CN116535665B - A room temperature preparation method and application of water-stable Zr-MOG material - Google Patents
A 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 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001179 sorption measurement Methods 0.000 claims abstract description 15
- 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
- 238000000034 method Methods 0.000 claims 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 description 2
- 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 2
- 238000009210 therapy by ultrasound Methods 0.000 claims 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000004108 freeze drying Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 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
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- 238000001308 synthesis method Methods 0.000 abstract description 3
- 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 15
- 229960003185 chlortetracycline hydrochloride Drugs 0.000 description 15
- 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 14
- 238000010586 diagram Methods 0.000 description 4
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- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 210000005266 circulating tumour cell Anatomy 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
- 239000000499 gel Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 239000004099 Chlortetracycline Substances 0.000 description 1
- 239000004100 Oxytetracycline Substances 0.000 description 1
- 239000004098 Tetracycline 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
- 229940124350 antibacterial drug Drugs 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960004475 chlortetracycline Drugs 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
- 235000019365 chlortetracycline Nutrition 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
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- 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
- 239000000126 substance Substances 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
- 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
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- 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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- 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
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- 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
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- 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
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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
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Abstract
本发明公开了一种水稳定的金属有机凝胶材料Zr‑MOG的室温制备方法及应用，制备方法为：取ZrOCl2·8H2O溶于水中，得到浓度为0.1 mol/L的溶液；取TATB加入水中，同时添加TEA促进其在水中溶解，得到浓度为0.1 mol/L的溶液；按照体积1:1的比例将所得到的两种溶液混合，Zr‑MOG在室温下瞬间形成；将得到的Zr‑MOG经水离心洗涤多次；对所得的材料进行冷冻干燥，最后得到水稳定Zr‑MOG材料。本发明的水稳定Zr‑MOG材料的室温合成方法节能、简单及快速，制得的Zr‑MOG材料具有丰富的活性位点、大的比表面积、多级的孔隙结构和优异的水稳定性的特点。该材料用于水中CTC的吸附去除，高效的吸附使其具有良好的应用前景。The invention discloses a room temperature preparation method and application of a water-stable metal organic gel material Zr-MOG. The preparation method is: dissolve ZrOCl 2 ·8H 2 O in water to obtain a solution with a concentration of 0.1 mol/L; TATB is added to water, and TEA is added to promote its dissolution in water to obtain a solution with a concentration of 0.1 mol/L; the two solutions obtained are mixed in a ratio of 1:1 by volume, and Zr‑MOG is formed instantly at room temperature; the result The Zr‑MOG was centrifuged and washed with water several times; the resulting material was freeze-dried, and finally a water-stable Zr‑MOG material was obtained. The room temperature synthesis method of the water-stable Zr-MOG material of the present invention is energy-saving, simple and fast. The prepared Zr-MOG material has rich active sites, large specific surface area, multi-level pore structure and excellent water stability. Features. This material is used for the adsorption and removal of CTC in water, and its efficient adsorption makes it have good application prospects.
Description
技术领域Technical field
本发明属于纳米材料与环境材料技术领域，具体涉及一种水稳定Zr-MOG材料的室温制备方法及其应用。The invention belongs to the technical field of nanomaterials and environmental materials, and specifically relates to a room temperature preparation method of water-stable Zr-MOG material and its application.
背景技术Background technique
四环素类抗生素是一类广谱抗菌药物，因其低成本和高功效而被广泛的应用于畜牧业、农业及制药业等，其主要包括四环素、土霉素和金霉素等。其中盐酸金霉素（CTC）因其特殊的化学性质，使其在环境中难以降解，长期累积在环境中的抗生素不仅会造成严重的环境污染，还易使人体产生耐药基因。目前，世界各地的水生环境中都已检测到CTC的存在。因此，去除水生环境中的CTC已经成为人们关注的重点。Tetracycline antibiotics are a class of broad-spectrum antibacterial drugs that are widely used in animal husbandry, agriculture and pharmaceutical industries due to their low cost and high efficacy. They mainly include tetracycline, oxytetracycline and chlortetracycline. Among them, chlortetracycline hydrochloride (CTC) is difficult to degrade in the environment due to its special chemical properties. Antibiotics accumulated in the environment for a long time will not only cause serious environmental pollution, but also easily cause the human body to develop drug-resistant genes. Currently, CTCs have been detected in aquatic environments around the world. Therefore, the removal of CTCs from the aquatic environment has become a focus of attention.
金属有机凝胶（Metal-organic gels,简称MOGs）是一类配位聚合物凝胶，通过利用超分子作用使金属离子和有机配体配位而形成的非晶态聚合物，具有金属离子可控和有机配体可调节的特点。MOGs因其具有大的比表面积和分级的多孔结构，使其在吸附、光催化以及药物等领域有着潜在价值。常规的MOGs合成方法大多耗时耗能，因此，开发一种快速温合及节能的制备方法是重中之重。此外，目前大多数的MOGs材料在水环境下会显露其骨架不稳定的缺点，而对于高价态的四价Zr离子，因能与有机配体产生更牢固的配位键，而可以构筑出水稳定性极强的MOGs材料，甚至在强酸、强碱的条件下仍可以保持原本的骨架结构。另外，四价Zr离子拥有更多的裸露的金属位点使其更有利于对水中污染物的捕获。Metal-organic gels (MOGs for short) are a type of coordination polymer gel. They are amorphous polymers formed by using supramolecular interactions to coordinate metal ions and organic ligands. They have the ability to bind metal ions. It has the characteristics of adjustable control and organic ligands. Because of their large specific surface area and hierarchical porous structure, MOGs have potential value in the fields of adsorption, photocatalysis, and medicine. Conventional MOGs synthesis methods are mostly time-consuming and energy-consuming. Therefore, developing a fast, warm and energy-saving preparation method is a top priority. In addition, most current MOGs materials will show the disadvantage of unstable skeletons in aqueous environments. However, for high-valence tetravalent Zr ions, they can form stronger coordination bonds with organic ligands and can build water-stable structures. The extremely strong MOGs material can maintain its original skeleton structure even under strong acid and alkali conditions. In addition, tetravalent Zr ions have more exposed metal sites, making them more conducive to capturing pollutants in water.
发明内容Contents of the invention
本发明的目的在于提供一种水稳定Zr-MOG材料的室温制备方法及其应用。利用耗能低、操作简单、条件温和及反应时间短的方法制得具有大的比表面积、多元的孔结构、丰富的活性位点以及水稳定性强的Zr-MOG材料。采用此材料实现对水中CTC的吸附去除。The purpose of the present invention is to provide a room temperature preparation method and application of water-stable Zr-MOG material. Zr-MOG materials with large specific surface area, multi-dimensional pore structure, abundant active sites and strong water stability are prepared using methods with low energy consumption, simple operation, mild conditions and short reaction time. This material is used to achieve the adsorption and removal of CTC in water.
本发明中，TATB为2,4,6-三（4-羧基苯基）-1,3,5-三嗪；TEA为三乙胺；CTC为盐酸金霉素；Zr-MOG为锆基金属有机凝胶。In the present invention, TATB is 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine; TEA is triethylamine; CTC is chlortetracycline hydrochloride; Zr-MOG is zirconium-based metal Organogel.
一种水稳定Zr-MOG材料的室温制备方法，包括如下步骤：A method for preparing water-stable Zr-MOG materials at room temperature, including the following steps:
步骤1）：取ZrOCl2·8H2O溶于水中，超声使其充分溶解，得到浓度为0.1 mol/L的溶液；Step 1): Dissolve ZrOCl 2 ·8H 2 O in water and use ultrasonic to fully dissolve it to obtain a solution with a concentration of 0.1 mol/L;
步骤2）：取TATB加入水中，同时添加TEA促进其在水中溶解，随后超声使其充分溶解，得到浓度为0.1 mol/L的溶液；Step 2): Add TATB to water, add TEA at the same time to promote its dissolution in water, and then use ultrasound to fully dissolve it to obtain a solution with a concentration of 0.1 mol/L;
步骤3）：按照体积1:1的比例将步骤1）所得到的溶液与步骤2）所得到的溶液混合，Zr-MOG在室温条件下快速生成；Step 3): Mix the solution obtained in step 1) and the solution obtained in step 2) according to a volume ratio of 1:1. Zr-MOG is rapidly generated at room temperature;
步骤4）：将步骤3）所得的Zr-MOG经水离心洗涤多次；Step 4): Centrifuge and wash the Zr-MOG obtained in step 3) several times with water;
步骤5）：将步骤4）所得的材料进行冷冻干燥，最后得到水稳定Zr-MOG材料。Step 5): Freeze-dry the material obtained in step 4), and finally obtain a water-stable Zr-MOG material.
本发明利用水稳定Zr-MOG材料实现对水中CTC的吸附去除。其中Zr-MOG材料在水体中的投加量为1.0 g/L,吸附温度为25℃。The present invention utilizes water-stabilized Zr-MOG materials to achieve adsorption and removal of CTC in water. The dosage of Zr-MOG material in water is 1.0 g/L, and the adsorption temperature is 25°C.
相对于现有技术，本发明具有的有益效果是：Compared with the prior art, the beneficial effects of the present invention are:
1、本发明制备的Zr-MOG材料的条件是室温，合成方法迅速、温和、操作简单以及能耗低；1. The conditions for the Zr-MOG material prepared by the present invention are room temperature, and the synthesis method is rapid, gentle, simple to operate and has low energy consumption;
2、本发明制备的Zr-MOG材料具有大的比表面积、分级的孔结构及丰富的活性位点；2. The Zr-MOG material prepared by the present invention has a large specific surface area, graded pore structure and abundant active sites;
3、本发明制备的Zr-MOG材料具有强的水稳定性；3. The Zr-MOG material prepared by the present invention has strong water stability;
4、对CTC的饱和吸附量可达到143.9 mg/g。4. The saturated adsorption capacity of CTC can reach 143.9 mg/g.
附图说明Description of the drawings
图1是本发明制得的水稳定Zr-MOG材料的SEM图；Figure 1 is an SEM image of the water-stable Zr-MOG material prepared by the present invention;
图2是本发明制得的水稳定Zr-MOG材料的BET图；Figure 2 is a BET diagram of the water-stable Zr-MOG material prepared by the present invention;
图3是本发明制得的水稳定Zr-MOG材料的FTIR图；Figure 3 is an FTIR diagram of the water-stable Zr-MOG material prepared by the present invention;
图4是本发明制得的水稳定Zr-MOG材料的XRD图；Figure 4 is an XRD pattern of the water-stable Zr-MOG material prepared by the present invention;
图5是本发明制得的水稳定Zr-MOG材料对于水体中CTC的吸附效果图。Figure 5 is a diagram showing the adsorption effect of the water-stable Zr-MOG material prepared by the present invention on CTC in water.
实施方式Implementation
实施例1:一种水稳定Zr-MOG材料的室温制备方法，包括如下步骤：Embodiment 1: A method for preparing water-stable Zr-MOG material at room temperature, including the following steps:
步骤1）：取ZrOCl2·8H2O溶于水中，超声使其充分溶解，得到浓度为0.1 mol/L的溶液；Step 1): Dissolve ZrOCl 2 ·8H 2 O in water and use ultrasonic to fully dissolve it to obtain a solution with a concentration of 0.1 mol/L;
步骤2）：取TATB加入水中，同时添加TEA促进其在水中溶解，随后超声使其充分溶解，得到浓度为0.1 mol/L的溶液；Step 2): Add TATB to water, add TEA at the same time to promote its dissolution in water, and then use ultrasound to fully dissolve it to obtain a solution with a concentration of 0.1 mol/L;
步骤3）：按照体积1:1的比例将步骤1）所得到的溶液与步骤2）所得到的溶液混合，Zr-MOG在室温条件下快速生成；Step 3): Mix the solution obtained in step 1) and the solution obtained in step 2) according to a volume ratio of 1:1. Zr-MOG is rapidly generated at room temperature;
步骤4）：将步骤3）所得的Zr-MOG经水离心洗涤多次；Step 4): Centrifuge and wash the Zr-MOG obtained in step 3) several times with water;
步骤5）：将步骤4）所得的材料进行冷冻干燥，最后得到水稳定Zr-MOG材料。Step 5): Freeze-dry the material obtained in step 4), and finally obtain a water-stable Zr-MOG material.
实施例2：涉及水稳定Zr-MOG材料作为吸附剂去除水体中CTC的应用。Example 2: Involves the application of water-stable Zr-MOG material as an adsorbent to remove CTC in water.
在实际应用中，本发明所提供的吸附剂对水体中CTC的吸附性能可采用以下方案进行测试：对初始浓度分别为100mg/L、150mg/L、200mg/L、250mg/L、300mg/L、350mg/L和400mg/L的CTC溶液进行吸附实验，以1.0 g/L的投加量分别加入本发明所提供的Zr-MOG，保持吸附温度为25℃，使用0.22μm 的膜过滤器过滤所取样品，而后通过紫外分光光度计测量364 nm处的CTC溶液的吸光度，即可获得Zr-MOG对不同浓度的CTC的吸附量。此外，根据Langmuir拟合模型计算，本发明制得的水稳定Zr-MOG材料对水体中CTC的最大吸附量可以达到143.9mg/g。In practical applications, the adsorption performance of the adsorbent provided by the present invention for CTC in water can be tested using the following scheme: the initial concentrations are 100 mg/L, 150 mg/L, 200 mg/L, 250 mg/L, and 300 mg/L respectively. Conduct adsorption experiments with CTC solutions of , 350 mg/L and 400 mg/L, respectively add Zr-MOG provided by the invention at a dosage of 1.0 g/L, keep the adsorption temperature at 25°C, and filter using a 0.22 μm membrane filter. Take the sample and then measure the absorbance of the CTC solution at 364 nm with a UV spectrophotometer to obtain the adsorption capacity of Zr-MOG for CTC at different concentrations. In addition, according to Langmuir fitting model calculations, the maximum adsorption capacity of the water-stable Zr-MOG material produced in the present invention for CTC in water can reach 143.9 mg/g.
本发明制得的水稳定Zr-MOG材料的SEM图如图1所示。The SEM image of the water-stable Zr-MOG material prepared by the present invention is shown in Figure 1.
本发明制得的水稳定Zr-MOG材料的BET图如图2所示。The BET diagram of the water-stable Zr-MOG material prepared by the present invention is shown in Figure 2.
本发明制得的水稳定Zr-MOG材料的FTIR图如图3所示。The FTIR pattern of the water-stable Zr-MOG material prepared by the present invention is shown in Figure 3.
本发明制得的水稳定Zr-MOG材料的XRD图如图4所示。The XRD pattern of the water-stable Zr-MOG material prepared by the present invention is shown in Figure 4.
本发明制得的水稳定Zr-MOG材料对于水体中CTC的吸附效果如图5所示。The adsorption effect of the water-stable Zr-MOG material prepared by the present invention on CTC in water is shown in Figure 5.
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