CN116284811B - Preparation method and application of Ga-MOGs - Google Patents
Preparation method and application of Ga-MOGs Download PDFInfo
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- CN116284811B CN116284811B CN202310063415.2A CN202310063415A CN116284811B CN 116284811 B CN116284811 B CN 116284811B CN 202310063415 A CN202310063415 A CN 202310063415A CN 116284811 B CN116284811 B CN 116284811B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- 239000000499 gel Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 5
- MSFXUHUYNSYIDR-UHFFFAOYSA-N 4-[4,6-bis(4-carboxyphenyl)-1,3,5-triazin-2-yl]benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1C1=NC(C=2C=CC(=CC=2)C(O)=O)=NC(C=2C=CC(=CC=2)C(O)=O)=N1 MSFXUHUYNSYIDR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- 239000003446 ligand Substances 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 239000011240 wet gel Substances 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 claims description 20
- 210000005266 circulating tumour cell Anatomy 0.000 claims description 19
- 238000009694 cold isostatic pressing Methods 0.000 claims description 19
- 208000037584 hereditary sensory and autonomic neuropathy Diseases 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229910009111 xH2 O Inorganic materials 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000003242 anti bacterial agent Substances 0.000 description 7
- 229940088710 antibiotic agent Drugs 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000003463 adsorbent Substances 0.000 description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- 229910002056 binary alloy Inorganic materials 0.000 description 3
- 229960001229 ciprofloxacin hydrochloride Drugs 0.000 description 3
- DIOIOSKKIYDRIQ-UHFFFAOYSA-N ciprofloxacin hydrochloride Chemical compound Cl.C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 DIOIOSKKIYDRIQ-UHFFFAOYSA-N 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 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 2
- 230000009471 action Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229940124307 fluoroquinolone Drugs 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- OGQYJDHTHFAPRN-UHFFFAOYSA-N 2-fluoro-6-(trifluoromethyl)benzonitrile Chemical compound FC1=CC=CC(C(F)(F)F)=C1C#N OGQYJDHTHFAPRN-UHFFFAOYSA-N 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000370 acceptor Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229960003185 chlortetracycline hydrochloride Drugs 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000013212 metal-organic material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 229940072172 tetracycline antibiotic Drugs 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A preparation method and application of Ga-MOGs are provided, wherein the preparation method is as follows: ga (NO 3)3·xH2 O0.1355 g) is weighed, placed in a glass container, 1 mL ethanol is added and ultrasonic treatment is carried out to fully dissolve the Ga (NO 3)3·xH2 O), 0.1576 g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine is weighed, dissolved in 5mL dimethyl sulfoxide and fully dissolved by ultrasonic treatment, the two solutions are mixed and ultrasonic treated, the mixed solution is transferred to a vacuum drying oven at 120 ℃ to heat 12h, the glass container is inverted to observe whether gel is formed, the obtained wet gel is dialyzed to remove metal ions and ligands which do not participate in coordination, and Ga-MOGs powder is obtained through freeze drying.
Description
Technical Field
The invention belongs to the field of nano material and environmental material preparation, and relates to a preparation method of Ga-MOGs and application of removing aureomycin hydrochloride and ciprofloxacin hydrochloride in an aqueous solution.
The Chinese name of Ga-MOGs is Ga-based metal organic gel.
Background
Antibiotics have the effects of preventing diseases and stimulating growth, are increasingly used in medicine, and are also used in action feeds. Antibiotics can have adverse effects on human health and ecosystem due to bioaccumulation, bioactivity, high water solubility, high persistence, even at low concentrations. Aureomycin hydrochloride (chlortetracycline hydrochloride, CTC) and ciprofloxacin hydrochloride (ciprofloxacin hydrochloride, CIP) are commonly present in domestic sewage, medical wastewater, industrial wastewater, surface water and even groundwater as the most typical tetracycline and fluoroquinolone antibiotics. Therefore, it is important to develop a technique for effectively removing antibiotics in water. The adsorption method has simple operation, economy, high efficiency and wide sources, and is considered as a promising means for removing organic pollutants in water.
The preparation of adsorbents with high adsorption capacity and selectivity is the key to antibiotic removal, and Metal-Organic gels (MOGs) are an emerging supermolecular Metal-Organic material, mainly by coordination interactions (e.g. hydrogen bonding, pi-pi stacking, van der waals forces) of Metal ions with Organic ligands to form porous networks. The unique hierarchical porous structure and high porosity of the porous structure help to quickly diffuse organic pollutant molecules, the ultrahigh specific surface area provides rich active sites to improve adsorption performance, so that huge application prospects are shown in the fields of catalysis, drug delivery, sensing, adsorption and the like, and the porous structure of the porous structure are possibly suitable for being adsorbed by MOGs through the actions of hydrogen bonds, pi-pi electron donor acceptors and the like, although the application of MOGs in the fields of selective adsorption and separation of antibiotics is still in a primary stage so far, the MOGs synthesized by trivalent metal centers (such as Al 3+、Fe3+) is reported to be used for removing antibiotics in water, but gallium-based MOGs (Ga-MOGs) is rarely constructed by using gallium, so that the exploration of novel gallium-based MOGs with large specific surface area and high porosity is necessary, and the application of the porous structure and the porous structure to the porous structure is possibly an ideal adsorbent for simultaneously removing CTC and CIP in an aqueous solution.
Disclosure of Invention
Aiming at the problems and the proposed feasible method, the invention provides a preparation method and application of Ga-MOGs material. The method has the greatest advantages that the preparation is simple and neutral, and the prepared novel Ga-MOGs material has larger specific surface area, high porosity, excellent stability, open metal sites and considerable adsorption capacity, and provides effective technical support for simultaneous removal of CTC and CIP in aqueous solution.
A preparation method of Ga-MOGs material comprises the following steps:
Step one: ga (NO 3)3·xH2 O0.1355 g) is weighed and placed in a glass container, 1 mL ethanol is added and the mixture is fully dissolved by ultrasonic treatment;
Step two: 0.1576 g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine is weighed out and dissolved in 5mL dimethyl sulfoxide, and is fully dissolved by ultrasound;
Step three: mixing the two solutions in the first step and the second step, performing ultrasonic treatment, transferring the mixed solution into a vacuum drying oven at 120 ℃ for heating 12 h, and inverting a glass container to observe whether gel is formed or not;
Step four: the wet gel obtained was dialyzed to remove metal ions and ligands not participating in the coordination, and Ga-MOGs powder was obtained by freeze-drying.
The invention provides an application of Ga-MOGs powder in removing CTC and CIP in water simultaneously, wherein the dosage of Ga-MOGs powder in water is 1.0 g/L, and the adsorption temperature is 298K.
The beneficial effects of the invention are as follows:
the Ga-MOGs provided by the invention is prepared under a solvothermal strategy, the steps of the preparation process are simple and environment-friendly, and the material can be used as an adsorbent for simultaneously removing CTC and CIP in an aqueous solution, thereby meeting the requirements of actual water treatment.
As can be seen from fig. 1, 2, 3, 4 and 5, the Ga-MOGs prepared according to the present invention has the following advantages:
1. large specific surface area, hierarchical porous structure;
2. Has rich active sites;
3. In the monobasic system, the saturated adsorption capacity of CTC can reach 406.50 mg/g, and the saturated adsorption capacity of CIP can reach 158.23 mg/g;
4. In the binary system, although the adsorption amount of Ga-MOGs to CTC and CIP is reduced, 207.90 mg/g and 126.90 mg/g can be achieved respectively.
The case results show that: the preparation method of Ga-MOGs provided by the invention is simple, and the synthesized Ga-MOGs has larger specific surface area, higher porosity, rich active sites and excellent stability, and can simultaneously and effectively remove tetracycline antibiotics and fluoroquinolone antibiotics in aqueous solution.
Drawings
FIG. 1 is a graph showing the adsorption and desorption curves and pore size distribution of N 2 of Ga-MOGs prepared according to the present invention;
FIG. 2 is an infrared spectrum of Ga-MOGs prepared according to the present invention;
FIG. 3 is a thermogravimetric plot of Ga-MOGs prepared according to the present invention;
FIG. 4 is a graph showing adsorption performance of Ga-MOGs prepared according to the present invention on CTC and CIP in a unitary system;
FIG. 5 is a graph showing adsorption performance of Ga-MOGs prepared according to the present invention on CTC and CIP in a binary system.
Description of the embodiments
Examples
A preparation method of Ga-MOGs material comprises the following steps:
Step one: ga (NO 3)3·xH2 O0.1355 g) is weighed and placed in a glass container, 1 mL ethanol is added and the mixture is fully dissolved by ultrasonic treatment;
Step two: 0.1576 g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine is weighed out and dissolved in 5mL dimethyl sulfoxide, and is fully dissolved by ultrasound;
Step three: mixing the two solutions in the first step and the second step, performing ultrasonic treatment, transferring the mixed solution into a vacuum drying oven at 120 ℃ for heating 12 h, and inverting a glass container to observe whether gel is formed or not;
Step four: the wet gel obtained was dialyzed to remove metal ions and ligands not participating in the coordination, and Ga-MOGs powder was obtained by freeze-drying.
Examples
Use of Ga-MOGs material to adsorb CTCs and CIPs from aqueous solutions.
In the adsorption experiment, the adsorption performance of the adsorbent provided by the invention on CTC and CIP in an aqueous solution can be tested by adopting the following scheme: in a monobasic system, preparing 50 mg/L, 75 mg/L, 100 mg/L, 150 mg/L, 200 mg/L, 300 mg/L, 400 mg/L, 600 mg/L and 800 mg/L of CTC and CIP solutions respectively, adding 1.0 g/L of Ga-MOGs provided by the invention, placing the reactor in a constant-temperature water bath oscillator in a dark environment, keeping the temperature at 298K, sampling for a certain time, filtering by a 0.22 mu m membrane filter, balancing, measuring the residual concentration of CTC and CIP in the solution by an ultraviolet spectrophotometer and having the maximum absorption wavelength of 365 nm and 270 nm, and obtaining the adsorption quantity of Ga-MOGs on CTC and CIP under different concentrations; for binary systems, the same concentration gradient as that of the monobasic system is adopted, the concentration ratio of CTC to CIP is always kept at 1:1, and the adsorption amounts of CTC and CIP at different concentrations are measured. In addition, the maximum adsorption amounts of Ga-MOGs material calculated according to Langmuir adsorption model in a monobasic system to CTC and CIP in an aqueous solution reach 406.50 mg/g and 158.23 mg/g respectively, and in a dibasic system to 207.90 mg/g and 126.90 mg/g respectively.
Claims (3)
1. A preparation method of Ga-MOGs is characterized in that: the method comprises the following steps:
Step one: ga (NO 3)3·xH2 O0.1355 g) is weighed and placed in a glass container, 1 mL ethanol is added and the mixture is fully dissolved by ultrasonic treatment;
Step two: 0.1576 g of 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine is weighed out and dissolved in 5mL dimethyl sulfoxide, and is fully dissolved by ultrasound;
Step three: mixing the two solutions in the first step and the second step, performing ultrasonic treatment, transferring the mixed solution into a vacuum drying oven at 120 ℃ for heating 12 h, and inverting a glass container to observe whether gel is formed or not;
Step four: the wet gel obtained was dialyzed to remove metal ions and ligands not participating in the coordination, and Ga-MOGs powder was obtained by freeze-drying.
2. Use of Ga-MOGs produced by the method of claim 1 to simultaneously remove CTCs and CIPs in aqueous solutions.
3. Use of Ga-MOGs according to claim 2 for simultaneous removal of CTCs and CIPs in aqueous solutions, characterized in that: the dosage of Ga-MOGs in the aqueous solution is 1.0 g/L, and the adsorption temperature is 298K.
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| CN202310063415.2A CN116284811B (en) | 2023-02-05 | 2023-02-05 | Preparation method and application of Ga-MOGs |
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| CN116284811A CN116284811A (en) | 2023-06-23 |
| CN116284811B true CN116284811B (en) | 2024-05-28 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249363A (en) * | 2011-07-13 | 2011-11-23 | 北京化工大学 | Method for using metal-organic framework material to purify water, exchange ions with water or magnetize water |
| CN108395544A (en) * | 2018-06-07 | 2018-08-14 | 中国科学院上海高等研究院 | A kind of large-scale producing method with triazine skeleton covalent polymer |
| CN109225144A (en) * | 2018-11-20 | 2019-01-18 | 河南师范大学 | A kind of preparation method of fluoroquinolone antibiotics adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US11642650B2 (en) * | 2020-05-14 | 2023-05-09 | Numat Technologies Inc. | Metal organic frameworks for removal of elemental impurities in pharmaceutical products |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249363A (en) * | 2011-07-13 | 2011-11-23 | 北京化工大学 | Method for using metal-organic framework material to purify water, exchange ions with water or magnetize water |
| CN108395544A (en) * | 2018-06-07 | 2018-08-14 | 中国科学院上海高等研究院 | A kind of large-scale producing method with triazine skeleton covalent polymer |
| CN109225144A (en) * | 2018-11-20 | 2019-01-18 | 河南师范大学 | A kind of preparation method of fluoroquinolone antibiotics adsorbent |
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