CN110041531A - The method of one step solvent structure Zn-MOF or Zn-Sn-MOF metal organic framework - Google Patents
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- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 14
- 229910007566 Zn-MOF Inorganic materials 0.000 title claims abstract description 9
- 239000013094 zinc-based metal-organic framework Substances 0.000 title claims abstract description 9
- 239000002904 solvent Substances 0.000 title abstract 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 70
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 39
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims abstract description 26
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 claims abstract description 17
- 238000004729 solvothermal method Methods 0.000 claims abstract description 11
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims 3
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000003446 ligand Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 abstract 1
- 229910017053 inorganic salt Inorganic materials 0.000 abstract 1
- 238000001878 scanning electron micrograph Methods 0.000 description 8
- 239000011148 porous material Substances 0.000 description 4
- GLBJKIIETSUMFV-UHFFFAOYSA-N O.O.O.O.O.Cl.Cl.Cl.Cl Chemical compound O.O.O.O.O.Cl.Cl.Cl.Cl GLBJKIIETSUMFV-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
本发明公开了一步溶剂热法合成Zn‑MOF或Zn‑Sn‑MOF金属有机骨架的方法，属于金属有机骨架的制备技术领域。将有机分子配体2‑甲基咪唑和无机盐硝酸锌分别溶解在甲醇溶剂中，再将两种溶液混合后加入不同浓度的五水合四氯化锡溶液，锌离子与2‑甲基咪唑结合成具有不同形貌的Zn‑Sn‑MOF金属有机框架。本发明具有成本低，装置简单，操作简易，高度可控，制备过程中不使用有毒试剂且对环境友好等优点。
The invention discloses a method for synthesizing Zn-MOF or Zn-Sn-MOF metal-organic framework by one-step solvothermal method, and belongs to the technical field of preparation of metal-organic framework. Dissolving the organic molecular ligand 2-methylimidazole and inorganic salt zinc nitrate in methanol solvent respectively, then mixing the two solutions and adding tin tetrachloride pentahydrate solutions of different concentrations, the zinc ion is combined with the 2-methylimidazole into Zn-Sn-MOF metal-organic frameworks with different morphologies. The invention has the advantages of low cost, simple device, simple operation, high controllability, no toxic reagents used in the preparation process, and environmental friendliness.
Description
技术领域technical field
本发明属于金属有机骨架的制备技术领域，具体涉及一种一步溶剂热法合成Zn-MOF或Zn-Sn-MOF金属有机骨架的方法。The invention belongs to the technical field of preparation of metal organic frameworks, in particular to a method for synthesizing Zn-MOF or Zn-Sn-MOF metal organic frameworks by one-step solvothermal method.
背景技术Background technique
金属有机骨架是一类由金属中心或者金属簇与有机配体以配位键的形式连接形成的具有特定拓扑结构和规则孔径的多孔材料。相比于其它多孔材料，具有更大的比表面积，其结构、多孔性和孔结构也可随金属或者配体的不同而进行调控,同时还可以进行功能化修饰改性,这些优异的特性使得材料在吸附与分离、催化和传感器等领域具有良好的潜在应用价值。Metal-organic frameworks are a class of porous materials with specific topology and regular pore size formed by the connection of metal centers or metal clusters with organic ligands in the form of coordination bonds. Compared with other porous materials, it has a larger specific surface area, and its structure, porosity and pore structure can also be adjusted with different metals or ligands. The material has good potential application value in the fields of adsorption and separation, catalysis and sensors.
发明内容SUMMARY OF THE INVENTION
本发明解决的技术问题是提供了一种工艺简单、成本低廉且高度可控的一步溶剂热法合成Zn-MOF或Zn-Sn-MOF金属有机骨架的方法。The technical problem solved by the present invention is to provide a method for synthesizing Zn-MOF or Zn-Sn-MOF metal organic framework by one-step solvothermal method with simple process, low cost and high controllability.
本发明为解决上述技术问题采用如下技术方案，一步溶剂热法合成Zn-MOF金属有机骨架的方法，其特征在于具体步骤为：将1.098g硝酸锌和3.300g 2-甲基咪唑分别加入到40mL甲醇溶液中并搅拌至完全溶解得到溶液A和溶液B，其中硝酸锌与2-甲基咪唑的质量比为1:3.3，将溶液A和溶液B搅拌混合均匀得到溶液C，将溶液C置于100-180℃高压反应釜中反应1-3h，反应结束后，自然冷却至室温，将产物取出后离心分离、干燥得到绣球花状的Zn-MOF金属有机骨架。The present invention adopts the following technical scheme in order to solve the above-mentioned technical problems, the method for synthesizing Zn-MOF metal organic framework by one-step solvothermal method is characterized in that the specific steps are: adding 1.098g zinc nitrate and 3.300g 2-methylimidazole to 40mL respectively solution A and solution B were obtained by stirring until completely dissolved in methanol solution, wherein the mass ratio of zinc nitrate and 2-methylimidazole was 1:3.3, and solution A and solution B were stirred and mixed to obtain solution C, and solution C was placed in the solution. The reaction is carried out in an autoclave at 100-180° C. for 1-3 hours. After the reaction is completed, it is naturally cooled to room temperature, and the product is taken out, centrifuged, and dried to obtain a hydrangea-like Zn-MOF metal organic framework.
本发明所述的一步溶剂热法合成Zn-Sn-MOF金属有机骨架的方法，其特征在于具体步骤为：将1.098g硝酸锌和3.300g 2-甲基咪唑分别加入到40mL甲醇溶液中并搅拌至完全溶解得到溶液A和溶液B，其中硝酸锌与2-甲基咪唑的摩尔比为1:3.3，将溶液A和溶液B搅拌混合均匀得到溶液C，将溶液C中加入五水合四氯化锡溶液后置于100-180℃高压反应釜中反应1-3h，其中五水合四氯化锡与硝酸锌的质量比为3:1，反应结束后自然冷却至室温，将产物取出后离心分离、干燥得到球形Zn-Sn-MOF金属有机骨架。The method for synthesizing Zn-Sn-MOF metal organic framework by one-step solvothermal method of the present invention is characterized in that the specific steps are: adding 1.098g zinc nitrate and 3.300g 2-methylimidazole to 40mL methanol solution respectively and stirring To completely dissolve to obtain solution A and solution B, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, stir and mix solution A and solution B to obtain solution C, add pentahydrate tetrachloride to solution C The tin solution is then placed in a 100-180 ℃ autoclave for 1-3 hours, wherein the mass ratio of tin tetrachloride pentahydrate and zinc nitrate is 3:1. After the reaction is completed, it is naturally cooled to room temperature, and the product is taken out and centrifuged. , drying to obtain spherical Zn-Sn-MOF metal organic framework.
本发明所述的一步溶剂热法合成Zn-Sn-MOF金属有机骨架的方法，其特征在于具体步骤为：将1.098g硝酸锌和3.300g 2-甲基咪唑分别加入到40mL甲醇溶液中并搅拌至完全溶解得到溶液A和溶液B，其中硝酸锌与2-甲基咪唑的摩尔比为1:3.3，将溶液A和溶液B搅拌混合均匀得到溶液C，在溶液C中加入五水合四氯化锡溶液后置于100-180℃高压反应釜中反应1-3h，其中五水合四氯化锡与硝酸锌的质量比为0.3:1，反应结束后自然冷却至室温，将产物取出后离心分离、干燥得到球形Zn-Sn-MOF金属有机骨架。The method for synthesizing Zn-Sn-MOF metal organic framework by one-step solvothermal method of the present invention is characterized in that the specific steps are: adding 1.098g zinc nitrate and 3.300g 2-methylimidazole to 40mL methanol solution respectively and stirring To completely dissolve to obtain solution A and solution B, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, stir and mix solution A and solution B to obtain solution C, add pentahydrate tetrachloride in solution C The tin solution is then placed in an autoclave at 100-180°C for 1-3 hours, wherein the mass ratio of tin tetrachloride pentahydrate and zinc nitrate is 0.3:1. After the reaction is completed, it is naturally cooled to room temperature, and the product is taken out and centrifuged. , drying to obtain spherical Zn-Sn-MOF metal organic framework.
本发明所述的一步溶剂热法合成Zn-Sn-MOF金属有机骨架的方法，其特征在于具体步骤为：将1.098g硝酸锌和3.300g 2-甲基咪唑分别加入到40mL甲醇溶液中并搅拌至完全溶解得到溶液A和溶液B，其中硝酸锌与2-甲基咪唑的摩尔比为1:3.3，将溶液A和溶液B搅拌混合均匀得到溶液C，在溶液C中加入五水合四氯化锡溶液后置于100-180℃高压反应釜中反应1-3h，其中五水合四氯化锡与硝酸锌的质量比为1:3，反应结束后自然冷却至室温，将产物取出后离心分离、干燥得到多面体形貌Zn-Sn-MOF金属有机骨架。The method for synthesizing Zn-Sn-MOF metal organic framework by one-step solvothermal method of the present invention is characterized in that the specific steps are: adding 1.098g zinc nitrate and 3.300g 2-methylimidazole to 40mL methanol solution respectively and stirring To completely dissolve to obtain solution A and solution B, wherein the molar ratio of zinc nitrate and 2-methylimidazole is 1:3.3, stir and mix solution A and solution B to obtain solution C, add pentahydrate tetrachloride in solution C The tin solution is then placed in an autoclave at 100-180°C for 1-3h reaction, wherein the mass ratio of tin tetrachloride pentahydrate and zinc nitrate is 1:3. After the reaction is completed, it is naturally cooled to room temperature, and the product is taken out and centrifuged. , drying to obtain polyhedral morphology Zn-Sn-MOF metal organic framework.
本发明具有成本低廉、装置简单、操作简易、高度可控、制备过程中不使用有毒试剂及环境友好等优点，通过控制硝酸锌和五水合四氯化锡的物料配比即可得到不同形貌的Zn-Sn-MOF金属有机骨架。The invention has the advantages of low cost, simple device, simple operation, high controllability, no toxic reagents in the preparation process, environmental friendliness and the like, and different morphologies can be obtained by controlling the material ratio of zinc nitrate and tin tetrachloride pentahydrate. Zn-Sn-MOF metal-organic framework.
附图说明Description of drawings
图1是实施例1制得绣球花状的Zn-MOF金属有机骨架的SEM图；Fig. 1 is the SEM image of the hydrangea-shaped Zn-MOF metal-organic framework obtained in Example 1;
图2是实施例2制得球形Zn-Sn-MOF金属有机骨架的SEM图；Fig. 2 is the SEM image of spherical Zn-Sn-MOF metal-organic framework obtained in Example 2;
图3是实施例3制得球形Zn-Sn-MOF金属有机骨架的SEM图；Fig. 3 is the SEM image of spherical Zn-Sn-MOF metal-organic framework obtained in Example 3;
图4是实施例4制得多面体形Zn-Sn-MOF金属有机骨架的SEM图。FIG. 4 is a SEM image of the polyhedral Zn-Sn-MOF metal-organic framework prepared in Example 4. FIG.
具体实施方式Detailed ways
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。The above-mentioned content of the present invention is described in further detail below through the examples, but it should not be understood that the scope of the above-mentioned subject matter of the present invention is limited to the following examples, and all technologies realized based on the above-mentioned content of the present invention belong to the scope of the present invention.
实施例1Example 1
将1.098g硝酸锌和3.300g 2-甲基咪唑分别加入到40mL甲醇溶液中并搅拌至完全溶解得到溶液A和溶液B，其中硝酸锌与2-甲基咪唑的质量比为1:3.3，将溶液A和溶液B搅拌混合均匀得到溶液C，将溶液C置于160℃高压反应釜中反应2h，反应结束后，自然冷却至室温，将产物取出后离心分离、干燥得到绣球花状的Zn-MOF金属有机骨架，其SEM图如图1所示。1.098g of zinc nitrate and 3.300g of 2-methylimidazole were respectively added to 40mL methanol solution and stirred until completely dissolved to obtain solution A and solution B, wherein the mass ratio of zinc nitrate and 2-methylimidazole was 1:3.3, the The solution A and the solution B were stirred and mixed evenly to obtain the solution C. The solution C was placed in an autoclave at 160 ° C for reaction for 2 hours. After the reaction was completed, it was naturally cooled to room temperature. The SEM image of the MOF metal-organic framework is shown in Figure 1.
实施例2Example 2
将1.098g硝酸锌和3.300g 2-甲基咪唑分别加入到40mL甲醇溶液中并搅拌至完全溶解得到溶液A和溶液B，其中硝酸锌与2-甲基咪唑的摩尔比为1:3.3，将溶液A和溶液B搅拌混合均匀得到溶液C，在溶液C中加入五水合四氯化锡溶液后置于160℃高压反应釜中反应2h，其中五水合四氯化锡与硝酸锌的质量比为3:1，反应结束后自然冷却至室温，将产物取出后离心分离、干燥得到球形Zn-Sn-MOF金属有机骨架，其SEM图如图2所示。1.098g of zinc nitrate and 3.300g of 2-methylimidazole were respectively added to 40mL methanol solution and stirred until completely dissolved to obtain solution A and solution B, wherein the mol ratio of zinc nitrate and 2-methylimidazole was 1:3.3, and the The solution A and the solution B are stirred and mixed evenly to obtain the solution C. After adding the tin tetrachloride pentahydrate solution to the solution C, it is placed in a 160 ℃ autoclave for reaction for 2 hours, wherein the mass ratio of tin tetrachloride pentahydrate and zinc nitrate is: 3:1, after the reaction, it was naturally cooled to room temperature, and the product was taken out, centrifuged, and dried to obtain a spherical Zn-Sn-MOF metal-organic framework, the SEM image of which is shown in FIG. 2 .
实施例3Example 3
将1.098g硝酸锌和3.300g 2-甲基咪唑分别加入到40mL甲醇溶液中并搅拌至完全溶解得到溶液A和溶液B，其中硝酸锌与2-甲基咪唑的摩尔比为1:3.3，将溶液A和溶液B搅拌混合均匀得到溶液C，在溶液C中加入五水合四氯化锡溶液后置于160℃高压反应釜中反应2h，其中五水合四氯化锡与硝酸锌的质量比为0.3:1，反应结束后自然冷却至室温，将产物取出后离心分离、干燥得到球形Zn-Sn-MOF金属有机骨架，其SEM图如图3所示。1.098g of zinc nitrate and 3.300g of 2-methylimidazole were respectively added to 40mL methanol solution and stirred until completely dissolved to obtain solution A and solution B, wherein the mol ratio of zinc nitrate and 2-methylimidazole was 1:3.3, and the The solution A and the solution B are stirred and mixed evenly to obtain the solution C. After adding the tin tetrachloride pentahydrate solution to the solution C, it is placed in a 160 ℃ autoclave for reaction for 2 hours, wherein the mass ratio of tin tetrachloride pentahydrate and zinc nitrate is: 0.3:1, after the reaction, it was naturally cooled to room temperature, and the product was taken out, centrifuged, and dried to obtain a spherical Zn-Sn-MOF metal-organic framework, the SEM image of which is shown in Figure 3.
实施例4Example 4
将1.098g硝酸锌和3.300g 2-甲基咪唑分别加入到40mL甲醇溶液中并搅拌至完全溶解得到溶液A和溶液B，其中硝酸锌与2-甲基咪唑的摩尔比为1:3.3，将溶液A和溶液B搅拌混合均匀得到溶液C，在溶液C中加入五水合四氯化锡溶液后置于160℃高压反应釜中反应2h，其中五水合四氯化锡与硝酸锌的质量比为1:3，反应结束后自然冷却至室温，将产物取出后离心分离、干燥得到多面体形Zn-Sn-MOF金属有机骨架，其SEM图如图4所示。1.098g of zinc nitrate and 3.300g of 2-methylimidazole were respectively added to 40mL methanol solution and stirred until completely dissolved to obtain solution A and solution B, wherein the mol ratio of zinc nitrate and 2-methylimidazole was 1:3.3, and the The solution A and the solution B are stirred and mixed evenly to obtain the solution C. After adding the tin tetrachloride pentahydrate solution to the solution C, it is placed in a 160 ℃ autoclave for reaction for 2 hours, wherein the mass ratio of tin tetrachloride pentahydrate and zinc nitrate is: 1:3, after the reaction, it was naturally cooled to room temperature, and the product was taken out, centrifuged, and dried to obtain a polyhedral Zn-Sn-MOF metal-organic framework, the SEM image of which is shown in FIG. 4 .
以上实施例描述了本发明的基本原理、主要特征及优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明原理的范围下，本发明还会有各种变化和改进，这些变化和改进均落入本发明保护的范围内。The above embodiments describe the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. The above embodiments and descriptions only describe the principles of the present invention. Without departing from the scope of the principles of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the protection scope of the present invention.
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| CN111072690A (en) * | 2019-12-25 | 2020-04-28 | 中国科学院宁波材料技术与工程研究所 | A kind of flower-shaped metal-organic framework composite material, its preparation method and application |
| CN112479246A (en) * | 2020-12-03 | 2021-03-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of Ni-doped stannic oxide formaldehyde sensitive composite material based on ZIF-8 metal organic framework template, product and application |
| CN116334653A (en) * | 2021-12-16 | 2023-06-27 | 中国科学院大连化学物理研究所 | A tin-based metal-organic framework catalyst and its preparation method and application in electrocatalysis of CO2 |
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