CN108355616A - A method of removing tetracycline using aluminium based metal organic backbone/graphene oxide composite material - Google Patents
A method of removing tetracycline using aluminium based metal organic backbone/graphene oxide composite material Download PDFInfo
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- CN108355616A CN108355616A CN201810369408.4A CN201810369408A CN108355616A CN 108355616 A CN108355616 A CN 108355616A CN 201810369408 A CN201810369408 A CN 201810369408A CN 108355616 A CN108355616 A CN 108355616A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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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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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
The invention belongs to Environmental Science and Engineering fields, disclose a kind of method removing tetracycline using aluminium based metal organic backbone/graphene oxide composite material.This method evenly spreads to aluminium based metal organic backbone/graphene oxide composite material in the water body containing tetracycline, adjusts pH and is adsorbed for 2~11.The composite material is positively charged, and tetracycline is negatively charged in aqueous solution, and strong electrostatic interaction can be formed between adsorbent and adsorbate；Secondly, the hexagonal carbon atomic plane of graphene oxide densification can generate π π with the phenyl ring on tetracycline and act on, and strengthen absorption；Again, the metal aluminium ion in composite material can form Al N covalent bonds with the nitrogen-atoms on tetracycline, further strengthen the active force between absorption.The synergistic effect of three is so that aluminium based metal organic backbone/graphene oxide composite material prepared by the present invention is known as very strong suction-operated and higher adsorption capacity to Fourth Ring in water.
Description
Technical field
The invention belongs to Environmental Science and Engineering fields, more particularly to a kind of to utilize aluminium based metal organic backbone/oxidation stone
The method of black alkene composite material removal tetracycline.
Background technology
In recent years, with industrialization development, environmental problem becomes increasingly conspicuous, and the abuse of antibiotic becomes global problem.I
State is abuse of antibiotics one of the countries with the most serious ..., and antibiotic detected successively in some trunk rivers, such as the Yellow River, pearl
The water bodys such as river, Chaohu and Jiulongjiang River.Tetracycline (Tetracycline, TC) is a kind of typical antibiotic, extensive
Applied in human medical and animal-breeding, to infection control, improves efficiency of feed utilization and promote growth of animal.However, dynamic
Object cannot carry out tetracycline metabolic degradation, and the tetracycline after use almost be not added with being discharged into environment of change, mainly with system
The mode of medicine industrial wastewater, medical waste water, animal husbandry waste water and agricultural runoff enters environment, and it is rich to carry out biology by food chain
Collection, pollutes.Meanwhile tetracycline is a kind of amphiphatic molecule, containing phenolic hydroxyl group, amino and hydroxyl, easily with cation and polarity
Or charge species interact.Tetracycline and its metabolite presence lasting in water environment, may will produce toxicity
Effect, component environment microorganism is killed in selectivity suppression, while inducing the generation of anti-medicine flora, is caused to ecological environment and human health
Unpredictable harm.Therefore, find it is a kind of efficiently separate removal tetracycline method have a very important significance.
At present both at home and abroad to the minimizing technology of Tetracyclines pollutant, mainly there are biological degradation method and physical chemistry processing
Method.In comparison, absorption method be current application at most, one of most promising methods, it is not only easy to operate, low energy consumption, and
And effectively target contaminant can be gone out under the premise of not generating secondary environmental pollution object.Current main adsorbent can divide
It it is 4 kinds, including organic adsorbent, carbonaceous sorbent, metal oxide sorbents and clay absorbent.Wherein, organic adsorbent
Mainly there are synthetic resin, chitosan etc.；Carbonaceous sorbent includes activated carbon, mesoporous carbon, carbon nanotube, graphene etc.；Metal oxygen
Compound adsorbent is mainly nano material, such as nano-TiO2, nanometer Al2O3, nano-magnetic Fe3O4Deng；Clay absorbent has swelling
Soil, Yi Laishi etc..But these adsorbents are used for the antibiotic in Pharmaceutical Wastewater Treatment, there is respective defect, not such as selectivity
Well, adsorption efficiency is not high, and most of manufacturing costs are higher, technique is more complex.
In terms of tetracycline adsorption, representative research is Rattanachueskul N.
(Rattanachueskul,N.,Saning,A.,Kaowphong,S.,Chumha,N.,&Chuenchom,L.(2017)
.Magnetic carbon composites with a hierarchical structure for adsorption of
tetracycline,prepared from sugarcane bagasse via hydrothermal carbonization
coupled with simple heat treatment process.Bioresource Technology,226,164-
Etc. 172) using magnetic carbon composite tetracycline adsorption, under conditions of initial concentration is 80mg/L, absorption 5h obtains maximum
Adsorption capacity is 28.1mg/g；Liu,Q.(Liu,Q.,Zhong,L.B.,Zhao,Q.B.,Frear,C.,&Zheng,Y.M.
(2015).Synthesis of Fe3O4/polyacrylonitrile composite electrospun nanofiber
mat for effective adsorption of tetracycline.Acs Appl Mater Interfaces,7(27),
14573-14583) etc. prepare electrospinning Fe3O4/ PAN nanofibers are used for Adsorption tetracycline, as initial a concentration of 360mg/L
When, it is 257.1mg/g that absorption 72h, which obtains maximum adsorption capacity,.Therefore, tetracycline molecule can be adsorbed in water again by researching and developing
It is very important with high-adsorption-capacity novel absorption material.
Invention content
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that offer is a kind of to utilize aluminium base
The method of metal organic framework/graphene oxide composite material removal tetracycline.
The purpose of the present invention is realized by following proposal：
A method of tetracycline being removed using aluminium based metal organic backbone/graphene oxide composite material, includes mainly
Following steps：
Aluminium based metal organic backbone/graphene oxide composite material is evenly spread in the water body containing tetracycline, is obtained
Adsorb initial soln；The pH for adjusting absorption initial soln is adsorbed for 2~11, obtains the aqueous solution after adsorption cleaning.
The dosage satisfaction of the aluminium based metal organic backbone/graphene oxide composite material and the water body containing tetracycline makes
A concentration of 0.05~0.5g/L of aluminium based metal organic backbone/graphene oxide composite material in obtained absorption initial soln,
Preferably 0.15~0.25g/L；
The water body containing tetracycline refers to the water body of Fourth Ring cellulose content≤100mg/L；
The absorption refers to that adsorption temp is 10~40 DEG C, adsorption time >=30min.
The pH value is preferably 4~10；
Aluminium based metal organic backbone/the graphene oxide composite material is mainly prepared by following methods：It can
Dissolubility aluminium salt, organic ligand and graphene oxide are dissolved in low boiling point organic solvent, obtain reaction mixture；To reaction mixture
Heating reaction is carried out, is after reaction cooled to room temperature gained reaction solution, is filtered, washed, to be drying to obtain aluminium based metal organic
Skeleton/graphene oxide composite material (MIL-68 (Al)/GO).
The aluminum soluble salt refers to aluminum nitrate or aluminium chloride；
The organic ligand is terephthalic acid (TPA)；
The low boiling point organic solvent is n,N-Dimethylformamide, propyl alcohol, isopropanol, in methanol or ethyl alcohol at least
It is a kind of.
The dosage of the aluminum soluble salt, organic ligand and graphene oxide meet aluminum soluble salt, organic ligand and
The mass ratio of graphene oxide is (1~5)：1：(0.01-0.15)；
A concentration of 0.10~0.25g/mL of aluminum soluble salt in the reaction mixture.
The heating reaction refers to 8~16h of isothermal reaction after being heated to 130~150 DEG C.
The washing refers to being washed with low boiling point organic solvent, and wherein low boiling point organic solvent is N, N- dimethyl
Formamide, propyl alcohol, isopropanol, at least one of methanol or ethyl alcohol；
The drying refers to dry 8~12h under the conditions of 60~120 DEG C.
The present invention mechanism be：
Aluminium based metal organic backbone/graphene oxide composite material prepared by the present invention is positively charged, and tetracycline is water-soluble
It is negatively charged in liquid, therefore, strong electrostatic interaction can be formed between adsorbent and adsorbate；Next, graphene oxide densification
Hexagonal carbon atomic plane can generate π-π with the phenyl ring on tetracycline and act on, and strengthen absorption；Again, the metal in composite material
Aluminium ion can form Al-N covalent bonds with the nitrogen-atoms on tetracycline, further strengthen the active force between absorption.The association of three
It is very strong that same-action so that aluminium based metal organic backbone/graphene oxide composite material prepared by the present invention is known as Fourth Ring in water
Suction-operated and higher adsorption capacity.
The present invention compared with the existing technology, has the following advantages and advantageous effect：
(1) aluminium based metal organic backbone/graphene oxide composite material water stability that the present invention uses is good, specific surface area
It is huge, it is capable of providing enough adsorption sites.
(2) aluminium based metal organic backbone/graphene oxide composite material for using of the present invention in Adsorption water four
There is higher adsorption capacity when ring element.
(3) aluminium based metal organic backbone/graphene oxide composite material that the present invention uses being capable of very fast Adsorption water
In tetracycline molecule.
(4) aluminium based metal organic backbone/graphene oxide composite material preparation process that the present invention uses is simple, at low cost
It is honest and clean.
Description of the drawings
Fig. 1 is the XRD diagram of MIL-68 (Al)/GO materials prepared in embodiment 1；
Fig. 2 is the curve graph of the adsorbance and removal rate under different adsorption times in embodiment 2；
Fig. 3 is the curve graph of the adsorbance under different initial concentrations under different adsorption temps in embodiment 3；
Fig. 4 is the curve graph of the adsorbance in embodiment 4 at various ph values；
Specific implementation mode
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
Embodiment 1：Prepare MIL-68 (Al)/GO materials
3.00g aluminium chloride and 3.00g terephthalic acid (TPA)s are dissolved in 150mL N, in mono- dimethylformamides of N-, being sufficiently stirred makes
It is completely dissolved, and is then slowly added into 0.12g graphene oxide powders, and reaction is uniformly mixed；It is stirred under 130 DEG C of constant temperatures anti-
16 hours are answered, cooled to room temperature.Filtered product first uses N, N- dimethylformamides to rinse 2~3 times, methanol cleaning 2~3
Secondary, the dry activation 12h under 105 DEG C of vacuum conditions, it is MIL-68 (Al)/GO to mark this sample.
Using the sharp shadow X-ray diffractometers of Empyrean of Dutch Panaco company production to prepared by the embodiment of the present invention 1
MIL-68 (Al)/GO materials characterized, wherein operating condition is：Copper target, 40KV, 40mA, 0.02626 degree of step-length, scanning
8.109 seconds/step of speed.The results are shown in Figure 1, it will be seen from figure 1 that MIL-68 (Al)/GO materials prepared in embodiment 1
XRD diffraction maximums and document (Wu S C, Yu L L, Xiao F F, et al.Synthesis of aluminum-based
MOF/graphite oxide composite and enhanced removal of methyl orange[J].Journal
Of Alloys＆Compounds, 2017.) the XRD diffraction maximum goodnesses of fit reported in are high, show MIL-68 (Al)/GO materials
It is successfully prepared.
Using the pore structure for the sample that ASAP2020 specific surface areas and distribution of pores structural test machines prepare embodiment 1
It is tested, design parameter is as shown in table 1.
1 porous material structural parameters of table
From table 1 it follows that the specific surface area 1276.69cm of MIL-68 (Al)/GO materials prepared by embodiment 12/
g；Micropore specific area 298cm2/g；Total pore volume 0.69cm3/g；Micropore volume 0.41cm3/g。
Application Example
After being all made of high performance liquid chromatography (HPLC, Waters 2695, the U.S.) measurement absorption in embodiment 2~4 below
The concentration of solution, test condition are：Mobile phase is acetonitrile/water, and its ratio be 20:80 (V/V), flow velocity 1.0mL/min, test
Temperature is 30 DEG C.Chromatographic column is Sunfire C18 chromatographic columns (250mm × 4.6mm), and detector is PDA detectors, Detection wavelength
For 355nm, sampling volume is 15 μ L.Then adsorbance and removal rate, wherein adsorbance=(initial soln concentration-suction are calculated
The concentration of attached solution) * solution volume/adsorbent quality, removal rate=(solution is dense after initial soln concentration-absorption
Degree)/initial soln concentration * 100%.
Embodiment 2：MIL-68 (Al)/absorption of the GO to tetracycline in water
Take 10 250mL conical flasks, every conical flask that a concentration of 50mg/L tetracyclines aqueous solutions of 100mL are added.Every group of cone
Shape bottle is separately added into MIL-68 (Al)/GO materials prepared in embodiment 1, and the material addition in every conical flask is
20mg.At a temperature of 298K, carry out adsorption experiment under the conditions of 150 revs/min in constant-temperature table, timing sampling measure solution concentration into
Row analysis, the curve graph of adsorbance and removal rate under different adsorption times is as shown in Fig. 2, as can be seen from Figure 2 MIL-68
(Al)/GO is very fast in preceding 90min to the rate of adsorption of tetracycline in water, and can reach adsorption equilibrium in 300min or so,
For the tetracycline that initial concentration is 50mg/L, maximal absorptive capacity can reach 202.65mg/g, and removal rate reaches
81.06%.
Embodiment 3：MIL-68 (Al)/absorption of the GO to tetracycline in water
21 250mL conical flasks are taken, are divided into three groups, every group of tetracycline concentration of aqueous solution gradient is 5,10,15,20,30,
40,60mg/L, volume is 100mL.Every conical flask is separately added into MIL-68 (Al)/GO materials prepared in embodiment 1,
Addition is 20mg.Three groups carry out not in the constant-temperature table at a temperature of 288K, 298K and 308K, under the conditions of 150 revs/min respectively
With the absorption of initial concentration, adsorption time 6h, the adsorbance under different adsorption temps and initial concentration is as shown in figure 3, from Fig. 3
It can be seen that when tetracycline initial concentration is less than 20mg/L, temperature has little effect adsorbance；When tetracycline is initially dense
When degree is more than 20mg/L, influence of the temperature to adsorbance starts to show, and with the raising of temperature, and adsorbance increases.In addition,
MIL-68 (Al)/GO under the conditions of 15,25 and 35 DEG C to water in the equilibrium adsorption capacity of tetracycline be respectively 207.81,212.87
And 219.61mg/g, MIL-68 (Al)/GO are big to the adsorption capacity of tetracycline.
Embodiment 4：MIL-68 (Al)/absorption of the GO to tetracycline in water
It takes 9 250mL conical flasks, every conical flask that a concentration of 50mg/L tetracyclines of 100mL are added, adjusts pH value ladder
Degree is 2.00,3.00,4.00,5.00,6.00,7.00,8.50,10.00,11.00.Every group of conical flask is separately added into embodiment 1
In prepared aluminium based metal organic backbone MIL-68 (Al)/GO materials, every conical flask material addition is 20mg.In 298K
At a temperature of, carry out the absorption of different pH value in the constant-temperature table under the conditions of 150 revs/min, adsorption time 6h, under different pH value
Adsorbance is as shown in Figure 4.Figure 4, it is seen that when pH value is less than 4 or is more than 10, adsorbance is relatively low；When pH value is equal to
When between 4 to 10, adsorbance is larger and keeps balancing, this is because MIL-68 (Al)/GO is unstable under the conditions of strong acid and strong base
Fixed, structure is destroyed and losing absorption property causes.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of method removing tetracycline using aluminium based metal organic backbone/graphene oxide composite material, it is characterised in that
It mainly includes the following steps that：Aluminium based metal organic backbone/graphene oxide composite material is evenly spread into the water containing tetracycline
In body, absorption initial soln is obtained；The pH for adjusting absorption initial soln is adsorbed for 2~11, obtains the water after adsorption cleaning
Solution.
2. according to claim 1 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that the aluminium based metal organic backbone/graphene oxide composite material is prepared by following methods：It will
Aluminum soluble salt, organic ligand and graphene oxide are dissolved in low boiling point organic solvent, obtain reaction mixture；Reaction is mixed
Liquid carries out heating reaction, is after reaction cooled to room temperature gained reaction solution, is filtered, washed, is drying to obtain aluminium based metal and has
Machine skeleton/graphene oxide composite material.
3. according to claim 2 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that：
The aluminum soluble salt refers to aluminum nitrate or aluminium chloride；
The organic ligand is terephthalic acid (TPA)；
The low boiling point organic solvent is n,N-Dimethylformamide, propyl alcohol, isopropanol, at least one in methanol or ethyl alcohol
Kind.
4. according to claim 2 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that：
The dosage of the aluminum soluble salt, organic ligand and graphene oxide meets aluminum soluble salt, organic ligand and oxidation
The mass ratio of graphene is (1~5)：1：(0.01-0.15)；A concentration of the 0.10 of aluminum soluble salt in the reaction mixture
~0.25g/mL.
5. according to claim 2 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that：
The heating reaction refers to 8~16h of isothermal reaction after being heated to 130~150 DEG C.
6. according to claim 2 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that：
The washing refers to being washed with low boiling point organic solvent, and wherein low boiling point organic solvent is N, N- dimethyl formyls
Amine, propyl alcohol, isopropanol, at least one of methanol or ethyl alcohol；
The drying refers to dry 8~12h under the conditions of 60~120 DEG C.
7. according to claim 1 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that：
The dosage satisfaction of the aluminium based metal organic backbone/graphene oxide composite material and the water body containing tetracycline makes to obtain
Absorption initial soln in aluminium based metal organic backbone/graphene oxide composite material a concentration of 0.05~0.5g/L；
The water body containing tetracycline refers to the water body of Fourth Ring cellulose content≤100mg/L.
8. according to claim 1 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that：
The dosage satisfaction of the aluminium based metal organic backbone/graphene oxide composite material and the water body containing tetracycline makes to obtain
Absorption initial soln in aluminium based metal organic backbone/graphene oxide composite material a concentration of 0.15~0.25g/L.
9. according to claim 1 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that：
The absorption refers to that adsorption temp is 10~40 DEG C, adsorption time >=30min.
10. according to claim 1 remove tetracycline using aluminium based metal organic backbone/graphene oxide composite material
Method, it is characterised in that：
The pH value is 4~10.
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| CN109704952B (en) * | 2019-02-21 | 2022-02-08 | 浙江诺诚技术发展有限公司 | Preparation method and application of graphene oxide-metal complex |
| CN111548506A (en) * | 2020-05-12 | 2020-08-18 | 湖南鑫恒环境科技有限公司 | Cobalt ion doped metal organic framework material and preparation method thereof |
| CN111939878A (en) * | 2020-08-28 | 2020-11-17 | 陕西科技大学 | Ternary composite aerogel and preparation method and application thereof |
| CN112892599A (en) * | 2021-01-29 | 2021-06-04 | 华南理工大学 | IL/GO/Fe-based MOFs composite photocatalytic material and preparation method and application thereof |
| CN112892599B (en) * | 2021-01-29 | 2022-04-05 | 华南理工大学 | IL/GO/Fe-based MOFs composite photocatalytic material and preparation method and application thereof |
| CN115356305A (en) * | 2022-07-08 | 2022-11-18 | 徐州工程学院 | Preparation method of novel aluminum-based MOF material and application of novel aluminum-based MOF material in tetracycline detection |
| CN115356305B (en) * | 2022-07-08 | 2023-06-16 | 徐州工程学院 | Preparation method of aluminum-based MOF material and application of aluminum-based MOF material in tetracycline detection |
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Application publication date: 20180803 |