CN109759016A - Preparation and use method of renewable waste clay-based activated carbon for adsorption and removal of antibiotics in water - Google Patents
Preparation and use method of renewable waste clay-based activated carbon for adsorption and removal of antibiotics in water Download PDFInfo
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- CN109759016A CN109759016A CN201910143238.2A CN201910143238A CN109759016A CN 109759016 A CN109759016 A CN 109759016A CN 201910143238 A CN201910143238 A CN 201910143238A CN 109759016 A CN109759016 A CN 109759016A
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- activated carbon
- waste clay
- water
- based activated
- antibiotics
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000004927 clay Substances 0.000 title claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000002699 waste material Substances 0.000 title claims abstract description 27
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003242 anti bacterial agent Substances 0.000 title claims abstract 12
- 229940088710 antibiotic agent Drugs 0.000 title claims abstract 12
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000000197 pyrolysis Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000011069 regeneration method Methods 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000004098 Tetracycline Substances 0.000 claims description 3
- 150000007660 quinolones Chemical class 0.000 claims description 3
- 235000019364 tetracycline Nutrition 0.000 claims description 3
- 150000003522 tetracyclines Chemical class 0.000 claims description 3
- 229940040944 tetracyclines Drugs 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 239000003120 macrolide antibiotic agent Substances 0.000 claims description 2
- 229940041033 macrolides Drugs 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- 150000003952 β-lactams Chemical class 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- 238000007670 refining Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 229940124530 sulfonamide Drugs 0.000 claims 1
- 150000003456 sulfonamides Chemical class 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 206010028980 Neoplasm Diseases 0.000 abstract description 2
- 201000011510 cancer Diseases 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 230000036541 health Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003403 water pollutant Substances 0.000 abstract description 2
- 230000009849 deactivation Effects 0.000 abstract 1
- 230000002085 persistent effect Effects 0.000 abstract 1
- 238000004061 bleaching Methods 0.000 description 40
- 230000003115 biocidal effect Effects 0.000 description 30
- 239000011159 matrix material Substances 0.000 description 17
- 238000010521 absorption reaction Methods 0.000 description 15
- 239000003463 adsorbent Substances 0.000 description 12
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 description 11
- 239000003610 charcoal Substances 0.000 description 5
- 230000006837 decompression Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 239000003651 drinking water Substances 0.000 description 3
- 235000020188 drinking water Nutrition 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 231100000086 high toxicity Toxicity 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- QYAPHLRPFNSDNH-MRFRVZCGSA-N (4s,4as,5as,6s,12ar)-7-chloro-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC(Cl)=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O QYAPHLRPFNSDNH-MRFRVZCGSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 239000007952 growth promoter Substances 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- -1 sulfamido Chemical class 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明提出一种用于吸附去除水中抗生素的可再生废白土基活性炭的制备及使用方法，属于水处理技术的应用领域。抗生素是一类广泛存在的水体污染物，不易降解且容易造成持久性的环境污染。进入人体内的抗生素会危害人体健康，甚至引发癌症。本发明采用热解的方法将废白土制备为废白土基活性炭吸附材料，其表面含有大量含氧官能团，能够快速高效地去除水中抗生素，对水体不产生二次污染。同时通过减压过滤或过滤，可以快速进行固液分离。该材料失活后可通过简单方法再生，具有多次应用的潜力。该技术中采用的原材料为废白土，来源广泛、价格低廉且实现了以废治废的目的，再生方法简单，没有化学品的添加，同时不会对环境造成二次污染。The invention provides a preparation and use method of renewable waste clay-based activated carbon for adsorbing and removing antibiotics in water, and belongs to the application field of water treatment technology. Antibiotics are a wide range of water pollutants, which are not easy to degrade and easily cause persistent environmental pollution. Antibiotics that enter the human body can endanger human health and even cause cancer. The invention adopts the method of pyrolysis to prepare waste clay as waste clay-based activated carbon adsorption material, and its surface contains a large number of oxygen-containing functional groups, which can quickly and efficiently remove antibiotics in water without secondary pollution to water. At the same time, solid-liquid separation can be carried out quickly by filtration or filtration under reduced pressure. The material can be regenerated by a simple method after deactivation, and has the potential for multiple applications. The raw material used in this technology is waste clay, which has a wide range of sources and low price, and achieves the purpose of treating waste with waste. The regeneration method is simple, no chemicals are added, and it will not cause secondary pollution to the environment.
Description
Technical field:
The present invention proposes a kind of method of preparation and use of the renewable spent bleaching clay matrix activated carbon of antibiotic in Adsorption water, belongs to
In the application field of water treatment technology.It, can be by simple after the material inactive using the spent bleaching clay matrix activated carbon of this method preparation
Method regeneration, has the potentiality that are applied multiple times, due to itself distinctive physicochemical properties and a large amount of oxygen-containing functional groups
In the presence of antibiotic in water can be effectively removed.
Background technique:
Antibiotic widely appears in a variety of surrounding mediums such as sewage, soil and surface water as a kind of emerging pollutant.It is anti-
Raw element mainly includes quinolones, macrolides, beta-lactam, Tetracyclines and sulfamido.It is preferable antibacterial because having
Or sterilizing function, for a long time, antibiotic is heavily used in human diseases treatment and is fed to as growth promoter dynamic
Object.Although antibiotic medically has important application, antibiotic can not be completely absorbed or be metabolized in vivo, cause
The 50% ~ 90% of its usage amount is expelled directly out in vitro, and its structural property stablize, it is not degradable in the environment and be easy to cause persistently
The environmental pollution of property.The long-term existence of antibiotic not only breaks up environment microecosystem in water body environment, and enters in human body
Antibiotic can be detrimental to health, may seriously cause cancer.Currently, not only Germany and the developed countries such as U.S. water and
Antibiotic residues are detected in soil, while all being deposited in China river water, reservoir water, seawater, underground water or even drinking water
In the different degrees of residual of the antibiotic such as Tetracyclines, sulfamido, quinolones, antibiotic has become China or even global face
One of great environmental problem faced.
Traditional sewage disposal technology such as bioanalysis cannot fundamentally be effectively removed antibiotic contamination in water body.It is high
Grade oxidizing process has the shortcomings that at high cost, to produce high toxicity Metabolic Intermediate.In comparison, absorption method is as a kind of common dirt
Water treatment technology, low cost, process and easy to operate, economical and efficient, while avoiding the risk of high toxicity metabolite generation.
Therefore, absorption is considered as one of most promising and most effective antibiotic minimizing technology in water treatment technology.Therefore, it is necessary to
Finding not only has low cost but also novel absorption material with high performance, and wherein spent bleaching clay is exactly such a selection.
Discarded byproduct-spent bleaching clay derives from the subtractive process of crude edible oil.Due to the residual of organic substance, remove
Additional oil component is the key that spent bleaching clay recycles.Currently, common extracting process is using solvent and supercritical carbon dioxide
Extraction.At present some researches show that, spent bleaching clay is prepared as charcoal adsorbent material by calcining through hydrothermal synthesis method and under aerobic environment,
Water pollutant can be adsorbed.But hydro-thermal method yield is small, and aerobic calcining, which can generate, endangers gas, to environmental effects.It will give up
The carclazyte activated carbon that high temperature pyrolysis generates under anoxic conditions can be the fertile absorber as water process, can be further sharp
With discarded spent bleaching clay resource, while will not be to environmental danger.
What the invention proposed goes the method for preparation and use of the spent bleaching clay matrix activated carbon of antibiotic in water removal, can effectively go
Antibiotic in water removal, and meet the environmental requirement of the treatment of wastes with processes of wastes against one another, the technology has not been reported in water-treatment technology field at present.
Summary of the invention:
The purpose of the present invention is for antibiotic pollutant especially in drinking water in water, provide a kind of performance efficiency and renewable
Adsorbent material.Spent bleaching clay matrix activated carbon has more oxygen-containing functional group and biggish specific surface area, Neng Gouyou due to itself
Antibiotic in effect ground absorption water.
The preparation method according to the present invention for removing the adsorbent material of antibiotic in water removal is: will be given up by the method for pyrolysis
Carclazyte is prepared as active carbon.Spent bleaching clay is constantly dried first, is then pyrolyzed under oxygen-free atmosphere, to be had
There is the material of stronger adsorption capacity.
It is according to the present invention go the application method of the adsorbent material of antibiotic in water removal first is that: it is living using spent bleaching clay base
Antibiotic in property charcoal Adsorption water.It is filtered after the completion of absorption by decompression or separation of solid and liquid is rapidly completed in the method for filtering, made
It obtains and is purified by the water body that antibiotic pollutes.
It is according to the present invention go water removal in antibiotic adsorbent material application method second is that: adsorption activity will be lost
Spent bleaching clay matrix activated carbon make adsorbent reactivation using the method for pyrolysis, i.e., adsorbent material is pyrolyzed under oxygen-free atmosphere,
Obtain regenerated spent bleaching clay matrix activated carbon.
The present invention can be used for removing in the water bodys such as drinking water and underground water by the adsorbent material that the method being pyrolyzed is prepared
The antibiotic pollutant contained.To realize that purpose as described above, the present invention now adopt the following technical solutions.
Spent bleaching clay matrix activated carbon is prepared by following technical solution:
(1) spent bleaching clay is dried to 12~72 h under the conditions of 65~105 DEG C；
(2) by grinding or crushing control partial size less than 5.0 mm；
(3) spent bleaching clay particle is placed in that system is closed or the oxygen-free atmosphere of inert gas shielding (nitrogen or argon gas) and 300~
It is pyrolyzed 0.5~4 h at 1200 DEG C, is taken out when temperature is lower than 100 DEG C, gained is spent bleaching clay matrix activated carbon.
The application method of spent bleaching clay matrix activated carbon removal antibiotic:
Water body to be clean is polluted by antibiotic and adds adsorbent material, and dosage is sufficiently mixed later in 1~25 g/L
It is even, so that its adsorption time is continued 1~24 h, absorption is filtered after completing using decompression or separation of solid and liquid can be realized in filtering；Or
Material is filled with adsorption column, polluted water body is passed through into adsorption column with the flow velocity of 0.5-6 m/h.
Deactivated spent bleaching clay matrix activated carbon passes through the method being pyrolyzed again and regenerates:
(1) spent bleaching clay is dried to 12~72 h under the conditions of 65~105 DEG C；
(2) the spent bleaching clay particle after drying is placed in that system is closed or the oxygen-free atmospheres such as inert gas shielding (nitrogen or argon gas)
It is pyrolyzed 0.5~4 h at 300~1200 DEG C, is taken out when temperature is lower than 100 DEG C, the namely regenerated spent bleaching clay base of gained is living
Property charcoal.
Compared with prior art, the present invention has the advantages that protrude as follows:
(1) raw material of active carbon of the present invention are spent bleaching clay, derive from vegetable oil subtractive process, from a wealth of sources, inexpensive
And be conducive to protect environment, it can achieve the purpose that the treatment of wastes with processes of wastes against one another.
(2) present invention does not have chemicals using the method being pyrolyzed in the absence of oxygen to spent bleaching clay, this method
Addition and secondary pollution are conducive to protect environment.
(3) itself there is a large amount of oxygen-containing function using the spent bleaching clay matrix activated carbon of the method preparation of pyrolysis in the present invention
Group, can effectively remove antibiotic in water, removal rate is up to 90% or more.
Specific embodiment:
It below in conjunction with specific embodiment, elaborates to technical solution of the present invention, it should be understood that these embodiments are only used for
Illustrate the present invention rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to the present invention
The modifications of various equivalent forms each fall in the application range as defined in the appended claims.
Embodiment 1:
The preparation of spent bleaching clay matrix activated carbon: spent bleaching clay is taken out into part and is placed on 105 DEG C of baking ovens 24 h of drying, uses mortar grinder
Spent bleaching clay is to partial size less than 0.150 mm.The spent bleaching clay particle of screening is put in vacuum tube furnace, by nitrogen atmosphere
2 h are pyrolyzed at (150 mL/min) and 700 DEG C.30 DEG C of taking-ups are reduced to temperature, what is obtained at this time is that spent bleaching clay base is living
Property charcoal.
Adsorb (by taking quadracycline as an example) applied to water body containing antibiotic: preparing 500 mL concentration is 0.1 mmol/L's
Quadracycline solution, is placed in conical flask.It weighs above-mentioned 1 g of adsorbent material to be invested in conical flask, uses magnetic agitation
Device, which is stirred continuously, is uniformly mixed it, and controlled at 25 DEG C.The mixing and absorption time is 2 h, and decompression is utilized after absorption
Suction filtration is separated by solid-liquid separation, and quadracycline concentration in solution, quadracycline removal rate are 90% after measurement absorption.
Embodiment 2:
The preparation of spent bleaching clay matrix activated carbon: spent bleaching clay is taken out into part and is placed on 105 DEG C of baking ovens 24 h of drying, uses mortar grinder
Spent bleaching clay is to partial size less than 0.150 mm.The spent bleaching clay particle of screening is put in vacuum tube furnace, by nitrogen atmosphere
2 h are pyrolyzed at (200 mL/min) and 800 DEG C.30 DEG C of taking-ups are reduced to temperature, what is obtained at this time is that spent bleaching clay base is living
Property charcoal.
Adsorb (by taking aureomycin hydrochloride as an example) applied to water body containing antibiotic: preparing 500 mL concentration is 0.1 mmol/L's
Quadracycline solution, is placed in conical flask.It weighs above-mentioned 2 g of adsorbent material to be invested in conical flask, uses magnetic agitation
Device, which is stirred continuously, is uniformly mixed it, and controlled at 25 DEG C.The mixing and absorption time is 2 h, and decompression is utilized after absorption
Suction filtration is separated by solid-liquid separation, and quadracycline concentration in solution, quadracycline removal rate are 93% after measurement absorption.
Embodiment 3:
The regeneration of spent bleaching clay matrix activated carbon: the spent bleaching clay matrix activated carbon for losing adsorption activity is taken out into part and is placed on 105 DEG C of bakings
Case dries 24 h.The spent bleaching clay particle of drying is put in vacuum tube furnace, by argon atmosphere (200 mL/min) and 700
2 h are pyrolyzed at DEG C.30 DEG C of taking-ups are reduced to temperature, the namely regenerated spent bleaching clay matrix activated carbon obtained at this time.
Adsorb (by taking quadracycline as an example) applied to water body containing antibiotic: preparing 500 mL concentration is 0.1 mmol/L's
Quadracycline solution, is placed in conical flask.It weighs above-mentioned 1 g of adsorbent material to be invested in conical flask, uses magnetic agitation
Device, which is stirred continuously, is uniformly mixed it, and controlled at 25 DEG C.The mixing and absorption time is 6 h, and decompression is utilized after absorption
Suction filtration is separated by solid-liquid separation, and quadracycline concentration in solution, quadracycline removal rate are 85% after measurement absorption.
Claims (7)
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910143238.2A CN109759016A (en) | 2019-02-26 | 2019-02-26 | Preparation and use method of renewable waste clay-based activated carbon for adsorption and removal of antibiotics in water |
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Cited By (3)
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|---|---|---|---|---|
| CN110368917A (en) * | 2019-07-16 | 2019-10-25 | 常州大学 | A kind of method and its application preparing efficient absorption material with paraffin oil decolorization roach |
| CN111001389A (en) * | 2020-01-06 | 2020-04-14 | 河南工业大学 | Preparation and use methods of renewable nano zero-valent iron-loaded waste clay-based activated carbon for removing heavy metals in water |
| CN111013541A (en) * | 2020-01-06 | 2020-04-17 | 河南工业大学 | Preparation and use method of modified waste argil charcoal for removing endocrine disruptors and antibiotics in water |
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| US5256613A (en) * | 1991-08-28 | 1993-10-26 | N.V. Vandemoortele International | Process for regenerating spent bleaching earth |
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| CN109174201A (en) * | 2018-10-12 | 2019-01-11 | 天津大学前沿技术研究院有限公司 | A kind of preparation method of the three-dimensional netted type adsorption catalyst based on spent bleaching clay |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368917A (en) * | 2019-07-16 | 2019-10-25 | 常州大学 | A kind of method and its application preparing efficient absorption material with paraffin oil decolorization roach |
| CN110368917B (en) * | 2019-07-16 | 2022-04-26 | 常州大学 | A method for preparing high-efficiency adsorption material from paraffin oil decolorized waste soil and its application |
| CN111001389A (en) * | 2020-01-06 | 2020-04-14 | 河南工业大学 | Preparation and use methods of renewable nano zero-valent iron-loaded waste clay-based activated carbon for removing heavy metals in water |
| CN111013541A (en) * | 2020-01-06 | 2020-04-17 | 河南工业大学 | Preparation and use method of modified waste argil charcoal for removing endocrine disruptors and antibiotics in water |
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