MAF-stu-13 material having ultra-microporous dia-a network topology as well as synthesis and application of MAF-stu-13 material

A technology of maf-stu-13 and network topology, applied in other chemical processes, ion exchange, organic chemistry, etc., can solve the problems of high cost, high energy consumption, complex process, etc., and achieve mild conditions, rapid mass synthesis, The effect of simple process

Active Publication Date: 2020-12-18
SHANTOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the chemical industry, the commonly used extractive distillation method has disadvantages such as high cost, complicated process, and large energy consumption, so it is not suitable for the separation of Bz and CH
In the past few decades, CH was mainly prepared by hydrogenation of Bz under catalyst conditions, but unreacted Bz still exists in the product, making it difficult to meet the demand for high-purity Bz / CH separation.

Method used

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  • MAF-stu-13 material having ultra-microporous dia-a network topology as well as synthesis and application of MAF-stu-13 material
  • MAF-stu-13 material having ultra-microporous dia-a network topology as well as synthesis and application of MAF-stu-13 material
  • MAF-stu-13 material having ultra-microporous dia-a network topology as well as synthesis and application of MAF-stu-13 material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] The synthesis route of the synthesis of MAF-stu-13 in this embodiment is as follows:

[0064] 1. Solvothermal synthesis of MAF-stu-13:

[0065] A certain proportion of metal zinc salt: 0.1mmol, ligand H 2 L: 0.1mmol, DMF: 2mL, H 2 O: 1mL was placed in a 10mL hard glass tube, and the glass tube mouth was sealed with a water welder (oxygen hydrogen machine), and ultrasonically treated for 30min. Shake well and put it into a stainless steel box, heat it in an oven to 120°C and keep it at a constant temperature for 48 hours, then cool it down to room temperature at a rate of 5°C / h, open the tube and filter it, wash it twice with methanol, and filter it at room temperature. After natural drying, a large number of colorless needle-like crystals were obtained with a yield of about 76% (based on the ligand). After vacuum activation at 160°C for 12h, the MAF-stu-13 material with dia-a network topology was obtained.

[0066] 2. Rapid mass synthesis of MAF-stu-13:

[0067] We...

Embodiment 2

[0070] Analysis of crystallographic data of MAF-stu-13 material

[0071] MAF-stu-13 material with ultramicroporous dia-a network topology, chemical formula {[Zn(MIBA) 2 ]} n , n is a non-zero natural number. MAF-stu-13 belongs to the tetragonal crystal system, P4nc space group, each asymmetric unit contains a crystallographically independent Zn(II) metal center, its occupancy rate is 1, and the coordination environment is as follows figure 1 shown. Zn(II) metal center adopts tetrahedral four-coordination mode The symmetry codes are: a-x-3 / 2, y+1 / 2, z+1 / 2; b x+1 / 2, -y-1 / 2, z+1 / 2; c-x-1, -y ,z. The Zn(II) metal center coordinates with the imidazole N and the carboxyl O in two independent ligands respectively, and one carboxyl O of the ligand does not participate in the coordination and is exposed in the channel (such as figure 2 shown). MAF-stu-13 is a quadruple interspersed structure (such as Figure 4 As shown), there is a one-dimensional channel in the c-axis dire...

Embodiment 3

[0077] Characterization of thermal stability and chemical stability of MAF-stu-13 material.

[0078] A certain quality of MAF-stu-13 crystal was weighed, and thermal stability, water stability, pH stability and organic solvent stability were tested respectively. The PXRD spectrum showed that MAF-stu-13 had excellent thermal stability and chemical stability.

[0079] In the TGA curve (such as Figure 7 shown), the weight loss platform of MAF-stu-13 before 80°C indicated that the guest molecules in the framework were lost and remained stable at 350°C, and then when the temperature continued to rise to 800°C, the weight loss reached 65%, and the MAF-stu-13 framework was completely Decomposition, the residue is ZnO. By variable temperature PXRD spectrum (such as Figure 8 (shown) shows that MAF-stu-13 crystals can remain stable below 350 °C. In addition, MAF-stu-13 can be maintained in aqueous solution for one month and heated in a boiling water bath for 7 days, and its struct...

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Abstract

The present invention relates to a MAF-stu-13 material having an ultra-microporous dia-a network topology, the chemical formula is {[Zn (MIBA) 2]} n, n is a non-zero natural number, and MIBA is 4-(2-methylimidazole) benzoxy; the material belongs to a tetragonal crystal system and a P4nc space group, has a one-dimensional pore channel in the c-axis direction, and has excellent thermal stability andchemical stability. The MAF-stu-13 can be rapidly synthesized in a large scale, a solution that a general MOFs material is difficult to synthesize in a large scale is provided, and the material synthesis process comprises the steps that metal zinc salt, ligand HMIBA and a DMF solvent are placed in a pressure-resistant bottle in a certain proportion and sealed, and heating and stirring are conducted for 1 h at the temperature of 120 DEG C through a solvothermal reaction. The MAF-stu-13 material with the ultra-micropore dia-a network topological structure can specifically adsorb Bz in a Bz andCH mixed solution, the Bz is eluted from a frame, the purity of the Bz is up to 99.4%, and therefore liquid-phase adsorption separation of Bz/CH is achieved. While the MAF-stu-13 is able to extract anamount of Bz from commercially pure CH. The MAFstu13 is capable of specifically adsorbing Bz and is based on a synergistic effect of size exclusion and supramolecular binding.

Description

technical field [0001] The invention relates to the field of metal-organic frameworks, in particular to a MAF-stu-13 metal-organic framework material with an ultramicroporous dia-a network topology and its use in a mixed solution of benzene (Bz) and cyclohexane (CH) Bz is specifically adsorbed, thereby realizing the liquid phase adsorption separation of Bz / CH. Background technique [0002] In recent years, with the continuous expansion of global demand for petrochemical raw materials, energy crisis and environmental pollution have gradually become major problems that need to be solved urgently at home and abroad. Among them, the cyclic hydrocarbon compound (C 6 ) is of great significance in the petrochemical field, and their separation is known as one of the "seven chemical separations that changed the world". As we all know, although benzene (Bz) is one of the important petrochemical raw materials, it is a recognized volatile organic compound. In contrast, cyclohexane (C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01D15/08C07C7/12C07C13/18C07C15/04
CPCB01J20/226B01D15/08C07C7/12C07C2601/14C07C13/18C07C15/04
Inventor 黄晓春叶春荣王文健李冕
Owner SHANTOU UNIV
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