CN116535665B - Room-temperature preparation method and application of water-stable Zr-MOG material - Google Patents
Room-temperature preparation method and application of water-stable Zr-MOG material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 16
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 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 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 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 description 2
- JDFUJAMTCCQARF-UHFFFAOYSA-N tatb Chemical compound NC1=C([N+]([O-])=O)C(N)=C([N+]([O-])=O)C(N)=C1[N+]([O-])=O JDFUJAMTCCQARF-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 238000001308 synthesis method Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract 1
- 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 13
- CYDMQBQPVICBEU-UHFFFAOYSA-N chlorotetracycline Natural products C1=CC(Cl)=C2C(O)(C)C3CC4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-UHFFFAOYSA-N 0.000 description 13
- 229960003185 chlortetracycline hydrochloride Drugs 0.000 description 13
- 210000005266 circulating tumour cell Anatomy 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000013110 organic ligand Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 239000004098 Tetracycline Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 235000019364 tetracycline Nutrition 0.000 description 2
- 229940040944 tetracyclines Drugs 0.000 description 2
- 150000003522 tetracyclines Chemical class 0.000 description 2
- 206010059866 Drug resistance Diseases 0.000 description 1
- 239000004100 Oxytetracycline Substances 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229920006125 amorphous polymer Polymers 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229960004475 chlortetracycline Drugs 0.000 description 1
- 235000019365 chlortetracycline Nutrition 0.000 description 1
- CYDMQBQPVICBEU-XRNKAMNCSA-N chlortetracycline Chemical compound 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)=C3C(=O)C2=C1O CYDMQBQPVICBEU-XRNKAMNCSA-N 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229920001795 coordination polymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012821 model calculation Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229960000625 oxytetracycline Drugs 0.000 description 1
- IWVCMVBTMGNXQD-PXOLEDIWSA-N oxytetracycline Chemical compound C1=CC=C2[C@](O)(C)[C@H]3[C@H](O)[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O IWVCMVBTMGNXQD-PXOLEDIWSA-N 0.000 description 1
- 235000019366 oxytetracycline Nutrition 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- IWVCMVBTMGNXQD-UHFFFAOYSA-N terramycin dehydrate Natural products C1=CC=C2C(O)(C)C3C(O)C4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O IWVCMVBTMGNXQD-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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]
-
- 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
- B01J20/28014—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 form
- B01J20/28047—Gels
-
- 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
Abstract
The invention discloses a room-temperature preparation method and application of a water-stable metal organic gel material Zr-MOG, wherein the preparation method comprises the following steps: taking ZrOCl 2 ·8H 2 O is dissolved in water to obtain a solution with the concentration of 0.1 mol/L; adding TATB into water, and simultaneously adding TEA to promote dissolution in the water to obtain a solution with the concentration of 0.1 mol/L; mixing the two obtained solutions according to the volume ratio of 1:1, wherein Zr-MOG is instantaneously formed at room temperature; carrying out centrifugal washing on the obtained Zr-MOG for a plurality of times by water; and freeze-drying the obtained material to obtain the water-stable Zr-MOG material. The room-temperature synthesis method of the water-stable Zr-MOG material is energy-saving, simple and quick, and the prepared Zr-MOG material has the characteristics of rich active sites, large specific surface area, multi-stage pore structure and excellent water stability. The material is used for CTC in waterAdsorption removal and efficient adsorption enable the catalyst to have good application prospect.
Description
Technical Field
The invention belongs to the technical field of nano materials and environmental materials, and particularly relates to a room-temperature preparation method and application of a water-stable Zr-MOG material.
Background
Tetracyclines are a broad-spectrum antibiotic drug which is widely used in animal husbandry, agriculture, pharmaceutical industry, etc. because of its low cost and high efficacy, and mainly include tetracyclines, oxytetracycline, aureomycin, etc. The chlortetracycline hydrochloride (CTC) is difficult to degrade in the environment due to the special chemical property, and antibiotics accumulated in the environment for a long time not only can cause serious environmental pollution, but also can easily cause drug resistance genes of human bodies. Currently, the presence of CTCs has been detected in aquatic environments throughout the world. Therefore, removal of CTCs in aquatic environments has become a focus of attention.
Metal-organic gels (MOGs) are a class of coordination polymer gels, and amorphous polymers formed by coordinating Metal ions and organic ligands by supermolecular action have the characteristics of controllable Metal ions and adjustable organic ligands. The MOGs have potential values in the fields of adsorption, photocatalysis, medicines and the like because of the large specific surface area and the graded porous structure. The conventional MOGs synthesis method is time-consuming and energy-consuming, so that the development of a rapid thermal synthesis and energy-saving preparation method is important. In addition, most MOGs materials at present have the defect of unstable frameworks under water environment, and for tetravalent Zr ions in high valence state, the MOGs materials with extremely strong water outlet stability can be constructed because of generating more firm coordination bonds with organic ligands, and the original framework structure can be maintained even under the conditions of strong acid and strong alkali. In addition, tetravalent Zr ions have more exposed metal sites, so that the tetravalent Zr ions are more beneficial to capture of pollutants in water.
Disclosure of Invention
The invention aims to provide a room-temperature preparation method and application of a water-stable Zr-MOG material. The Zr-MOG material with large specific surface area, multiple pore structures, rich active sites and strong water stability is prepared by using the method with low energy consumption, simple operation, mild condition and short reaction time. The material is adopted to realize the adsorption removal of CTC in water.
In the present invention, TATB is 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine; TEA is triethylamine; CTC is aureomycin hydrochloride; zr-MOG is zirconium-based metal organic gel.
A room temperature preparation method of a water-stable Zr-MOG material comprises the following steps:
step 1): taking ZrOCl 2 ·8H 2 Dissolving O in water, and performing ultrasonic treatment to fully dissolve the O to obtain a solution with the concentration of 0.1 mol/L;
step 2): adding TATB into water, adding TEA to promote dissolution in water, and then performing ultrasonic treatment to fully dissolve to obtain a solution with the concentration of 0.1 mol/L;
step 3): mixing the solution obtained in the step 1) with the solution obtained in the step 2) according to the volume ratio of 1:1, and rapidly generating Zr-MOG under the room temperature condition;
step 4): washing Zr-MOG obtained in the step 3) for a plurality of times by water centrifugation;
step 5): and (3) freeze-drying the material obtained in the step (4) to obtain the water-stable Zr-MOG material.
The invention realizes the adsorption removal of CTC in water by using the water-stabilized Zr-MOG material. Wherein the adding amount of the Zr-MOG material in the water body is 1.0 g/L, and the adsorption temperature is 25 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. the Zr-MOG material prepared by the method has the conditions of room temperature, rapid and mild synthesis method, simple operation and low energy consumption;
2. the Zr-MOG material prepared by the invention has large specific surface area, graded pore structure and rich active sites;
3. the Zr-MOG material prepared by the invention has strong water stability;
4. the saturated adsorption capacity of CTC can reach 143.9mg/g.
Drawings
FIG. 1 is an SEM image of a water-stable Zr-MOG material prepared according to the present invention;
FIG. 2 is a BET plot of a water stable Zr-MOG material made in accordance with the present invention;
FIG. 3 is a FTIR diagram of a water stable Zr-MOG material made in accordance with the present invention;
FIG. 4 is an XRD pattern of a water-stabilized Zr-MOG material prepared according to the present invention;
FIG. 5 is a graph showing the adsorption effect of the water-stable Zr-MOG material prepared by the invention on CTC in water.
Description of the embodiments
Example 1A room temperature preparation method of a water stable Zr-MOG material comprises the following steps:
step 1): taking ZrOCl 2 ·8H 2 Dissolving O in water, and performing ultrasonic treatment to fully dissolve the O to obtain a solution with the concentration of 0.1 mol/L;
step 2): adding TATB into water, adding TEA to promote dissolution in water, and then performing ultrasonic treatment to fully dissolve to obtain a solution with the concentration of 0.1 mol/L;
step 3): mixing the solution obtained in the step 1) with the solution obtained in the step 2) according to the volume ratio of 1:1, and rapidly generating Zr-MOG under the room temperature condition;
step 4): washing Zr-MOG obtained in the step 3) for a plurality of times by water centrifugation;
step 5): and (3) freeze-drying the material obtained in the step (4) to obtain the water-stable Zr-MOG material.
Example 2: relates to an application of a water-stable Zr-MOG material as an adsorbent for removing CTC in water.
In practical application, the adsorption performance of the adsorbent provided by the invention on CTC in water can be tested by adopting the following scheme: adsorption experiments are carried out on CTC solutions with initial concentrations of 100mg/L, 150mg/L, 200mg/L, 250mg/L, 300mg/L, 350mg/L and 400mg/L respectively, zr-MOG provided by the invention is added respectively in an adding amount of 1.0 g/L, the adsorption temperature is kept at 25 ℃, a membrane filter with the thickness of 0.22 mu m is used for filtering the obtained sample, and then the absorbance of the CTC solution at 364 nm is measured by an ultraviolet spectrophotometer, so that the adsorption amount of the Zr-MOG on CTCs with different concentrations can be obtained. In addition, according to Langmuir fitting model calculation, the maximum adsorption quantity of the water-stable Zr-MOG material prepared by the invention to CTC in water body can reach 143.9mg/g.
SEM (scanning electron microscope) pictures of the water-stable Zr-MOG material prepared by the invention are shown in figure 1.
BET diagrams of the water-stable Zr-MOG materials prepared by the invention are shown in FIG. 2.
The FTIR of the water-stable Zr-MOG material prepared by the invention is shown in figure 3.
The XRD pattern of the water-stable Zr-MOG material prepared by the invention is shown in figure 4.
The adsorption effect of the water-stable Zr-MOG material prepared by the invention on CTC in water is shown in figure 5.
Claims (3)
1. The room-temperature preparation method of the water-stable Zr-MOG material is characterized by comprising the following steps of:
step 1): taking ZrOCl 2 ·8H 2 Dissolving O in water, and performing ultrasonic treatment to fully dissolve the O to obtain a solution with the concentration of 0.1 mol/L;
step 2): adding 2,4, 6-tris (4-carboxyphenyl) -1,3, 5-triazine into water, adding triethylamine to promote the solution in the water, and then performing ultrasonic treatment to fully dissolve the solution to obtain a solution with the concentration of 0.1 mol/L;
step 3): mixing the solution obtained in the step 1) with the solution obtained in the step 2) according to the volume ratio of 1:1, and rapidly generating Zr-MOG under the room temperature condition;
step 4): washing Zr-MOG obtained in the step 3) for a plurality of times by water centrifugation;
step 5): and (3) freeze-drying the material obtained in the step (4) to obtain the water-stable Zr-MOG material.
2. The use of the water-stable Zr-MOG material prepared by the method of claim 1 for adsorbing and removing aureomycin hydrochloride in water.
3. The use of the water-stable Zr-MOG material of claim 2 for adsorbing and removing aureomycin hydrochloride in a water body, wherein: the adding amount of the water-stable Zr-MOG material in the water body is 1.0 g/L, and the adsorption temperature is 25 ℃.
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| CN202310617572.3A CN116535665B (en) | 2023-05-30 | 2023-05-30 | Room-temperature preparation method and application of water-stable Zr-MOG material |
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| CN202310617572.3A CN116535665B (en) | 2023-05-30 | 2023-05-30 | Room-temperature preparation method and application of water-stable Zr-MOG material |
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