CN105217715B - A kind of method that absorbent charcoal material removes processing antibiotic sulfacetamide - Google Patents
A kind of method that absorbent charcoal material removes processing antibiotic sulfacetamide Download PDFInfo
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- CN105217715B CN105217715B CN201510707517.9A CN201510707517A CN105217715B CN 105217715 B CN105217715 B CN 105217715B CN 201510707517 A CN201510707517 A CN 201510707517A CN 105217715 B CN105217715 B CN 105217715B
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- sulfacetamide
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Abstract
The present invention relates to a kind of method that absorbent charcoal material removes processing antibiotic sulfacetamide, activated carbon and hydrogen peroxide solution are added first in sulfacetamide solution, the wherein ratio of sulfacetamide, activated carbon and hydrogen peroxide is 0.3875 μm of ol：(6~7.5) mg：(8~12) μm ol, 20~100min is then handled at room temperature, complete the removal processing of antibiotic sulfacetamide.The present invention is by using absorbent charcoal material; concerted catalysis effect can be produced with hydrogen peroxide; remove antibiotic sulfacetamide; remove in processing procedure; the problem of chemical method secondary pollution and cost height etc. can be avoided; and it is easy to operate, processing method of the present invention only needs at room temperature to add the absorbent charcoal material in sulfacetamide solution, greatly simplifies industrial treatment step；Meanwhile the absorbent charcoal material reclaims convenience, suitable for commercial Application in itself, the industrial removal especially suitable for antibiotic sulfacetamide is handled.
Description
【Technical field】
The invention belongs to the processing technology field of antibioticses waste water, and in particular to it is anti-that a kind of absorbent charcoal material removes processing
The method of raw plain sulfacetamide.
【Background technology】
Antibiotic refers to that biological (plant, animal or microorganism) produces in life process or by external world's acquisition, energy
The organic substance of other biological activity is selectively influenceed or suppressed under humble concentration.Antibiotic because of its unique drug effect,
Critical role is occupied in field of medicaments.The 3rd is occupied in mankind's medical usage amount, accounts for more than the 6% of prescription medicine total amount,
It is even more to account for more than 70% in veterinary drug dosage, wherein China is antibiotics production and the big country that uses.Antibiotic has volatilization
The features such as property is poor, vapour pressure is small low with hydrophobicity, so, its transfer in the environment is mainly based on water and food chain.Largely
Use antibiotic so that it is constantly detected in the environment, already become one of emerging pollutant.At present for anti-
The minimizing technology of raw element is not also very ripe, so can detect its residual in each environmental system.The abuse of antibiotic is led
It is caused constantly to enter in environment, however, most antibiotic can not be by the microorganism in environment or institute of sewage treatment plant
Processing.Therefore, increasing report shows that the Water Environment Systems such as surface water, river, drinking water, hospital wastewater detect antibiosis
Element residual.Long-term being present in environment of antibiotic can not only cause bacterium to produce drug resistance, can also be as food chain is in dynamic, plant
Accumulated in thing and human body, so as to threaten the health of animals and plants or even human body.So the removal of antibiotic in recent years be processed into order to
The hot fields of research.
At present, mainly have to the processing method of antibiotic：Traditional treatment method, physical method, chemical oxidization method.At tradition
Reason method includes activated sludge method, filtering and sedimentation etc..Activated sludge method is because its is simple to operate, low cost and other advantages extensively should
For most of sewage treatment plant.But activated sludge method is applied to extensive sewage disposal, and treatment effect is bad.Change
Method refers to add some chemical reagent in system and carry out a series of chemical reaction, main so as to reach removal purpose
There are chemical oxidization method and electrochemical process.The advantages of chemical treatment method be the operation cycle it is short and oxidation ratio more thoroughly, it is this
Method is also relatively more suitable for the processing of the higher pollutant of concentration, but is easy to produce secondary dirt after chemical oxidization method processing
Dye, and the cost of chemical oxidization method is higher, application is poor, and this greatly limits its answering in terms of environmental contaminants processing
With.Conventional physical method mainly includes absorption, ultrafiltration, UF membrane and ion exchange etc..It is journey using the advantages of physical method
Sequence is simple, workable, and cost is relatively low, quick.Wherein activated carbon (AC) is a kind of conventional adsorbent, and it has hole
The features such as structure is flourishing, specific surface area is high, chemical property is stable.
【The content of the invention】
It is an object of the invention to overcome above-mentioned problems of the prior art, there is provided at a kind of absorbent charcoal material removal
The method for managing antibiotic sulfacetamide, synergy is produced using activated carbon and hydrogen peroxide, can effectively remove antibiotic acetyl
Sulfanilamide (SN).
The technical scheme is that：
Activated carbon and hydrogen peroxide solution, wherein sulfacetamide, activated carbon and dioxygen are added first in sulfacetamide solution
The ratio of water is 0.3875 μm of ol：(6~7.5) mg：(8~12) μm ol, 20~100min is then handled at room temperature, complete antibiosis
The removal processing of plain sulfacetamide.
Further, the preparation process of activated carbon includes：
(1) clean walnut shell is taken to be placed in H after crushing3PO4In solution, carried out after impregnating 14.5~15.5h at 90~95 DEG C
Dry, obtain H3PO4Impregnant；
(2) by H3PO4Impregnant is activated in 240~250 DEG C of insulation charings, then at 490~500 DEG C, and activation is completed
Afterwards, in N2Protection decline warms to room temperature, and obtains activated material；
(3) activated material is subjected to pickling, is then washed to neutrality, activated carbon is obtained after drying.
Further, walnut shell clean in step (1) is walnut shell through washing, is then obtained in 80~85 DEG C of dry 48h
Arrive.
Further, H when being impregnated in step (1)3PO4Mass ratio with walnut shell is (1~4)：1.
Further, the drying after being impregnated in step (1) is in 120~125 DEG C of dry 12~13h.
Further, carbonization time and soak time are 60~70min in step (2).
Further, pickling is that activated material is placed in triangular flask in step (3), and it is molten to add the HCl that mass concentration is 1%
Liquid, it is placed in shaking table and 180~200min is shaken with 120r/min.
Further, the washing in step (3) is carried out using 75~85 DEG C of deionized water, drying be 120~
125 DEG C of dry 24h.
Further, the concentration of sulfacetamide solution is 155 μm of ol/L.
Further, the concentration of hydrogen peroxide solution is 0.2mol/L.
Compared with prior art, the present invention has technique effect beneficial below：
For the present invention by using absorbent charcoal material, the material has flourishing pore structure, specific surface area height, chemical property steady
The features such as determining, concerted catalysis effect can be produced with hydrogen peroxide, antibiotic sulfacetamide is removed, removes in processing procedure, can
The problem of avoiding chemical method secondary pollution and cost height etc., and sulfacetamide can be degraded, processing method of the present invention is only
The absorbent charcoal material need to be added in sulfacetamide solution at room temperature, greatly simplify industrial treatment step, operation is easy；Together
When, the absorbent charcoal material reclaims convenience, suitable for commercial Application in itself, at the industrial removal of antibiotic sulfacetamide
Reason, degradation rate are up to 57.59%；The method for being currently based on charcoal absorption-catalytic elimination antibiotic sulfacetamide yet there are no report
Road.
Further, the present invention prepares activated carbon using walnut shell, and preparing raw material is cheap and easy to get, by impregnating and activating
Step, preparation process is simple, and the time is short, and cost is low, and the activated carbon of gained has huge specific surface area, and specific surface area can reach
727.1112m2/ g, has an efficient absorption removal ability, and recovery is convenient, suitable for commercial Application, has considerable economic benefit and wide
Wealthy application prospect.
【Brief description of the drawings】
Fig. 1 is the scanning electron microscope (SEM) photograph of the absorbent charcoal material prepared in the embodiment of the present invention 1 by walnut shell, and multiplication factor is
2400 times.
Fig. 2 be absorbent charcoal material obtained by the embodiment of the present invention 1 and hydrogen peroxide in 20~100min to 155 μm of ol/L
Clearance-time diagram of sulfacetamide.
Fig. 3 is that the absorbent charcoal material adsorption treatment process obtained by the embodiment of the present invention 1 reuses number with going relatively
Except the graph of a relation of rate
Fig. 4 is that absorbent charcoal material absorption-catalytic treating process obtained by the embodiment of the present invention 1 reuses number and phase
To the graph of a relation of clearance.
【Embodiment】
The preparation of activated carbon of the present invention and applying step are as follows：
1st, the preparation of activated carbon (AC) material
(1) walnut shell pre-processes：Walnut shell is put into baking oven in 80~85 DEG C of dry 48h, crushed through washing dedusting and sandstone
It is 40~120 mesh to particle diameter, obtains walnut shell powder, be placed in drier and save backup.
(2)H3PO4It is prepared by impregnant：Accurately weigh walnut shell powders of the 5g through pulverizer pulverization process to be placed in beaker, Xiang Qi
Middle addition 25mL H3PO4Solution, H3PO4Ratio with walnut shell quality is (1~4)：1, sealed after being sufficiently stirred, in baking oven 90~
95 DEG C of 14.5~15.5h of dipping, remove sealing, in 120~125 DEG C of dry 12~13h of baking oven, and stir it is loose, such as every 2~
3h is stirred once；H is obtained after drying3PO4Impregnant.
(3) prepared by activated material：By H3PO4Impregnant moves to tube-type atmosphere furnace calcining at constant temperature, and experiment is warming up to 10 DEG C/min
240~250 DEG C of carbonization temperature is set, after insulation charing to 60~70min of experiment setting carbonization time, with identical heating rate
Experiment 490~500 DEG C of activation temperature of setting is warming up to, 60~70min is incubated, after the completion of question response, in N2It is cooled under protection
Room temperature, obtain activated material.Activated material is transferred in triangular flask, add 50mL mass concentration 1%HCl solution, be placed in shaking table with
120r/min shakes 180~200min and carries out pickling.It is neutral to be washed again with 75~85 DEG C of deionized waters to pH, in baking oven
120~125 DEG C of dry 24h, obtain walnut shell activated carbon, are placed in drier and save backup.
2nd, activated carbon (AC) material resistant gives birth to the removal processing of plain sulfacetamide
The 155 μm of ol/L antibiotic sulfacetamide aqueous solution is prepared, is centrifuged to the 10ml containing 2.5mL sulfacetamide solution
Activated carbon (AC) material prepared by 6.0~7.5mg walnut shells is added in pipe, absorption-catalyzing cooperation effect processing is treated
The H that 40~60 μ L concentration are 0.2mol/L is added in journey2O2Trigger degraded, by calculating, draw sulfacetamide, walnut shell activity
The ratio of charcoal and hydrogen peroxide is 0.3875 μm of ol：(6.0~7.5) mg：(8~12) μm ol；It is placed in water bath with thermostatic control concussion and is inhaled
Attached removal processing, handles 20~100min at room temperature, completes the removal processing of antibiotic sulfacetamide.
Using the characteristic absorption peak of UV-VIS spectrophotometry detection different periods sulfacetamide, pass through the extinction number of degrees
Value calculates clearance, evaluates the performance of prepared activated carbon (AC) material.
(3) antibiotic sulfacetamide clearance η is calculated
Antibiotic sulfacetamide clearance η is calculated as follows：
η=[(A0-At)/A0] × 100%
η is sulfacetamide clearance in formula, A0It is the initial absorbance of sulfacetamide characteristic wavelength, AtWhen being adsorption treatment t
Between after sulfacetamide absorbance.
The characteristic absorption wavelength of sulfacetamide is 262nm.
The present invention is described in more detail with reference to the accompanying drawings and examples, but the present invention is not limited only to these implementations
Example.
Embodiment 1
It is prepared by activated carbon：Accurately weigh walnut shell powders of the 5g through pulverizer pulverization process to be placed in beaker, add thereto
25mL H3PO4Solution, H3PO4Mass ratio with walnut shell is 4:1, seal after being sufficiently stirred, in 90 DEG C of dipping 15h of baking oven, go
Fall sealing, in 120 DEG C of dry 12h of baking oven, and every 2h stirrings once, progress is loose, obtains H after drying3PO4Impregnant.Will
H3PO4Impregnant moves to tube-type atmosphere furnace constant temperature zone, and experiment 250 DEG C of carbonization temperature of setting, insulation charing are warming up to 10 DEG C/min
To experiment setting carbonization time 60min, experiment 500 DEG C of activation temperature of setting, insulation are warming up to identical heating rate
60min, after the completion of question response, in N2Protection decline warms to room temperature, and obtains activated material, activated material is transferred in triangular flask, add
Enter 50mL mass concentration 1%HCl solution, be placed in shaking table and pickling is carried out with 120r/min concussions 180min.Again with 80 ± 5 DEG C go from
Sub- water washing is neutrality to pH, and 120~125 DEG C of dry 24h, finally give target product activated carbon A in baking oven.
Electron-microscope scanning is carried out to target product activated carbon A, as a result as shown in Figure 1, it can be seen that the target product activity of preparation
Charcoal C belongs to loose porous structure, has larger specific surface area, and nitrogen adsorption test shows that its specific surface area can reach
727.1112m2/g。
7.5mg materials are added into the 10ml centrifuge tubes containing the sulfacetamide aqueous solution that 2.5mL concentration is 155 μm of ol/L
A, it is placed at room temperature in water-bath concussion and is removed processing.Adsorption treatment is directly to handle 20~100min at room temperature, absorption-
Catalyzing cooperation effect processing is that the H that 50 μ L concentration are 0.2mol/L is added in catalytic process2O2Trigger degraded, processing time is
20~100min, the clearance of sulfacetamide is calculated, its result is as shown in Figure 2.
From Fig. 2 it can be found that as time went on, the clearance of absorption and absorption-catalysis increases, but inhale
Attached-catalyzing cooperation effect clearance is of a relatively high, and only adds the system for handling of hydrogen peroxide not have obvious catalytic effect, only inhales
When attached, adsorption rate 40.03%, during absorption-catalysis collective effect, clearance 56.01%.It is several during as individually added hydrogen peroxide
Catalytic action can not be played to sulfacetamide.
By using the target product A of treated sulfacetamide, respectively by the step of embodiment one and condition repeat into
Row adsorption treatment and absorption-catalyzing cooperation effect processing, see first time adsorption treatment and the clearance of absorption-catalytic treatment
Into 100%, during reuse, equally weighed with relative clearance clearance each time later by comparison
Reusability.Its result is as shown in Figure 3 and Figure 4.It can be seen that increasing with number is reused, absorption and
Situation about gradually reducing all is presented in the relative clearance of absorption-catalysis.After simple adsorption process is reused 4 times, its is relative
Clearance declines comparatively fast more than 50%, shows that charcoal absorption sulfacetamide tends to saturation.Relative to individually adsorbing
Journey, absorption-catalytic process the clearance of sulfacetamide is declined it is relatively slow, after reusing 10 times, with respect to clearance according to
So more than 50%, show and adsorb incomparable advantage, show in absorption-catalytic process, sulfacetamide is in activated carbon
It is degraded with the collective effect of hydrogen peroxide, rather than simple absorption.
Embodiment 2
Preparing H3PO4During impregnant, H3PO4Mass ratio with walnut shell is 2:1, other conditions and step with
Embodiment one is identical, and target product activated carbon B is made.
Adsorption treatment is carried out to sulfacetamide using target product activated carbon B and absorption-catalyzing cooperation effect is handled, condition
It is identical with embodiment one with step, the clearance of sulfacetamide is calculated, when discovery is only adsorbed, adsorption rate 27.99%, is inhaled
During attached-catalysis collective effect, degradation rate 41.67%.
Embodiment 3
Preparing H3PO4During impregnant, H3PO4Mass ratio with walnut shell is 1:1, other conditions and step with
Embodiment one is identical, and target product activated carbon C is made.
Adsorption treatment is carried out to sulfacetamide using target product activated carbon C and absorption-catalyzing cooperation effect is handled, condition
It is identical with embodiment one with step, found through overtesting, as time went on, the clearance of sulfacetamide gradually increases.
Under conditions of not adding hydrogen peroxide, highest adsorption rate only has 13.66%, and when absorption and catalysis act synergistically, the
During 100min, degradation rate can reach 21.22%.
Embodiment 4
It is prepared by activated carbon：Accurately weigh walnut shell powders of the 5g through pulverizer pulverization process to be placed in beaker, add thereto
25mL H3PO4Solution, H3PO4Mass ratio with walnut shell is 2:1, sealed after being sufficiently stirred, in baking oven, 93 DEG C impregnate 14.5h,
Remove sealing, in 123 DEG C of dry 12.5h of baking oven, and every 2.5h stirrings once, progress is loose, obtains H after drying3PO4Leaching
Stain material.By H3PO4Impregnant moves to tube-type atmosphere furnace constant temperature zone, and experiment 240 DEG C of carbonization temperature of setting is warming up to 10 DEG C/min,
After insulation charing sets carbonization time 65min to experiment, experiment setting activation temperature 490 is warming up to identical heating rate
DEG C, 65min is incubated, after the completion of question response, in N2Protection decline warms to room temperature, and obtains activated material, activated material is transferred into triangle
In bottle, 50mL mass concentration 1%HCl solution is added, shaking table is placed in and pickling is carried out with 120r/min concussions 190min.Again with 80 ±
It is neutrality that 5 DEG C of deionized waters, which are washed to pH, and 120 DEG C of dry 24h, finally give target product activated carbon D in baking oven.
6mg material D are added into the 10ml centrifuge tubes containing the sulfacetamide aqueous solution that 2.5mL concentration is 155 μm of ol/L,
And 40 μ L concentration be 0.2mol/L H2O2Trigger degraded, processing time 100min.Calculate the degradation rate of sulfacetamide, drop
Solution rate is 31.52%.
Embodiment 5
It is prepared by activated carbon：Accurately weigh walnut shell powders of the 5g through pulverizer pulverization process to be placed in beaker, add thereto
25mL H3PO4Solution, H3PO4Mass ratio with walnut shell is 4:1, sealed after being sufficiently stirred, in baking oven, 95 DEG C impregnate 15.5h,
Remove sealing, in 125 DEG C of dry 13h of baking oven, and every 3h stirrings once, progress is loose, obtains H after drying3PO4Impregnant.
By H3PO4Impregnant moves to tube-type atmosphere furnace constant temperature zone, is warming up to experiment 245 DEG C of carbonization temperature of setting with 10 DEG C/min, is incubated charcoal
Change to experiment setting carbonization time 70min, experiment 495 DEG C of activation temperature of setting, insulation are warming up to identical heating rate
70min, after the completion of question response, in N2Protection decline warms to room temperature, and obtains activated material, activated material is transferred in triangular flask, add
Enter 50mL mass concentration 1%HCl solution, be placed in shaking table and pickling is carried out with 120r/min concussions 200min.Again with 80 ± 5 DEG C go from
Sub- water washing is neutrality to pH, and 125 DEG C of dry 24h, finally give target product activated carbon E in baking oven.
7mg materials E and 60 is added into the 10ml centrifuge tubes of the sulfacetamide aqueous solution containing 155 μm of ol/L of 2.5mL
μ L concentration is 0.2mol/L H2O2Trigger degraded, processing time 100min.The degradation rate of sulfacetamide is calculated, degradation rate is
57.59%.
Absorbent charcoal material of the present invention is simple to operate to the removal processing of sulfacetamide antibiotic, applicability is strong, and prepares
Material category waste reuses, and economizes on resources, reduces cost.
Claims (7)
1. a kind of method that absorbent charcoal material removes processing antibiotic sulfacetamide, it is characterised in that：It is molten in sulfacetamide first
Activated carbon and hydrogen peroxide solution are added in liquid, the wherein ratio of sulfacetamide, activated carbon and hydrogen peroxide is 0.3875 μm of ol：(6~
7.5)mg：(8~12) μm ol, 20~100min is then handled at room temperature, complete the removal processing of antibiotic sulfacetamide；
The preparation process of activated carbon includes：
(1) clean walnut shell is taken to be placed in H after crushing3PO4In solution, done after impregnating 14.5~15.5h at 90~95 DEG C
It is dry, obtain H3PO4Impregnant；H during dipping3PO4Mass ratio with walnut shell is (1~4)：1；
(2) by H3PO4Impregnant in 240~250 DEG C of insulation 60~70min of charing, then carry out at 490~500 DEG C activation 60~
70min, after the completion of activation, in N2Protection decline warms to room temperature, and obtains activated material；
(3) activated material is subjected to pickling, is then washed to neutrality, activated carbon is obtained after drying.
2. the method that a kind of absorbent charcoal material according to claim 1 removes processing antibiotic sulfacetamide, its feature exist
In：Clean walnut shell is walnut shell through washing in step (1), is then obtained in 80~85 DEG C of dry 48h.
3. the method that a kind of absorbent charcoal material according to claim 1 removes processing antibiotic sulfacetamide, its feature exist
In：Drying after being impregnated in step (1) is in 120~125 DEG C of dry 12~13h.
4. the method that a kind of absorbent charcoal material according to claim 1 removes processing antibiotic sulfacetamide, its feature exist
In：Pickling is that activated material is placed in triangular flask in step (3), adds the HCl solution that mass concentration is 1%, is placed in shaking table
180~200min is shaken with 120r/min.
5. the method that a kind of absorbent charcoal material according to claim 1 removes processing antibiotic sulfacetamide, its feature exist
In：Washing in step (3) is carried out using 75~85 DEG C of deionized water, and drying is in 120~125 DEG C of dry 24h.
6. the method that a kind of absorbent charcoal material according to claim 1 removes processing antibiotic sulfacetamide, its feature exist
In：The concentration of sulfacetamide solution is 155 μm of ol/L.
7. the method that a kind of absorbent charcoal material according to claim 1 removes processing antibiotic sulfacetamide, its feature exist
In：The concentration of hydrogen peroxide solution is 0.2mol/L.
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| CN105948158A (en) * | 2016-06-03 | 2016-09-21 | 上海大学 | Method for removing antibiotic-sulfadiazine in water through activated carbon fiber adsorbent |
| CN108373146A (en) * | 2018-04-27 | 2018-08-07 | 哈尔滨工业大学 | A kind of algae-residue charcoal and the preparation method and application thereof |
| CN115196616B (en) * | 2022-08-04 | 2023-08-11 | 山东农业大学 | Magnesium salt modified biochar material and application thereof in reducing abundance of antibiotic resistance genes |
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| CN102423688B (en) * | 2011-08-26 | 2013-04-03 | 昆明理工大学 | Preparation method for walnut shell active carbon adsorbent for purifying low concentration phosphine |
| CN103011155A (en) * | 2013-01-05 | 2013-04-03 | 湖南奇异生物科技有限公司 | Method for preparing activated carbon by utilizing camellia oleifera shells |
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