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A kind of solvent-free synthesis method of metal polyazole framework material

A framework material and synthesis method technology, applied in the direction of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problems of high cost, difficulty in activation, low reaction yield, etc., and achieve production efficiency High, high product yield, high purity effect

Inactive Publication Date: 2011-12-21
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to provide a green and environment-friendly solvent-free preparation of metal polyazoles based on the problems of high cost, low reaction yield, difficulty in activation, especially solvents and by-products in the synthesis process of existing metal polyazole framework materials. Method for polyazole framework materials
Heating can choose direct heating or microwave heating

Method used

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  • A kind of solvent-free synthesis method of metal polyazole framework material
  • A kind of solvent-free synthesis method of metal polyazole framework material
  • A kind of solvent-free synthesis method of metal polyazole framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] High-temperature and high-efficiency preparation of Example 1 MAF-4 (that is, SOD type 2-methylimidazolium zinc)

[0034] After grinding ZnO (200 mg, 2.5 mmol) and Hmim (410 mg, 5.0 mmol) uniformly, they were placed in a 15 mL reaction kettle with a polytetrafluoroethylene substrate, nitrogen was blown for 5 minutes, and the mixture was sealed and heated to 180 °C and kept After 12 hours, a white powder product was obtained with a yield of about 100%. The X-ray diffraction pattern of the obtained MAF-4 and the comparison result of the diffraction pattern of its single crystal simulation are shown in figure 1 .

Embodiment 2

[0035] Example 2 High-temperature and efficient direct molding preparation of MAF-4

[0036] After grinding ZnO (2.44 g, 30 mmol) and Hmim (4.93 g, 60 mmol) evenly, they were naturally filled in a 15 mL reaction vessel with a polytetrafluoroethylene substrate, heated to 180 °C and kept for 12 hours in an airtight manner to obtain White molded product, the yield is about 100%. The X-ray diffraction pattern of the obtained MAF-4 and the comparison result of the diffraction pattern of its single crystal simulation are shown in figure 2 . Product photo see image 3 , the scanning electron microscope results see Figure 4 .

Embodiment 3

[0037] Example 3 High-temperature and efficient preparation of MAF-27 (i.e. nbo type 3-(3-methyl-2-pyridine)-5-(4-pyridine)-1,2,4-triazole magnesium)

[0038] in Mg(OH) 2 (15 mg, 0.25 mmol) was added to Hmdpt (119 mg, 0.50 mmol), after grinding evenly, it was placed in a 10 mL glass tube, nitrogen gas was passed for 5 minutes, sealed and heated to 300 ° C and kept for 16 hours to obtain a white powder, The yield is about 100%. The X-ray diffraction pattern of the obtained MAF-27 and the comparison result of the diffraction pattern of its single crystal simulation are shown in Figure 5 . Product scanning electron microscope results see Figure 6 .

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Abstract

The invention discloses a solventless synthesis method for a metal polynitrogen azole framework material and belongs to the preparation field of porous coordination polymers. The synthesis method of the invention mainly comprises the following steps: uniformly mixing a polynitrogen azole ligand and a metal oxide or metal hydroxide in a stoichiometric ratio of the target metal polynitrogen azole framework material, heating, and reacting to obtain the required metal polynitrogen azole framework material. In the synthesis method, the need of adding solvent and other additives are avoided, the process steps are simplified, the product yield is very high, the reaction byproduct or waste liquid treatment problem is eliminated, and vapor is the only byproduct and does not affect subsequent reactions; the purity of the obtained metal polynitrogen azole framework material is high, the crystallizing property is excellent, the crystalform is controllable and the specific surface area is very high; and the metal polynitrogen azole framework material can be used for absorption storage, separation and the like. The synthesis method has no requirement on the size of the reactor and can be used in production at various scales.

Description

technical field [0001] The invention relates to the field of preparation of porous coordination polymers, in particular to a solvent-free synthesis method for preparing metal polyazole framework materials based on metal oxides / hydroxides as raw materials and without solvents. Background technique [0002] Porous coordination polymer is a new type of material composed of metal ions and organic ligands, which has broad potential application prospects. Although the assembly of porous coordination polymers is somewhat predictable, subtle differences in reaction conditions can still have a dramatic impact on their product structure, yield, and performance. Therefore, methods for efficiently synthesizing specific porous coordination polymers have been widely concerned by researchers. At present, porous coordination polymers are generally prepared based on solution reactions, including solvothermal (water or organic solvent) (relevant foreign patents include US 5648508, US 5648508...

Claims

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Application Information

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IPC IPC(8): C07F3/06C07F3/02B01J20/22B01J20/28
Inventor 张杰鹏林健斌林锐标洪惠玲陈小明
Owner SUN YAT SEN UNIV
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