CN109593209B - Method for preparing zeolite imidazole ester framework material ZIF-8 nano octapods through seed growth synthesis - Google Patents
Method for preparing zeolite imidazole ester framework material ZIF-8 nano octapods through seed growth synthesis Download PDFInfo
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Abstract
The invention relates to a method for preparing a zeolite imidazole ester framework material ZIF-8 nanometer octapods by using seed growth synthesis, which comprises the following steps: (1) mixing and dissolving zinc salt, imidazole ligand, surfactant and water at room temperature, keeping the temperature at room temperature for 1-4h, washing to obtain ZIF-8 truncated dodecahedral seeds, and dispersing into water to obtain seed dispersion liquid; (2) stirring, mixing and dissolving zinc salt, imidazole ligand, surfactant, seed dispersion liquid and solvent at room temperature, preserving heat at room temperature for 1-12h, and washing to obtain a ZIF-8 nano octopodosome product. The nano octopodomer ZIF-8 synthesized by the method breaks through the bottleneck of the polyhedral morphology of the ZIF-8 for a long time, and provides more possibility for the morphology of the product of the ZIF-8.
Description
The technical field is as follows:
the invention relates to a method for preparing a ZIF-8 nano octapods, belonging to the technical field of synthesis of crystal materials.
Background art:
zeolite imidazolate framework materials (ZIFs) are metal organic framework Materials (MOFs) with zeolite framework structures, wherein transition metals are mainly divalent Zn, Co and the like, and organic ligands are imidazole or imidazole derivatives. Compared with the traditional zeolite, the transition metal ions replace Si and Al elements in the traditional zeolite, and the imidazole ester replaces an oxygen bridge in the traditional zeolite and is connected through nitrogen atoms on an imidazole ring to form a zeolite-like structural material.
ZIF-8 is a member of zeolitic imidazolate framework materials (ZIFs) consisting of 2-methylimidazole and the metal atom Zn, each of which coordinates with the N atom of four 2-methylimidazole rings to form a ZnN having a regular tetrahedral structure4Clusters are taken as nodes and are connected through imidazole rings on 2-methylimidazole to form a cage-shaped coordination compound with a regular hexahedral crystal form. ZIF-8 has a higher specific surface area (up to 1947 m) than other inorganic particles2/g), high thermal stability and good chemical stability. Because of these advantages, ZIF-8 is widely used in the fields of catalysis, gas separation and storage.
The existing preparation technology of ZIF-8 mainly comprises a room temperature synthesis method, a hydrothermal method, a template method, a microwave synthesis method and the like. For example: chinese patent document CN105985362A discloses a method for preparing a zeolitic imidazolate framework material, which uses inorganic base or organic amine as a deprotonating agent to form a zeolitic imidazolate framework material (ZIFs) from imidazole compounds and zinc and cobalt metal ions at normal temperature and pressure. The method is rapid and efficient, has high purity of target product, contains no impurities such as zinc oxide, etc., has nanometer particle size, high specific surface area and yield of more than 85%. Chinese patent document CN108129670A discloses a preparation method of a gradient porous metal organic framework ZIF-8, which comprises the steps of dissolving an organic ligand 2-methylimidazole in deionized water, adding a polydiallyldimethylammonium chloride solution after the 2-methylimidazole is completely dissolved, and uniformly stirring; dissolving divalent zinc salt in deionized water, mixing with the organic ligand solution after completely dissolving, and stirring to react to obtain a suspension; and filtering or centrifugally separating the suspension to obtain a solid product, washing the solid product with deionized water, and drying to obtain the ZIF-8 series material. However, most of the methods are one-step synthesis methods, and are difficult to control in the nucleation and growth stages, so that the control and innovation of the morphology of ZIF-8 are limited.
The invention content is as follows:
aiming at the defects of the prior art, the invention provides a preparation method of a ZIF-8 nano octapods.
Description of terms:
room temperature: the room temperature of the invention is the temperature of the operation environment, and is generally 15-28 ℃.
The technical scheme of the invention is as follows:
a method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) mixing and dissolving zinc salt, imidazole ligand, surfactant and water at room temperature, keeping the temperature at room temperature for 1-4h, washing to obtain ZIF-8 truncated dodecahedral seeds, and dispersing into water to obtain seed dispersion liquid;
(2) stirring, mixing and dissolving zinc salt, imidazole ligand, surfactant, seed dispersion liquid and solvent at room temperature, preserving heat at room temperature for 1-12h, and washing to obtain a ZIF-8 nano octopodosome product.
According to the present invention, preferably, the zinc salt in step (1) comprises one of zinc nitrate, zinc acetate, zinc sulfate and zinc chloride, preferably zinc acetate;
the imidazole ligand comprises one of imidazole, 2-methylimidazole, nitroimidazole, benzimidazole, 4-methylimidazole, 4-nitroimidazole and N-propylimidazole, and 2-methylimidazole is preferred;
the surfactant comprises one of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride, polyvinylpyrrolidone, sodium polystyrene sulfonate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate, and preferably cetyl trimethyl ammonium bromide.
According to the present invention, it is preferable that the molar ratio of the zinc salt, the imidazole ligand and the surfactant in the step (1) is (1-2): (12-15): (0.002-0.004), and more preferably 1.37: 13.6: 0.0025;
preferably, the volume ratio of the molar amount of the imidazole ligand to the water is 13.6: (8-15) mol/L.
According to the present invention, it is preferable that the washing reagent in step (1) is methanol, water or ethanol;
preferably, the mass concentration of the seed dispersion liquid is 1-100 g/L.
According to the present invention, preferably, the zinc salt in step (2) comprises one of zinc nitrate, zinc acetate, zinc sulfate and zinc chloride, preferably zinc nitrate;
the imidazole ligand comprises one of imidazole, 2-methylimidazole, nitroimidazole, benzimidazole, 4-methylimidazole, 4-nitroimidazole and N-propylimidazole, and 2-methylimidazole is preferred;
the surfactant comprises one of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride, polyvinylpyrrolidone, sodium polystyrene sulfonate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate, and preferably cetyl trimethyl ammonium bromide.
The solvent is one of water, methanol and N, N-dimethylformamide, and preferably water.
According to the present invention, it is preferable that the molar ratio of the zinc salt, the imidazole ligand and the surfactant in the step (2) is (1-200): (100-3000): (0.01-4); further preferably 0.096:1.32: 0.00144;
preferably, the volume ratio of the molar usage of the imidazole ligand to the solvent is (0.1-3): (2-4) mol/L, more preferably 1.32:3 mol/L;
preferably, the volume ratio of the molar amount of the imidazole ligand to the seed dispersion is (0.1-3): (0.1-0.5) mol/L, more preferably 1.32:0.2 mol/L.
The principle and the beneficial effects of the invention are as follows:
1. the invention uses a seed growth method to prepare the ZIF-8 nanometer octapods, and selects pre-synthesized seeds rather than precursors as the starting points of crystal growth. Generally, seeds are initially of high purity in terms of size, shape and crystallinity, and then are introduced sequentially with reagents such as precursors, reducing agents, capping agents, etc., in that order, to initiate crystal growth. Compared with the one-step synthesis method, the method can avoid the complex and difficult-to-control initial nucleation step and accurately control the growth stage from the aspects of thermodynamics and kinetics.
2. The preparation method has simple conditions, does not need heating, microwave and other conditions, and can be successfully synthesized only at room temperature. And the morphology can be precisely controlled.
3. The nano octopodomer ZIF-8 synthesized by the method breaks through the bottleneck of the polyhedral morphology of the ZIF-8 for a long time, and provides more possibility for the morphology of the product of the ZIF-8.
Description of the drawings:
FIG. 1 is a low Scanning Electron Microscope (SEM) image of ZIF-8 nano octapods made in example 1.
FIG. 2 is a high Scanning Electron Microscope (SEM) image of ZIF-8 nano octapods made in example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples, but is not limited thereto.
Example 1
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Scanning Electron Microscope (SEM) images of the ZIF-8 nano octapods produced in this example are shown in fig. 1 and 2. As shown in fig. 1 and 2, after the cubic seeds grow into larger cubes, rod-shaped structures with lengths of about 300nm are respectively grown in three directions of eight vertexes of the cubes, and the final product presents a shape of a nano-octa-tripodia.
Example 2
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) And stirring, mixing and dissolving 96 mu mol of zinc acetate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide and 200 mu L of seed dispersion liquid with 3mL of water at room temperature, keeping the temperature of the mixture at the room temperature for 3 hours, and washing the reaction liquid to obtain a ZIF-8 nano octatripodia product.
Example 3
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc sulfate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide and 200 mu L of seed dispersion with 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction solution to obtain the ZIF-8 nano octopodosome product.
Example 4
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 5
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 6
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyltrimethylammonium chloride and 200 mu L of seed dispersion with 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction solution to obtain a ZIF-8 nano octopodosome product.
Example 7
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of polyvinylpyrrolidone, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain a ZIF-8 nano octopodosome product.
Example 8
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) And stirring, mixing and dissolving 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide and 200 mu L of seed dispersion liquid with 3mL of methanol at room temperature, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 9
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide and 200 mu L of seed dispersion with 3ml of N-dimethylformamide at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction solution to obtain a ZIF-8 nano octopodosome product.
Example 10
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 2mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 11
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 4mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 12
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) 1 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water are stirred, mixed and dissolved at room temperature, the mixture is kept at the room temperature for 3 hours, and the reaction liquid is washed to obtain a ZIF-8 nano octatripodia product.
Example 13
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing and dissolving 200 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide and 200 mu L of seed dispersion with 3mL of water at room temperature, keeping the mixture at room temperature for 3 hours, and washing the reaction solution to obtain a ZIF-8 nano octatripodia product.
Example 14
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 0.10mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 15
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 3.00mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 16
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 0.01 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 17
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 4.00 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 18
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 100 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 19
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) And stirring, mixing and dissolving 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide and 500 mu L of seed dispersion liquid with 3mL of water at room temperature, keeping the temperature of the mixture at the room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 20
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 1 hour, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Example 21
A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the temperature of the mixture at room temperature for 12 hours, and washing the reaction liquid to obtain the ZIF-8 nano octatripodia product.
Comparative example 1
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) 0.1 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide, 200 mu L of seed dispersion liquid and 3mL of water are stirred, mixed and dissolved at room temperature, the mixture is kept at the room temperature for 3 hours, and the reaction liquid is washed to obtain a ZIF-8 nano octatripodia product.
Comparative example 2
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) Mixing 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 200 mu L of seed dispersion liquid and 3mL of water at room temperature, stirring, mixing and dissolving, keeping the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain a ZIF-8 nano octopodosome product.
Comparative example 3
(1) 1.37mmol of zinc acetate, 13.6mmol of 2-methylimidazole, 2.5. mu. mol of cetyltrimethylammonium bromide and 10mL of water were stirred, mixed and dissolved at room temperature, the mixture was kept at room temperature for 2 hours, the reaction solution was washed to obtain ZIF-8 truncated dodecahedral seeds, and the seeds were dispersed in 10mL of water to obtain a seed dispersion.
(2) And stirring, mixing and dissolving 96 mu mol of zinc nitrate, 1.32mmol of 2-methylimidazole, 1.44 mu mol of hexadecyl trimethyl ammonium bromide and 1mL of seed dispersion liquid with 3mL of water at room temperature, keeping the temperature of the mixture at room temperature for 3 hours, and washing the reaction liquid to obtain the ZIF-8 nano octopodosome product.
Claims (6)
1. A method for preparing a zeolite imidazole ester framework material ZIF-8 nano octapods by using seed growth synthesis comprises the following steps:
(1) mixing and dissolving zinc salt, imidazole ligand, surfactant and water at room temperature, keeping the temperature at room temperature for 1-4h, washing to obtain ZIF-8 truncated dodecahedral seeds, and dispersing into water to obtain seed dispersion liquid;
the molar ratio of the zinc salt to the imidazole ligand to the surfactant is (1-2): (12-15): (0.002-0.004), wherein the mass concentration of the seed dispersion liquid is 1-100 g/L;
(2) stirring, mixing and dissolving zinc salt, imidazole ligand, surfactant, seed dispersion liquid and solvent at room temperature, preserving heat at room temperature for 1-12h, and washing to obtain a ZIF-8 nano octopodosome product;
the molar ratio of the zinc salt, the imidazole ligand and the surfactant is (1-200): (100-3000): (0.01-4);
the volume ratio of the molar dosage of the imidazole ligand to the seed dispersion liquid is (0.1-3): (0.1-0.5) mol/L.
2. The method for preparing a zeolitic imidazolate framework material ZIF-8 nano-octapods according to claim 1, wherein said zinc salt in step (1) comprises one of zinc nitrate, zinc acetate, zinc sulfate, zinc chloride;
the imidazole ligand is 2-methylimidazole;
the surfactant comprises one of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride, polyvinylpyrrolidone, sodium polystyrene sulfonate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate.
3. The method for preparing the zeolitic imidazolate framework material ZIF-8 nano-octapods according to claim 1, wherein the volume ratio of the molar amount of imidazole ligands to water in step (1) is 13.6: (8-15) mol/L.
4. The method for preparing the zeolitic imidazolate framework material ZIF-8 nano-octapods according to claim 1, wherein the washing reagent used in step (1) is methanol, water or ethanol.
5. The method for preparing a zeolitic imidazolate framework material ZIF-8 nano-octapods according to claim 1, wherein said zinc salt in step (2) comprises one of zinc nitrate, zinc acetate, zinc sulfate, zinc chloride;
the imidazole ligand is 2-methylimidazole;
the surfactant comprises one of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride, polyvinylpyrrolidone, sodium polystyrene sulfonate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate;
the solvent is one of water, methanol and N, N-dimethylformamide.
6. The method for preparing the zeolitic imidazolate framework material ZIF-8 nano-octapods according to claim 1, characterized in that the volume ratio of the molar amount of imidazole ligands to solvent in step (2) is (0.1-3): (2-4) mol/L.
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