Nitrogen-containing tridentate ligand organic microporous polymer material as well as preparation and application thereof

A porous polymer and organic technology, applied in the preparation of organic compounds, carbon-based compounds, organic compound/hydride/coordination complex catalysts, etc.

Active Publication Date: 2014-12-17
SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, triptycene-based organic porous polymers with multidentat

Method used

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  • Nitrogen-containing tridentate ligand organic microporous polymer material as well as preparation and application thereof
  • Nitrogen-containing tridentate ligand organic microporous polymer material as well as preparation and application thereof
  • Nitrogen-containing tridentate ligand organic microporous polymer material as well as preparation and application thereof

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Experimental program
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Example Embodiment

[0080] A more preferred preparation method is as follows:

[0081] Step 1) In an inert solvent, add hexaaminotriptycene hydrochloride (HATH), and cool the reaction to below 0°C and stir under the protection of nitrogen.

[0082] Step 2) Prepare an inert solvent solution of 2,6-diformylpyridine (DFPY) and remove oxygen by bubbling.

[0083] Step 3) Slowly add the solution prepared in step 2 dropwise to the reaction system in step 1. After the addition process is completed, keep the reaction temperature constant for several hours. Then the temperature of the reaction system was gradually raised to room temperature.

[0084] Step 4) Blow air into the reaction system that has been raised to room temperature. Then the reaction system was transferred to a sealed tube and sealed, and the reaction was gradually raised.

[0085] Step 5) The reaction system in step 4 was cooled to room temperature to obtain a yellow fluffy precipitate. After filtering, the filter cake is washed, soaked, and va...

Example Embodiment

[0119] Example 1 Synthesis of organic microporous polymer

[0120] The reaction formula is as figure 1 As shown, a 100 mL round bottom flask was charged with 2,3,6.7,14,15-hexaaminotriptycene hydrochloride (HATH) (90 mg, 0.16 mmol) and 30 mL DMF. System in N 2 Stir at -30°C for 10 min in the atmosphere, and then slowly add dropwise a DMF solution (32.4 mg, 0.24 mmol, 20 mL DMF) of 2,6-diformylpyridine (DFPY) bubbling to remove oxygen. The reaction system was stirred at -30°C for 6 hours and then gradually warmed to room temperature. During the stirring process, yellow-brown precipitation can be observed. Before heating, air was blown into the reaction system for 30 minutes and transferred to a 100 mL sealed tube. The sealed reaction system was heated at 140°C for 72 hours to obtain a fluffy yellow precipitate. Filtration, the yellow precipitate obtained is sequentially used DMF, acetone, H 2 O, 0.5M HCl, 0.5M NaOH, H 2 O and acetone washing, then in acetone / CH 2 Cl 2 (1:1v:v) ...

Example Embodiment

[0124] Example 2 Catalyst loading process

[0125] Add Pd(OAc) to 25mL round bottom flask 2 (40mg) and 10mL CH 2 Cl 2 , Stir until all the solids are dissolved, and then add POP-bbp (110mg). The reaction system was heated at 60°C for 24 hours, and the filtered solid was leached with acetone in a Soxhlet extractor for 12 hours. Vacuum drying at 100℃ overnight to obtain the supported catalyst Pd(OAc) 2 POP-bbp (102mg). Elemental analysis: theoretical value, C (47.7%), H (3.80%), N (12.46%); experimental value, C (48.58%), H (3.77%), N (13.60%). ICP-AES analysis: Pd content, 5.89wt%.

[0126] image 3 , Figure 4 , Figure 5 For POP-bbp and Pd(OAc) 2 The infrared spectrum comparison chart of POP-bbp, the raw material and the model molecule, it can be seen that there are 2,6-bis(2-benzimidazolyl)pyridine (bbp) basic unit and triptycene skeleton in the product, indicating that the product is The formation of 2,6-bis (2-benzimidazolyl) pyridine (bbp) basic unit, while maintaining the ...

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Abstract

The invention provides a nitrogen-containing tridentate ligand organic microporous polymer material as well as preparation and an application thereof and particularly provides an organic porous polymer which has a triptycene structural unit and a 2, 6-di(2-benzimidazolyl) structural unit. The triptycene structural unit and the 2, 6-di(2-benzimidazolyl) structural unit have the arrangement mode shown in a formula I. The organic porous polymer provided by the invention is a good adsorbing material and catalyst-loading material and has a good application prospect in metal catalyst loading, particularly noble metal loading.

Description

technical field [0001] The invention belongs to the field of functional materials, and in particular relates to the preparation and application of a nitrogen-containing tridentate ligand organic microporous polymer material. Background technique [0002] Organic porous materials have received extensive attention due to their high specific surface area, low density, high physical and chemical stability, and structural modification. The current research directions are mainly concentrated in the fields of adsorption and separation, heterogeneous catalysis, gas storage, optoelectronics, and semiconductors. Traditional porous materials include inorganic crystal structure materials (such as zeolites) and amorphous network structures (such as silica, activated carbon). In recent years, the research on organic porous materials has made new developments, and some organic porous materials with different structural properties have emerged, such as Metal-Organic Frameworks (Metal-Organ...

Claims

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Application Information

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IPC IPC(8): C08G61/12B01J32/00B01J31/22C07C205/06C07C201/12C07C39/15C07C37/18C07C1/32C07C15/14C07C15/24C07C43/205C07C41/30C07C49/784C07C45/68
Inventor 赵新文强
Owner SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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