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Preparation method and application of dibenzothienyl lanthanide metal organic framework compound

A dibenzothienyl lanthanum and metal organic framework technology, which is applied in the direction of organic compound/hydride/coordination complex catalyst, organic chemistry, chemical instruments and methods, etc., can solve the difficulty of increasing process flow, unfavorable purification and separation, Catalysts are easy to deactivate and other problems, and achieve good industrialization prospects, easy separation and purification, and simple synthesis methods

Pending Publication Date: 2022-04-01
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cost of small organic molecules and macromolecular biological enzymes is slightly higher, and the catalyst is easily deactivated after catalysis. Although the cost of metal inorganic salts is low, they are easily soluble in various reaction systems, which is not conducive to purification and separation after the reaction. Increased difficulty in the process

Method used

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  • Preparation method and application of dibenzothienyl lanthanide metal organic framework compound
  • Preparation method and application of dibenzothienyl lanthanide metal organic framework compound
  • Preparation method and application of dibenzothienyl lanthanide metal organic framework compound

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Experimental program
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Effect test

Embodiment 1

[0029] Add Ligand H to 5 small empty vials respectively 2 sbdc (0.091g, 0.3mmol) and Tb (NO 3 ) 2 ·6H 2 O (0.091g, 0.2mmol), then add 5mL ethanol and 1mL deionized water to these 5 vials respectively, stir evenly, then place these 5 vials in an oven, burn at 140°C for 96h, close the oven, and cool At room temperature, colorless cubic crystals were produced, filtered, and dried to obtain the target material Tb-sbdc, about 380 mg was obtained from 5 vials, and the yield was about 60%. Molecular formula: C 42 h 24 o 21 S 3 Tb2. Elemental analysis (%) Found: C 37.31%, H 2.679%. The crystal structure diagram of the target material Tb-sbdc obtained, such as figure 1 As shown, the 3D structure schematic diagram, such as figure 2 As shown in the XRD diagram, such as image 3 As shown, the thermogravimetric analysis diagram, such as Figure 4 As shown, the catalytic cycle utilization diagram, such as Figure 11 shown.

Embodiment 2

[0031] Add Ligand H to 5 small empty vials respectively 2 sbdc (0.091g, 0.3mmol) and TbCl 3 ·6H 2O (0.075g, 0.2mmol), then add 5mL ethanol and 1mL deionized water to these 5 vials respectively, stir evenly, then place these 5 vials in an oven, burn at 140°C for 96h, close the oven, and cool At room temperature, colorless cubic crystals were produced, filtered and dried to obtain the target material Tb-sbdc, about 370 mg was obtained from 5 vials, and the yield was about 58%. Molecular formula: C 42 h 24 o 21 S 3 Tb 2 . Elemental analysis (%) Found: C 37.31%, H2.679%. The crystal structure diagram of the target material Tb-sbdc obtained, such as figure 1 As shown, the 3D structure schematic diagram, such as figure 2 As shown in the XRD diagram, such as image 3 As shown, the thermogravimetric analysis diagram, such as Figure 4 As shown, the catalytic cycle utilization diagram, such as Figure 11 shown.

Embodiment 3

[0033] 10 mg Tb-sbdc was weighed and soaked in a solution of 2',7'-dichlorofluorescein in dichloromethane for 24 hours, then the product was filtered and washed with 10 mL of dichloromethane to obtain a solid. Then the solid is dissolved with 100 microliters of concentrated hydrochloric acid, and this solution is constant volume in a 50mL volumetric flask with methanol, and the dye adsorption ultraviolet curve of the prepared solution is measured, as shown in Figure 5 shown. Comparing the UV absorption standard curve of fluorescein, the mass ratio of Tb-sbdc to fluorescein was calculated to be 6.3%.

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Abstract

The invention belongs to the technical field of catalytic materials, and relates to a preparation method and application of a dibenzothienyl lanthanide metal organic framework compound, and the preparation method comprises the following steps: taking dibenzo [b, d] thiophene-2, 8-dicarboxylic acid-5, 5-dioxide H2sbdc in a dibenzothiophene derivative as a linking ligand, and carrying out one-step reaction to obtain the dibenzothienyl lanthanide metal organic framework compound. And preparing the dibenzothienyl lanthanide metal organic framework compound Tb-sbdc with a pore channel structure by taking Tb < 3 + > in lanthanide metal salt as a node through a hydrothermal synthesis method. According to the present invention, the catalyst synthesis method is simple, the practical operation is simple, the catalyst and the raw materials for the catalytic reaction are low in price, the reaction yield is high, and the obtained functional material has characteristics of thermal stability and chemical stability, easy large-area promotion and application, adaptation to the requirements of large-scale industrial production, and good industrial prospect.

Description

technical field [0001] The invention relates to a preparation method and application of a dibenzothienyl lanthanide metal organic framework compound, belonging to the technical field of catalytic materials. Background technique [0002] With the advancement of science and technology and the rapid development of human society, the cyanidation reaction has gradually become an important organic chemical reaction in chemical production, among which the common industrial products aromatic aldehydes and cyanides are the least toxic trimethyl cyanide The silane cyanation reaction of silane has attracted extensive attention from major chemical production plants in recent years. The special intermediate cyanohydrin produced by the silicocyanation reaction has a wide range of applications in medical treatment, materials, pesticides, and chemicals. This intermediate can quickly and easily prepare some important compounds in the fields of natural products and biomedicine through simple...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/22C07F7/18
Inventor 何成刘屿芊赵沛然段春迎
Owner DALIAN UNIV OF TECH
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