CN109692665B - A kind of preparation method of N doping porous charcoal removal antibiotic adsorbent - Google Patents
A kind of preparation method of N doping porous charcoal removal antibiotic adsorbent Download PDFInfo
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- CN109692665B CN109692665B CN201910093731.8A CN201910093731A CN109692665B CN 109692665 B CN109692665 B CN 109692665B CN 201910093731 A CN201910093731 A CN 201910093731A CN 109692665 B CN109692665 B CN 109692665B
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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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- 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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
A kind of preparation method of N doping porous charcoal removal antibiotic adsorbent of disclosure of the invention with urea, aminotriacetic acid sodium and hydroxypropyl methyl cellulose etc. for raw material obtains a kind of N doping porous carbon material using high temperature solid state reaction.Step are as follows: a) urea, aminotriacetic acid sodium and hydroxypropyl methyl cellulose are separately dried processing, and are ground into fine particle；B) urea, aminotriacetic acid sodium and hydroxypropyl methyl cellulose are sufficiently mixed rear high temperature solid-state polymerization reaction.N doping porous charcoal made from this method has biggish specific surface area and higher hydrophily, and the adsorption treatment effect to antibiotic in water can be enhanced, to enable the material to be effectively applied to antibiotic waste water processing.
Description
Technical field
The present invention relates to a kind of preparation methods of N doping porous charcoal removal antibiotic adsorbent, and the material of acquisition can be real
Now antibiotic in water is effectively removed, belongs to environmental treatment technical field.
Background technique
Antibiotic is that the movable microbial secondary metabolism of certain biological lifes can selectively be inhibited to produce at low concentrations
Object and its molecular design or fully synthetic derivative.Antibiotic has inhibition or killing effect to pathogenic microorganism, is prevention and treatment
The important drugs of infectious diseases.Antibiotics exists and has had for a long time, and antibiotics is widely used in people
And new analytical technology is constantly studied, until mid-term the 1990s, a large amount of presence of the antibiotic in ecological environment are just opened
Begin to become focus concerned by people.A large amount of antibiotic that the mankind discharge into environment can give the various biozones of ocean and land
It is next potentially hazardous, because even the antibiotic of low concentration also will affect the quantity of bacterium.According to incompletely statistics, China is annual
210,000 tons of antibiotic feedstock capacity superelevation, wherein there is 9.7 ten thousand tons (account for gross annual output amount 46.1%) for animal husbandry.This
Outside, using being listed in preceding 15 drugs with sales volume, to have 10 kinds be antimicrobial DP finish, the use of hospital antibiotic at present in China
Rate is in 67%-82%.However, during treating the mankind and livestock and poultry and promoting growth of animals or poultry, 85% or more antibiotic
Be excreted in the form of raw medicine or metabolite, eventually enter into ecological environment, there is an urgent need to develop antibiotic efficiently it is low at
Present treatment technology.The traditional active sludge organism facture of removal antibiotic method, chloridising, advanced oxidation processes, electrochemistry
Facture, membrane separation process and absorption method.It is absorption method technology maturation, low in cost, easy to operate compared to other technologies, therefore inhale
Attached method is in the technology for being widely used and efficiently being gone as one kind antibiotic in water removal at present.
Active carbon is a kind of cheap mass producible adsorbent material, is often used to the various organic pollutants of adsorption treatment,
But it is higher to the removal efficiency of hydrophobic contaminant since active carbon is typically all hydrophobic base, and most antibiotics are all
It is to have hydrophily, is unfavorable for the absorption of active carbon, therefore, preparation hydrophilic active carbon can effectively improve the suction to antibiotic
It is attached.The present invention is namely based on above-mentioned consideration, prepares a kind of hydrophily N doping porous charcoal, realize to tetracycline, A Mosilin,
The efficient removal of the Multiple Classes of Antibiotics such as sulfanilamide (SN).
Summary of the invention
The present invention provides a kind of preparation methods of N doping porous charcoal removal antibiotic adsorbent, with urea, amino three
Sodium acetate and hydroxypropyl methyl cellulose are raw material, obtain a kind of N doping porous carbon material using high temperature solid state reaction.The material
Material has biggish specific surface area and higher hydrophily, can effectively enhance the adsorption treatment effect to antibiotic in water, from
And it enables the material to be effectively applied to antibiotic waste water processing.
The synthesis process of material the following steps are included:
(1) a certain amount of urea is placed in baking oven drying under certain temperature and is ground into fine particle after a certain period of time；
(2) by a certain amount of aminotriacetic acid sodium be placed in baking oven under certain temperature it is dry be ground into after a certain period of time it is tiny
Particle；
(3) a certain amount of hydroxypropyl methyl cellulose drying under certain temperature is placed in baking oven to be ground into after a certain period of time
Fine particle；
(4) urea, aminotriacetic acid sodium and the hydroxypropyl methyl cellulose after drying and grinding are mixed in a certain ratio simultaneously
Grinding is uniformly, rear to place in high temperature furnace, with nitrogen as protection gas pyroreaction.Be cooled to room temperature after the reaction was completed, spend from
Sub- water washing, drying obtain N doping porous charcoal.
The drying temperature of urea in an oven is 60~80oC in step (1), the time 3~4 hours, is ground into little particle grain
Diameter is 0.1~0.2mm；
The drying temperature of aminotriacetic acid sodium in an oven is 60~80oC in step (2), the time 3~4 hours, is ground into
Little particle partial size is 0.1~0.2mm；
The drying temperature of hydroxypropyl methyl cellulose in an oven is 60~80oC in step (3), the time 3~4 hours, is ground
Wearing into little particle partial size is 0.1~0.2mm；
Urea, aminotriacetic acid sodium and hydroxypropyl methyl cellulose are 2:0.5~1:1~2 according to mass ratio in step (4)
Ratio mixed；
After urea, aminotriacetic acid sodium are mixed with hydroxypropyl methyl cellulose in step (4), high-temperature reaction process is as follows:
Room temperature to heating rate between 80oC keeps 5oC/min, and 80oC constant temperature keeps 50min；Heating rate keeps 5oC/ between 80~200oC
Min keeps 1-2h in 200oC；Heating rate keeps 10oC/min between 200~600oC, cold after keeping 3~6h at 600oC
But to room temperature.
Since the material has biggish specific surface area and higher hydrophily, to tetracycline, A Mosilin, sulfanilamide (SN) in water
Equal antibiotic have very strong adsorptivity, to enable the material to be effectively applied to antibiotic treatment in water.
Specific embodiment
Following embodiments are further explanations for the content of present invention using as the explaination to the technology of the present invention content, but
Substantive content of the invention is not limited in described in following embodiments, those of ordinary skill in the art can with and should know any
Simple change or replacement based on true spirit should belong to protection scope of the presently claimed invention.
Embodiment 1
Step 1: first 10g urea, 5g aminotriacetic acid sodium being put into 80oC in baking oven with 10 hydroxypropyl methyl celluloses and done
Dry processing 3h is ground to 0.1-0.2mm particle after dry respectively, then is sufficiently mixed uniformly, is added in the crucible of 50mL.
Step 2: the crucible reaction device for filling mixed reactant being put into heat temperature raising in muffle furnace, room temperature rises between 80oC
Warm rate keeps 5oC/min, and 80oC constant temperature keeps 50min；Heating rate keeps 5oC/min between 80~200oC, protects in 200oC
Hold 1h；Heating rate keeps 10oC/min between 200~600oC, after keeping 4h at 600oC, is cooled to room temperature, deionization washing
Drying is washed, N doping porous carbon material is obtained.
N doping porous charcoal obtained by this example is applied to the absorption of antibiotic in water: weighing the nitrogen for implementing to prepare in 1 and mixes
It each three parts, every part of 0.5g of miscellaneous porous charcoal, is separately added into three water samples containing antibiotic such as tetracycline, A Mosilin, sulfanilamide (SN),
Volume of water sample is 1L, and concentration is 10mg/L, stirs two hours at room temperature, makes its adsorption saturation, be then separated by filtration to obtain
The water of purification, tetracycline, A Mosilin, sulfanilamide (SN) concentration are respectively in each water sample after being filtered by high performance liquid chromatography detection
0.04,0.2 and 0.1mg/L.
Embodiment 3
Step 1: 10g urea, 5g aminotriacetic acid sodium and 5g hydroxypropyl methyl cellulose being first put into 60oC in baking oven and done
Dry processing 3h is ground to 0.1-0.2mm particle after dry respectively, then is sufficiently mixed uniformly, is added in the crucible of 50mL.
Step 2: the crucible reaction device for filling mixed reactant being put into heat temperature raising in muffle furnace, room temperature rises between 80oC
Warm rate keeps 5oC/min, and 80oC constant temperature keeps 50min；Heating rate keeps 5oC/min between 80~200oC, protects in 200oC
Hold 2h；Heating rate keeps 10oC/min between 200~600oC, after keeping 5h at 600oC, is cooled to room temperature, deionization washing
Drying is washed, N doping porous carbon material is obtained.
N doping porous charcoal obtained by this example is applied to the absorption of antibiotic in water: weighing the nitrogen for implementing to prepare in 2 and mixes
It each three parts, every part of 0.5g of miscellaneous porous charcoal, is separately added into three water samples containing antibiotic such as tetracycline, A Mosilin, sulfanilamide (SN),
Volume of water sample is 1L, and concentration is 10mg/L, stirs two hours at room temperature, makes its adsorption saturation, be then separated by filtration to obtain
The water of purification, tetracycline, A Mosilin, sulfanilamide (SN) concentration are respectively in each water sample after being filtered by high performance liquid chromatography detection
0.02,0.05 and 0.1mg/L.
Embodiment 3
Step 1: 10g urea, 3g aminotriacetic acid sodium and 8g hydroxypropyl methyl cellulose being first put into 60oC in baking oven and done
Dry processing 4h is ground to 0.1-0.2mm particle after dry respectively, then is sufficiently mixed uniformly, is added in the crucible of 50mL.
Step 2: the crucible reaction device for filling mixed reactant being put into heat temperature raising in muffle furnace, room temperature rises between 80oC
Warm rate keeps 5oC/min, and 80oC constant temperature keeps 50min；Heating rate keeps 5oC/min between 80~200oC, protects in 200oC
Hold 1.5h；Heating rate keeps 10oC/min between 200~600oC, after keeping 6h at 600oC, is cooled to room temperature, deionized water
Drying is washed, N doping porous carbon material is obtained.
N doping porous charcoal obtained by this example is applied to the absorption of antibiotic in water: weighing the nitrogen for implementing to prepare in 3 and mixes
It each three parts, every part of 0.5g of miscellaneous porous charcoal, is separately added into three water samples containing antibiotic such as tetracycline, A Mosilin, sulfanilamide (SN),
Volume of water sample is 1L, and concentration is 10mg/L, stirs two hours at room temperature, makes its adsorption saturation, be then separated by filtration to obtain
The water of purification, tetracycline, A Mosilin, sulfanilamide (SN) concentration are respectively in each water sample after being filtered by high performance liquid chromatography detection
0.06,0.1 and 0.08mg/L.
Embodiment 4
Step 1: 10g urea, 3.5g aminotriacetic acid sodium and 6g hydroxypropyl methyl cellulose being first put into 60oC in baking oven
It is dried 4h, is ground to 0.1-0.2mm particle respectively after dry, then is sufficiently mixed uniformly, is added in the crucible of 50mL.
Step 2: the crucible reaction device for filling mixed reactant being put into heat temperature raising in muffle furnace, room temperature rises between 80oC
Warm rate keeps 5oC/min, and 80oC constant temperature keeps 50min；Heating rate keeps 5oC/min between 80~200oC, protects in 200oC
Hold 2h；Heating rate keeps 10oC/min between 200~600oC, after keeping 5h at 600oC, is cooled to room temperature, deionization washing
Drying is washed, N doping porous carbon material is obtained.
N doping porous charcoal obtained by this example is applied to the absorption of antibiotic in water: weighing the nitrogen for implementing to prepare in 3 and mixes
It each three parts, every part of 0.5g of miscellaneous porous charcoal, is separately added into three water samples containing antibiotic such as tetracycline, A Mosilin, sulfanilamide (SN),
Volume of water sample is 1L, and concentration is 10mg/L, stirs two hours at room temperature, makes its adsorption saturation, be then separated by filtration to obtain
The water of purification, tetracycline, A Mosilin, sulfanilamide (SN) concentration are respectively in each water sample after being filtered by high performance liquid chromatography detection
0.01,0.09 and 0.06mg/L.
Embodiment 5
Step 1: 10g urea, 4.5g aminotriacetic acid sodium and 5g hydroxypropyl methyl cellulose being first put into 60oC in baking oven
It is dried 4h, is ground to 0.1-0.2mm particle respectively after dry, then is sufficiently mixed uniformly, is added in the crucible of 50mL.
Step 2: the crucible reaction device for filling mixed reactant being put into heat temperature raising in muffle furnace, room temperature rises between 80oC
Warm rate keeps 5oC/min, and 80oC constant temperature keeps 50min；Heating rate keeps 5oC/min between 80~200oC, protects in 200oC
Hold 2h；Heating rate keeps 10oC/min between 200~600oC, after keeping 5h at 600oC, is cooled to room temperature, deionization washing
Drying is washed, N doping porous carbon material is obtained.
N doping porous charcoal obtained by this example is applied to the absorption of antibiotic in water: weighing the nitrogen for implementing to prepare in 3 and mixes
It each three parts, every part of 0.5g of miscellaneous porous charcoal, is separately added into three water samples containing antibiotic such as tetracycline, A Mosilin, sulfanilamide (SN),
Volume of water sample is 1L, and concentration is 10mg/L, stirs two hours at room temperature, makes its adsorption saturation, be then separated by filtration to obtain
The water of purification, tetracycline, A Mosilin, sulfanilamide (SN) concentration are respectively in each water sample after being filtered by high performance liquid chromatography detection
0.02,0.05 and 0.03mg/L.
Claims (6)
1. a kind of preparation method of N doping porous charcoal removal antibiotic adsorbent, comprising the following steps:
(1) a certain amount of urea is placed in baking oven drying under certain temperature and is ground into fine particle after a certain period of time；
(2) a certain amount of aminotriacetic acid sodium is placed in baking oven drying under certain temperature and is ground into tiny after a certain period of time
Grain；
(3) by a certain amount of hydroxypropyl methyl cellulose be placed in baking oven under certain temperature it is dry be ground into after a certain period of time it is tiny
Particle；
(4) urea, aminotriacetic acid sodium and the hydroxypropyl methyl cellulose after drying and grinding are mixed in a certain ratio and are ground again
Uniformly, it places in high temperature furnace afterwards, with nitrogen as protection gas pyroreaction；
It is cooled to room temperature after the reaction was completed, is washed with deionized, dries, obtain N doping porous charcoal.
2. a kind of preparation method of N doping porous charcoal removal antibiotic adsorbent as described in claim 1, which is characterized in that step
Suddenly in (1) drying temperature of urea in an oven be 60~80oC, the time 3~4 hours, be ground into little particle partial size be 0.1~
0.2mm。
3. a kind of preparation method of N doping porous charcoal removal antibiotic adsorbent as described in claim 1, which is characterized in that step
Suddenly the drying temperature of aminotriacetic acid sodium in an oven is 60~80oC in (2), the time 3~4 hours, is ground into little particle partial size
For 0.1~0.2mm.
4. a kind of preparation method of N doping porous charcoal removal antibiotic adsorbent as described in claim 1, which is characterized in that step
Suddenly the drying temperature of hydroxypropyl methyl cellulose in an oven is 60~80oC in (3), the time 3~4 hours, is ground into little particle
Partial size is 0.1~0.2mm.
5. a kind of preparation method of N doping porous charcoal removal antibiotic adsorbent as described in claim 1, which is characterized in that step
Suddenly urea, aminotriacetic acid sodium and hydroxypropyl methyl cellulose are carried out according to the ratio that mass ratio is 2:0.5~1:1~2 in (4)
Mixing.
6. a kind of preparation method of N doping porous charcoal removal antibiotic adsorbent as described in claim 1, which is characterized in that step
Suddenly after urea, aminotriacetic acid sodium are mixed with hydroxypropyl methyl cellulose in (4), high-temperature reaction process is as follows: room temperature to 80oC
Between heating rate keep 5oC/min, 80oC constant temperature keep 50min；Heating rate keeps 5oC/min between 80~200oC, in 200o
C keeps 1-2h；Heating rate keeps 10oC/min between 200~600oC, after keeping 3~6h at 600oC, is cooled to room temperature.
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| CN111592089B (en) * | 2020-05-25 | 2022-04-26 | 同济大学 | Method for removing medicine in urine by activating peroxyacetic acid with human excrement biochar |
| CN111744459A (en) * | 2020-07-22 | 2020-10-09 | 安徽农业大学 | Preparation method of rice straw modified biochar for removing tetracycline in water body |
| CN112619593B (en) * | 2020-12-16 | 2022-08-02 | 吉林建筑大学 | Adsorption material for sulfonamide antibiotics in sewage and preparation method thereof |
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