earth salts（Cerous acetate, praseodymium acetate）In one kind；And carbon material, nitrogen substance, magnetic
Property material precursor mass ratio be 100: 60:20~100:80:50.
The solvent is the one kind in methyl alcohol, water, tetrahydrofuran, acetonitrile.
The drying is dried in 50~90 DEG C of baking oven；The inert gas be nitrogen, argon gas, in xenon at least
It is a kind of.
（Two）The sign of magnetic carbon composite adsorbing material
1st, XRD is characterized
Fig. 1 is the X-ray diffractogram of magnetic carbon composite adsorbing material prepared by the present invention.From figure 1 it appears that economical magnetic
Property adsorbent only has two characteristic peaks of carbon, respectively at 25 ° and 45 ° or so, corresponding to carbon material（002）With（001）It is brilliant
Face；Again without other characteristic peaks, this is formd caused by mainly amorphous structure mainly due to heating process.
2nd, BET is characterized
Fig. 2 is the specific surface area figure of economical magnetic adsorbent prepared by the present invention.From figure 2 it can be seen that prepared by the present invention
Magnetic carbon composite adsorbing material there is obvious sluggishness tropic characteristic, illustrate that its internal pore structure enriches, specific surface area is big
（Reach 59.82 m2g-1）, for there is preferable adsorption function to provide guarantee for it.
3rd, magnetic characterization
Fig. 3 is the magnetic characterization of economical magnetic adsorbent prepared by the present invention.From figure 3, it can be seen that prepared by the present invention
The coercivity of magnetic carbon composite adsorbing material is up to 55.38 Oe, can be that the magnetic recovery of adsorbent provides safeguard.
（Three）The absorption property of magnetic carbon composite adsorbing material
Suction-operated of the magnetic adsorbent to methylene blue：Respectively in 10mg/L, in the methylene blue solution of 15mg/L, 20mg/L
The magnetic adsorbent of 50mg is added to absorb it, Fig. 4（1）The adsorbance to methylene blue and time for magnetic adsorbent
Graph of a relation.From the graph, it is apparent that the suction speed within 20 minutes is most fast, it is almost full in absorption within an hour
With, and have adsorbance higher.Fig. 4（2）The clearance of methylene blue and the relation of time are absorbed for magnetic adsorbent.Can be with
Find out, clearance has nearly reached 100% in the short period of time, hereafter the change of clearance is extremely slow, illustrates magnetic absorption
The absorption property of agent is fine.
Suction-operated of the magnetic adsorbent to acid blue 80：Respectively in 10mg/L, the acid blue 80 of 15mg/L, 20mg/L is molten
The economical magnetic adsorbent of 50mg is added to absorb it in liquid.Fig. 5（1）Absorption for magnetic adsorbent to acid blue 80
Amount and the graph of a relation of time.It can be seen that absorption of the magnetic adsorbent to acid blue 80 is more delayed compared to methylene blue
Slowly, but having also nearly reached adsorption saturation within an hour, and there is adsorbance higher.Fig. 5（2）To absorb acid blue 80
Clearance and time relation.As can be seen that clearance has reached 60% in the short period of time, hereafter clearance is in always
Ascendant trend, illustrates the absorption property of magnetic adsorbent preferably, has been at absorbing state, reaches the time of clearance higher
At two more than hour.
Fig. 6 is the recycling figure that magnetic adsorbent prepared by the present invention absorbs to acid blue 80.As seen from Figure 6,
Recycling efficiency of the invention is fabulous, still can keep clearance higher after recycling every time, and reclaim every time
Loss can not ignore, reuse 15 times afterwards, clearance may also stay at more than 50%.
In sum, the present invention has advantages below compared with the prior art：
1st, sorbing material prepared by the present invention has absorption property good, and adsorption capacity is big, and absorption efficiency is high, recoverable number of times
It is many；
2nd, elapsed time is short in the treatment of waste water for sorbing material prepared by the present invention, is easily settled after being dispersed in water, not
Be can be used under same water process environment；
3rd, the adsorbent recycling performance that prepared by the present invention is good, and waste water is may apply to again by simple treatment after recovery
In treatment, and absorption property declines less；
4th, preparation process is simple of the present invention, raw material is cheap and easy to get, with good cost advantage.
Brief description of the drawings
Fig. 1 is the X-ray diffraction of economical magnetic adsorbent of the invention（XRD）Figure.
Fig. 2 is the specific surface area of economical magnetic adsorbent of the invention（BET）Figure.
Fig. 3 is economical magnetic adsorbent magnetic characterization of the invention.
Fig. 4 is magnetic adsorbent of the present invention to the adsorbance of methylene blue and the graph of a relation of time（1）And clearance and when
Between relation（2）.
Fig. 5 is magnetic adsorbent of the present invention to the adsorbance of acid blue 80 and the graph of a relation of time（1）And clearance and when
Between relation（2）.
Fig. 6 is the magnetic adsorbent of present invention preparation to methylene blue（1）With acid blue 80（2）The recycling of absorption
Figure.Specific embodiment
Economical magnetic adsorbent performance prepared by the present invention is described further below by specific embodiment.
Nitrogen substance and carbon material ultrasonic disperse are obtained into mixing suspension in solvent, before being added thereto to magnetic material
Body, it is fully dispersed under ultrasound condition after, be heated to 30~120 DEG C, mixing time is 1~8h, is separated, and is dried, and obtains mixture powder
End；It is fully ground after mix powder is processed into 0.5~8h at a high temperature of 120~900 DEG C under inert gas shielding again, mistake
20~300 mesh sieves, obtain final product magnetic carbon composite adsorbing material.
Embodiment 1
10g ammonium polyphosphates are added among the tetrahydrofuran of 300mL and are well mixed；Afterwards by the graphite powder ultrasound point of 10g
It is scattered to wherein obtain mixing suspension；0.6g ferric sulfate is dissolved into 200mL tetrahydrofurans and is added under ultrasound condition
State in mixing suspension, stir 8h at being heated to 80 DEG C, suction filtration obtains mixture and first dries 12h in an oven obtaining mixture powder
End；Then mix powder is placed in tube furnace, in treatment 6 hours at 600 DEG C under argon gas protection（Programming rate be 5 DEG C/
min）, it is fully ground afterwards, sieve 200 mesh, obtains 20.6g magnetic carbon composite adsorbing materials.The sorbing material is to methylene blue
Clearance can reach 92% or so first, and clearance is maintained at more than 50% afterwards for Reusability 15 times.
Embodiment 2
2g urea is added among the methyl alcohol of 100mL and is well mixed, then by the activated carbon ultrasonic disperse of 8g to must wherein mix
Suspension；In being dissolved into 10g cobalt chlorides in 100mL methyl alcohol and add it under ultrasound condition above-mentioned mixing suspension,
Be heated to 30 DEG C of stirring 8h, suction filtration obtains mixture and dry 8h in an oven, be subsequently placed in tube furnace, under nitrogen protection
Processed 6 hours at 1000 DEG C（Programming rate is 20 DEG C/min）, it is fully ground afterwards, sieve 100 mesh, obtains 20g magnetic carbons and answers
Close sorbing material.To acid blue, clearance can reach 95% or so to the sorbing material first, the clearance afterwards of Reusability 15 times
It is maintained at more than 45%.
Embodiment 3
5g bipyridyl ammoniums are added among the hot water of 100mL and are well mixed；Again by the CNT ultrasonic disperse of 8g to wherein
Obtain mixing suspension；By 10g magnetic CeCo3It is distributed in 100mL water and above-mentioned mixing is added it under ultrasound condition
In suspension；70 DEG C of stirring 5h are heated to, suction filtration, the mixture for obtaining first dries 5h, is subsequently placed in tube furnace, nitrogen in an oven
Processed 4 hours at 500 DEG C under gas shielded（Programming rate is 1 DEG C/min）, it is fully ground afterwards, sieve 150 mesh, obtains 16g magnetic
Property carbon composite adsorbing material.To acid blue, clearance can reach 90% or so to the sorbing material first, and Reusability 12 times is afterwards
Clearance is maintained at more than 50%.
Embodiment 4
The ethylenediamine of 5mL is added among the hot water of 100mL and is well mixed, then by the activated carbon ultrasonic disperse of 8g to wherein must
Mixing suspension；In being dissolved into 10g praseodymium acetates in 100mL water and add under ultrasound condition above-mentioned mixing suspension, heating
To 90 DEG C of stirring 4h, suction filtration, the mixture for obtaining first dries 8h, is subsequently placed in tube furnace in an oven, 800 after mixing nitrogen
Processed 1 hour at DEG C（Programming rate is 8 DEG C/min）, it is fully ground afterwards, sieve 150 mesh, obtains 16g carbon composite adsorption materials
Material.The sorbing material is to acid blue and methyl blue mixed liquor（Mol ratio 1:1）Clearance can reach 98% or so first, repeatedly
Using 10 times afterwards clearance be maintained at more than 70%.
Embodiment 5
The sodium ethylene diamine tetracetate of 5g is added in the acetonitrile of 100mL and is well mixed；The activated carbon ultrasonic disperse of 8g is arrived again
Wherein obtain mixing suspension；10g ferric nitrates are dissolved into 100mL acetonitriles and above-mentioned mix suspending is added under ultrasound condition
In liquid, 110 DEG C of stirring 8h are heated to, suction filtration, the mixture for obtaining first dries 2h, be subsequently placed in tube furnace, mixes in an oven
Argon gas, is processed 1 hour at 950 DEG C（Programming rate is 8 DEG C/min）, it is fully ground afterwards, sieve 150 mesh, obtains 20g carbon and is combined
Sorbing material.To acid blue, clearance can reach 92% or so to the sorbing material first, and clearance is protected afterwards for Reusability 10 times
Hold more than 40%.
Embodiment 6
The urea of 5g is added among the hot water of 100mL and is well mixed, then by the activated carbon ultrasonic disperse of 12g to wherein obtaining
Mixing suspension；4g iron chloride 6g and cobaltous sulfate are dissolved into 100mL water, and above-mentioned mix suspending is added under ultrasound condition
In liquid, 100 DEG C of stirring 8h are heated to, suction filtration, the mixture for obtaining first dries 8h, be subsequently placed in tube furnace, mixes in an oven
Nitrogen, is processed 6 hours at 1000 DEG C（Programming rate is 20 DEG C/min）, it is fully ground afterwards, sieve 150 mesh, obtains 26g carbon
Composite adsorbing material, the sorbing material is to acid blue and methyl blue mixed liquor（Mol ratio 1:2）Clearance can reach 98% first
Left and right, clearance is maintained at more than 50% afterwards for Reusability 20 times.
Claims (10)
1. a kind of preparation method of magnetic carbon composite adsorbing material, is that nitrogen substance and carbon material ultrasonic disperse are obtained in solvent
Mixing suspension, is added thereto to magnetic material precursor, it is fully dispersed under ultrasound condition after, be heated to 30~120 DEG C, during stirring
Between be 1~8h, separate, dry, obtain mix powder；Again under inert gas shielding by mix powder in 120~900 DEG C
It is fully ground after processing 0.5~8h under high temperature, crosses 20~300 mesh sieves, obtains final product magnetic carbon composite adsorbing material.
2. the preparation method of magnetic carbon composite adsorbing material as claimed in claim 1, it is characterised in that：The nitrogen substance is urine
At least one in element, ethylenediamine, disodium ethylene diamine tetraacetate, ammonium polyphosphate, bipyridyl or melamine.
3. the preparation method of magnetic carbon composite adsorbing material as claimed in claim 1, it is characterised in that：The carbon material is graphite
At least one in powder, activated carbon, CNT.
4. the preparation method of magnetic carbon composite adsorbing material as claimed in claim 1, it is characterised in that：The magnetic material precursor
It is the one kind in iron oxide red, etal molysite, cobalt salt, rare earth material or rare-earth salts.
5. the preparation method of magnetic carbon composite adsorbing material as claimed in claim 4, it is characterised in that：The molysite is chlorination
Iron, ferric sulfate, ferric nitrate or high molecular polymerization molysite.
6. the preparation method of magnetic carbon composite adsorbing material as claimed in claim 4, it is characterised in that：The cobalt salt is chlorination
Cobalt, cobaltous sulfate or cobalt nitrate.
7. the preparation method of magnetic carbon composite adsorbing material as claimed in claim 4, it is characterised in that：The rare earth material is
NdCo3Or CeCe3。
8. the preparation method of magnetic carbon composite adsorbing material as claimed in claim 4, it is characterised in that：The rare-earth salts is acetic acid
Cerium or praseodymium acetate.
9. as described in claim 1 ~ 8 any magnetic carbon composite adsorbing material preparation method, it is characterised in that：The carbon
Material, nitrogen substance, the mass ratio of magnetic material precursor are 100: 60:20~100:80:50.
10. as described in claim 1 ~ 8 any magnetic carbon composite adsorbing material preparation method, it is characterised in that：It is described
Solvent is the one kind in methyl alcohol, water, tetrahydrofuran, acetonitrile.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107349905A (en) * | 2017-08-30 | 2017-11-17 | 华南理工大学 | The method that a kind of nitrogen co-doped magnetic carbon material of fluorine removes hexavalent chromium in industrial wastewater |
| CN107774261A (en) * | 2017-11-01 | 2018-03-09 | 枣庄学院 | A kind of preparation method of heterogeneous type Fenton catalyst Co/C composites |
| CN108636338A (en) * | 2018-05-11 | 2018-10-12 | 杭州诚洁环保有限公司 | A kind of Fe/C complex solids adsorbent and its preparation method and application |
| CN109772258A (en) * | 2019-03-13 | 2019-05-21 | 厦门大学 | A kind of preparation method of magnetism fluorinated carbon nanomaterial |
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| CN108636338B (en) * | 2018-05-11 | 2020-09-29 | 杭州诚洁环保有限公司 | Fe/C composite solid adsorbent and preparation method and application thereof |
| CN109772258A (en) * | 2019-03-13 | 2019-05-21 | 厦门大学 | A kind of preparation method of magnetism fluorinated carbon nanomaterial |
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