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Method for preparing rare earth-organoboron framework compound

A framework compound and organoboron technology, which is applied in the field of preparation of rare earth-organoboron framework compounds, can solve the problems of improved hydrothermal stability, low activity and reaction efficiency, etc.

Inactive Publication Date: 2013-11-06
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reported rare earth MOF materials usually have low activity and reaction efficiency. The thermal stability of the known rare earth MOFs in air can reach nearly 400 °C, but their hydrothermal stability still needs to be improved.

Method used

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  • Method for preparing rare earth-organoboron framework compound
  • Method for preparing rare earth-organoboron framework compound
  • Method for preparing rare earth-organoboron framework compound

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029]

[0030]1,2,4,5-Tetramethylbenzene (10g, 74.6mmol) and iodine (0.394g, 1.56mmol) were dissolved in 380ml of dry dichloromethane, and slowly poured into the light-proof reactor under nitrogen protection. Slowly add 40 ml of dichloromethane solution dissolved in bromine (9 ml, 175.6 mmol) dropwise (not less than 30 minutes), and reflux for 1 hour after the dropwise addition is completed. Return to room temperature after the reaction, add 20 ml of 5M sodium hydroxide solution to quench, separate the layers, wash the organic phase several times with water, and dry with anhydrous magnesium sulfate. After drying, the desiccant was filtered off, spin-dried to obtain a white solid, and then recrystallized with dichloromethane to obtain the white needle-shaped target product 1,4-dibromo-2,3,5,6-tetramethylbenzene 16.76g (yield : 77%).

[0031]

[0032] Under the protection of nitrogen, 1,4-dibromo-2,3,5,6-tetramethylbenzene (10g, 34.3mmol) was dissolved in 300ml of dry et...

Embodiment 2

[0038] Weigh 0.01mmolLa(NO 3 ) 3 ·6H 2 O, 0.005 mmol Ligand H 3 L 3 and 0.005mmolK 2 CO 3 In a 10mL sample bottle, add N,N'-dimethylformamide (0.5mL), tetrahydrofuran (1mL) and ethanol (0.5mL), and after fully dissolved, tighten the bottle cap and heat in an oven at 80°C. After 2 days, the sample bottle was taken out, and the reaction solution was filtered off after cooling to room temperature, and the obtained colorless crystals were washed several times with ether and then dried in the air to obtain compound b, whose structural formula was

[0039] [Me 2 NH 2 ][La 4 (CO 3 )(L 3 ) 4 (DMF) 4 (H 2 O) 2 ]·2H 2 O.

Embodiment 3

[0041] Weigh 0.005mmol of compound a into a dry 10mL Schlenk bottle, add dry dichloromethane 1mL, reaction substrate aldehyde / ketone 1mmol and trimethylsilyl cyanide 2mmol under the protection of nitrogen, react at room temperature for 12-48h and pass nuclear magnetic resonance Hydrogen spectrum calibration yield. The reaction substrate aldehyde / ketone is one of benzaldehyde, 1-naphthaldehyde, 2-naphthaldehyde, p-methoxybenzaldehyde, quaterphenylformaldehyde, acetophenone, and quaterracetophenone.

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Abstract

The invention relates to a method for preparing a rare earth-organoboron framework compound which belongs to the chemical technical field. The chemical formula of the compound is [Me2NH2][Ln4(CO3)L4(DMF)n(H2O)2].2H20, wherein: L is tri-(4-carboxyl-2,3,5,6-tetramethyl benzene)borane anion, Ln is Nd or La, the corresponding n is 2 or 4. The method of the invention uses a neodymium-organoboron framework material with strong thermostability and hydrothermal stability as well as nonsaturated metal active site which are the characteristics of an excellent out-phase Lewis acid catalyst to effectively catalyze silicon cyanation addition of aldehyde / ketone and ring-opening reaction of epoxides.

Description

technical field [0001] The invention relates to a method in the technical field of chemical engineering, in particular to a method for preparing a highly stable rare earth-organoboron framework compound. Background technique [0002] Rational selection of metal ions and organic ligands can achieve excellent control of the composition and structure of metal-organic frameworks (MOFs), which provides an effective way to prepare porous hybrid materials, and also endows porous materials with broad application prospects. Compared with structures such as zeolites, the relatively low hydrothermal and chemical stability of MOFs materials is still an unsolved problem, which largely limits their large-scale industrial applications. Recently, some MOFs based on imidazole groups with good thermal and hydrothermal stability have been obtained by using strong metal-nitrogen (heterocyclic) bonds or by introducing polynuclear clusters formed by Al / Cr and carboxylic acids. MIL-n type MOFs. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00B01J31/22C07F7/18C07C213/04C07C215/44C07C215/08C07C215/30
Inventor 董倩刘燕崔勇
Owner SHANGHAI JIAOTONG UNIV