CN109437362A - A method of Enrofloxacin is adsorbed using montmorillonite adsorbent - Google Patents
A method of Enrofloxacin is adsorbed using montmorillonite adsorbent Download PDFInfo
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- CN109437362A CN109437362A CN201811530300.5A CN201811530300A CN109437362A CN 109437362 A CN109437362 A CN 109437362A CN 201811530300 A CN201811530300 A CN 201811530300A CN 109437362 A CN109437362 A CN 109437362A
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
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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
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/36—Organic compounds containing halogen
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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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- Hydrology & Water Resources (AREA)
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Silicates, Zeolites, And Molecular Sieves (AREA)
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Abstract
The present invention discloses one kind using montmorillonite as adsorbent, montmorillonite is characterized using X-ray diffraction (XRD), Fourier infrared spectrum (FTIR), scanning electron microscope (SEM) and specific surface area analysis instrument, montmorillonite is studied to the absorption property and influence factor of Enrofloxacin in water simultaneously, the development and application that analysis isothermal adsorption and dynamic process are montmorillonite in antibiotic treatment provide reference.
Description
Technical field
The invention belongs to heavy-metal contaminated soil Treatment process fields more particularly to a kind of utilization montmorillonite adsorbent to adsorb
The method of Enrofloxacin.
Background technique
Since antibiotic is widely used, the residual of Multiple Classes of Antibiotics has been had found in more and more natural environments, is resisted
Raw element is a kind of chemical substance of biological function that other species can be influenced with humble concentration.Although its discovery with answer
With, great role has been played in terms of human health and the animals and plants prevention and control of plant diseases, pest control, it is still, dirty as antibiotic largely uses
Dye problem is increasing therewith.Enrofloxacin (enrofloxacin) is the fluoroquinolones of first animal specific,
It is succeeded in developing and is come into operation by German Bayer AG within 1987, be mainly used for treating fowl bacterial disease and mycoplasma sense
Dye, is the most commonly used veterinary drug in China.In order to guarantee the health of livestock and poultry, Enrofloxacin is often added in feed.Studies have shown that
It after livestock and poultry intake, can not only be remained in animal products, and ecological environment can be entered with excrement, urine, pollute ambient soil,
Surface water, moreover it is possible to be had an impact by normal activities of the food chain to animals and plants and microorganism, finally influence the mankind certainly
The health of body.
Montmorillonite (montmorillonite, MMT) is by pressing from both sides one layer of aluminium (magnesium) oxygen octahedral among two layers of tetrahedral si-o film
2: the 1 type layered silicate clay mineral that body is constituted, the cation of synusia can occur isomorphous replacement effect, crystal layer unit caused to produce
Raw permanent negative electrical charge makes smectite structure layer have the oxygen or hydroxyl not shared between permanent negative electrical charge smectite structure elementary layer
Base, thus binding force between layers is weaker, hydrone or other exchangeable cations can enter interlayer, and play connection
Effect.The interlamination region constituted between smectite structure elementary layer has huge internal surface area, and there is Inter layer exchange, interlayer to inhale
Characteristics, these characteristics such as attached, interlayer is catalyzed, interlayer polymerize, interlayer is pillared have established montmorillonite in environmental contaminants adsorption treatment
Etc. application foundation.But current montmorillonite to such as absorption property of the antibiotic of Enrofloxacin class and its mechanism of action still
It is not clear.
Summary of the invention
In view of the above-mentioned problems, the present invention provides a kind of method using montmorillonite adsorbent absorption Enrofloxacin, it is de- to cover
Stone is adsorbent, is integrated using X-ray diffraction (XRD), Fourier infrared spectrum (FTIR), scanning electron microscope (SEM) and specific surface
Analyzer characterizes montmorillonite, while studying montmorillonite to the absorption property and influence factor of Enrofloxacin in water, analysis etc.
The development and application that temperature absorption and dynamic process are montmorillonite in antibiotic treatment provide reference.
In order to achieve the above objectives, the specific technical proposal of the invention is: a kind of adsorb En Nuosha using montmorillonite adsorbent
The method of star, comprising the following steps:
(1) Enrofloxacin standard solution is prepared: weighing Enrofloxacin 0.200g into beaker, HCl is added to dissolving, shifts
Into 1000 mL brown volumetric flasks, with deionized water constant volume, Enrofloxacin concentration of standard solution is 200mg/L；
(2) montmorillonite physicochemical property characterizes: specific surface area is measured with BET method by specific surface area measuring instrument；Charcoal
Surface topography and structure of functional groups pass through scanning electron microscope；X-ray diffractometer and Fourier Transform Infrared Spectrometer (Nicolet
380) it is analyzed；
(3) adsorption experiment:
A, influence of the pH to montmorillonite absorption Enrofloxacin:
Dilute Enrofloxacin stock solution to 50mgL-1, using HCl or NaOH adjust pH be respectively 2.0,4.0,6.0,
8.0,10.0, it weighs 0.05g montmorillonite and is placed in 100mL conical flask, and be separately added into the Enrofloxacin that 50mL regulates pH value
Solution shakes up, and is put into shaking table, shakes under 25 DEG C, 150rmin-1 and filters afterwards for 24 hours, and Enrofloxacin is dense in measurement filtrate
Degree, and montmorillonite is calculated to the removal rate of Enrofloxacin, determine optimum pH；
B, influence of the reaction time to montmorillonite absorption Enrofloxacin:
Enrofloxacin stock solution is diluted to 50mgL-1, is adjusted to optimum pH, is weighed 0.05g montmorillonite and be placed in 100mL
In conical flask, and it is separately added into the Enrofloxacin solution that 50mL regulates pH value, shakes up, be put into shaking table, at 25 DEG C, 150r
Different time is vibrated under min-1 respectively: 10min, 30min, 1h, 3h, 5h, 9h, 12h, being filtered afterwards for 24 hours, grace promise in filtrate is measured
The concentration of Sha Xing, and calculate montmorillonite to the removal rate of Enrofloxacin；
C, influence of the influence of initial concentration solution to montmorillonite absorption Enrofloxacin:
Enrofloxacin stock solution is diluted to 5,10,25,50,100,150,200mgL-1, is adjusted to optimum pH, is weighed
0.05 g montmorillonite is placed in 100mL conical flask, and is separately added into the Enrofloxacin solution of 50mL various concentration, is shaken up, is put into
Shaking table is vibrated under 25 DEG C, 150rmin-1 and is filtered afterwards for 24 hours, measures the concentration of Enrofloxacin in filtrate, and calculates get Meng Tuo
Removal rate of the stone to Enrofloxacin；
D, Enrofloxacin analysis method:
Enrofloxacin concentration is measured at wavelength 271nm using UV visible spectroscopy, and calculates adsorbance and removal rate,
Calculation method is as follows:
In formula: qe is adsorbance (mgg-1)；C0 is the mass concentration (mgL-1) of solution before adsorbing；Ce is after adsorbing
The mass concentration (mgL-1) of solution；V is Enrofloxacin liquor capacity (mL)；M is montmorillonite quality (mg)；U is removal rate
(%).
Compared with prior art, the present invention has the advantage that utilizing X-ray diffraction using montmorillonite as adsorbent
(XRD), Fourier infrared spectrum (FTIR), scanning electron microscope (SEM) and specific surface area analysis instrument characterize montmorillonite, simultaneously
Montmorillonite is studied to the absorption property and influence factor of Enrofloxacin in water, analyzes isothermal adsorption and dynamic process, it is de- to cover
Development and application of the stone in antibiotic treatment provide reference.
Detailed description of the invention
Fig. 1 a and Fig. 1 b are X-ray diffraction (XRD) spectrogram and infrared spectrum (FT-IR) of montmorillonite；
Fig. 2 a and Fig. 2 b are the scanning electron micrograph (SEM) of montmorillonite；
The nitrogen adsorption parsing thermoisopleth and pore size distribution curve of Fig. 3 a and Fig. 3 b montmorillonite；
Fig. 4 a, 4b, 4c are the influence of Ph, time, initial concentration to adsorbance respectively；
Fig. 5 a, 5b are adsorption isotherm line model.
Fig. 6 a, 6b and 6c are X-ray diffraction (XRD) spectrogram, the infrared spectrum (FT- of montmorillonite after adsorbing Enrofloxacin
) and scanning electron micrograph (SEM) IR；
Specific embodiment
Example 1: a method of Enrofloxacin is adsorbed using montmorillonite adsorbent, comprising the following steps:
(1) Enrofloxacin standard solution is prepared: weighing Enrofloxacin 0.200g into beaker, HCl is added to dissolving, shifts
Into 1000 mL brown volumetric flasks, with deionized water constant volume, Enrofloxacin concentration of standard solution is 200mg/L；
(2) montmorillonite physicochemical property characterizes: specific surface area is measured with BET method by specific surface area measuring instrument；Charcoal
Surface topography and structure of functional groups pass through scanning electron microscope；X-ray diffractometer and Fourier Transform Infrared Spectrometer (Nicolet
380) it is analyzed；
(3) adsorption experiment:
A, influence of the pH to montmorillonite absorption Enrofloxacin:
Dilute Enrofloxacin stock solution to 50mgL-1, using HCl or NaOH adjust pH be respectively 2.0,4.0,6.0,
8.0,10.0, it weighs 0.05g montmorillonite and is placed in 100mL conical flask, and be separately added into the Enrofloxacin that 50mL regulates pH value
Solution shakes up, and is put into shaking table, shakes under 25 DEG C, 150rmin-1 and filters afterwards for 24 hours, and Enrofloxacin is dense in measurement filtrate
Degree, and montmorillonite is calculated to the removal rate of Enrofloxacin, determine optimum pH；
B, influence of the reaction time to montmorillonite absorption Enrofloxacin:
Enrofloxacin stock solution is diluted to 50mgL-1, is adjusted to optimum pH, is weighed 0.05g montmorillonite and be placed in 100mL
In conical flask, and it is separately added into the Enrofloxacin solution that 50mL regulates pH value, shakes up, be put into shaking table, at 25 DEG C, 150r
Different time is vibrated under min-1 respectively: 10min, 30min, 1h, 3h, 5h, 9h, 12h, being filtered afterwards for 24 hours, grace promise in filtrate is measured
The concentration of Sha Xing, and calculate montmorillonite to the removal rate of Enrofloxacin；
C, influence of the influence of initial concentration solution to montmorillonite absorption Enrofloxacin:
Enrofloxacin stock solution is diluted to 5,10,25,50,100,150,200mgL-1, is adjusted to optimum pH, is weighed
0.05 g montmorillonite is placed in 100mL conical flask, and is separately added into the Enrofloxacin solution of 50mL various concentration, is shaken up, is put into
Shaking table is vibrated under 25 DEG C, 150rmin-1 and is filtered afterwards for 24 hours, measures the concentration of Enrofloxacin in filtrate, and calculates get Meng Tuo
Removal rate of the stone to Enrofloxacin；
(4) Enrofloxacin analysis method:
Enrofloxacin concentration is measured at wavelength 271nm using UV visible spectroscopy, and calculates adsorbance and removal rate,
Calculation method is as follows:
(2)
In formula: qe is adsorbance (mgg-1)；C0 is the mass concentration (mgL-1) of solution before adsorbing；Ce is after adsorbing
The mass concentration (mgL-1) of solution；V is Enrofloxacin liquor capacity (mL)；M is montmorillonite quality (mg)；U is removal rate
(%).
The operation that average value is carried out using Excel 2013, using 7.0 software of Adobe Photoshop to SEM image
Processing is mapped using 8.1 software of Origin.
(5) data are analyzed
Using Langmuir model and Freundlich models fitting charcoal to lead-copper-zinc adsorption isotherm,
Shown in the equation at constant temperature of Langmuir model such as formula (3), (4), the equation at constant temperature of Freundlich model such as formula (5), (6) institute
Show,
Being converted into linear equation is
Being converted into linear equation is
In formula, qeFor equilibrium adsorption capacity (mg/g)；CeFor balance solution concentration (mg/L)；qmaxFor maximal absorptive capacity (mg/
g)；KL、KF, n be absorption constant.Wherein, Langmuir model is to indicate to adsorb monolayer on homogeneous surfaces and not have each other
There is interaction；And Freundlich model is empirical equation, commonly used in describing the chemisorption on Heterogeneous surface.
Using mathematical model (pseudo-first-order kinetics equation and pseudo-second order kinetic equation) come the dynamics of simulation test,
Shown in expression formula such as formula (7) and (8).
In formula, qeAnd qtRespectively adsorption equilibrium and the adsorbance (mg/g) when t；k1Indicate pseudo-first-order adsorbing filament technique
(min-1)；k2Indicate quasi- secondary absorption rate constant (g/mgmin).Table 1 is different dynamic model fitting parameter.
1 different dynamic model fitting parameter of table
The present invention is used for the absorption of antibiotic Enrofloxacin using montmorillonite as adsorbent, inquires into its absorption to Enrofloxacin
Effect, to provide scientific basis to repair the pollution of water body antibiotic using montmorillonite.Wherein Fig. 1 a-XRD, Fig. 1 b-FT-IR are real
Testing result verification test raw materials is montmorillonite.It can be seen that montmorillonite particle is larger from Fig. 2 a, rough surface is gathered into
Agglomerate or titbit shape aggregate, the thicker pattern that random fluctuation is presented of sheet body.Photo is further amplified to show, montmorillonite surface
In layer structure, irregular flaky crystal, sheet accumulation, and loosely organized, lamella curling.Fig. 3 a and Fig. 3 b BET result table
Bright, montmorillonite has big specific surface area (18.56m2/ g), it is more advantageous to absorption.Then montmorillonite is had studied to Enrofloxacin
Absorption property.The study found that montmorillonite is to Enrofloxacin removal rate as the increase of pH is first dropped in the range of pH2-10
It is increased after low.PH6 is optimum pH.Montmorillonite meets pseudo-second order kinetic equation to Enrofloxacin adsorption dynamics adsorption kinetics, related
Coefficients R2> 0.999 illustrates that the rate of adsorption is mainly determined by chemisorption.Montmorillonite XRD, FT-IR after adsorbing Enrofloxacin
It is proved with sem analysis, it is (Fig. 6) carried out by way of interlayer that montmorillonite, which adsorbs Enrofloxacin,.In addition, montmorillonite is to grace promise
Sha Xing absorption meets Langmuir adsoption equation, and it is electrical to be higher than reported adsorbent by maximal absorptive capacity 115.74mg/g
Stone, mud granule etc. (it is as shown in the table).Therefore montmorillonite is a kind of adsorbent of efficiently removal water body antibiotic Enrofloxacin.
Claims (1)
1. a kind of method using montmorillonite adsorbent absorption Enrofloxacin, which comprises the following steps:
(1) Enrofloxacin standard solution is prepared: weighing Enrofloxacin 0.200g into beaker, HCl is added to dissolving, is transferred to
In 1000mL brown volumetric flask, with deionized water constant volume, Enrofloxacin concentration of standard solution is 200mg/L；
(2) montmorillonite physicochemical property characterizes: specific surface area is measured with BET method by specific surface area measuring instrument；The surface of charcoal
Pattern and structure of functional groups pass through scanning electron microscope；X-ray diffractometer and Fourier Transform Infrared Spectrometer (Nicolet 380) into
Row analysis；
(3) adsorption experiment:
A, influence of the pH to montmorillonite absorption Enrofloxacin:
Dilute Enrofloxacin stock solution to 50mgL-1, using HCl or NaOH adjust pH be respectively 2.0,4.0,6.0,8.0,
10.0, it weighs 0.05g montmorillonite and is placed in 100mL conical flask, and be separately added into the Enrofloxacin solution that 50mL regulates pH value,
It shakes up, is put into shaking table, shake under 25 DEG C, 150rmin-1 and filter afterwards for 24 hours, measure the concentration of Enrofloxacin in filtrate, and count
Calculation obtains montmorillonite to the removal rate of Enrofloxacin, determines optimum pH；
B, influence of the reaction time to montmorillonite absorption Enrofloxacin:
Enrofloxacin stock solution is diluted to 50mgL-1, is adjusted to optimum pH, is weighed 0.05g montmorillonite and be placed in 100mL taper
In bottle, and it is separately added into the Enrofloxacin solution that 50mL regulates pH value, shakes up, be put into shaking table, at 25 DEG C, 150rmin-1
It is lower to vibrate different time respectively: 10min, 30min, 1h, 3h, 5h, 9h, 12h, to filter afterwards for 24 hours, measure Enrofloxacin in filtrate
Concentration, and calculate montmorillonite to the removal rate of Enrofloxacin；
C, influence of the influence of initial concentration solution to montmorillonite absorption Enrofloxacin:
Enrofloxacin stock solution is diluted to 5,10,25,50,100,150,200mgL-1, is adjusted to optimum pH, is weighed
0.05g montmorillonite is placed in 100mL conical flask, and is separately added into the Enrofloxacin solution of 50mL various concentration, is shaken up, is put into and shakes
Bed, vibrates under 25 DEG C, 150rmin-1 and filters afterwards for 24 hours, measures the concentration of Enrofloxacin in filtrate, and calculates to obtain montmorillonite
To the removal rate of Enrofloxacin；
D, Enrofloxacin analysis method:
Enrofloxacin concentration is measured at wavelength 271nm using UV visible spectroscopy, and calculates adsorbance and removal rate, is calculated
Method is as follows:
In formula: qe is adsorbance (mgg-1)；C0 is the mass concentration (mgL-1) of solution before adsorbing；Ce is solution after absorption
Mass concentration (mgL-1)；V is Enrofloxacin liquor capacity (mL)；M is montmorillonite quality (mg)；U is removal rate (%).
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Cited By (3)
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| CN111721737A (en) * | 2020-06-15 | 2020-09-29 | 上海应用技术大学 | Characterization method for researching interaction mechanism of slow-release essence nanoparticles and paper |
| CN113717101A (en) * | 2021-08-30 | 2021-11-30 | 深圳市博林达科技有限公司 | Purification process for enrofloxacin |
| CN113813369A (en) * | 2021-11-09 | 2021-12-21 | 浙江省农业科学院 | EGF/MMT compound for preventing/treating intestinal tract injury of piglets |
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