Method for preparing TEMPO free radical functionalized hollow conjugated microporous polymer based on SiO2 template and application

A conjugated microporous, functionalized technology, applied in chemical instruments and methods, catalyst activation/preparation, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as limiting the diffusion rate of substrates and products, Achieve the effects of simple preparation, large contact area and improved catalytic efficiency

Pending Publication Date: 2021-01-01
GUIZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, conventional CMPs are usually micron or even millimeter-sized spherical or massive solid powders, which limit the diffusion rate of substrates and products in catalytic reactions.

Method used

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  • Method for preparing TEMPO free radical functionalized hollow conjugated microporous polymer based on SiO2 template and application
  • Method for preparing TEMPO free radical functionalized hollow conjugated microporous polymer based on SiO2 template and application
  • Method for preparing TEMPO free radical functionalized hollow conjugated microporous polymer based on SiO2 template and application

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preparation example Construction

[0039] The present invention is based on SiO 2 Nano microsphere is the preparation method of functionalized hollow conjugated microporous polymer of template, comprises the following steps:

[0040] (a) Pd catalyst with cuprous iodide (CuI) and SiO 2 The nano-microspheres were added into the organic solvent, and stirred vigorously for 1 h under a nitrogen-protected room temperature environment to make the SiO 2 Nano-microspheres are fully dispersed in the solvent;

[0041] (b) Add acetylenic monomers and functionalized monomers into the reaction system of step (a), raise the reaction temperature from room temperature to 100° C., reduce the stirring speed to 100 rpm, and react for 48 hours. Use chloroform, methanol, acetone to wash the product successively after the reaction and collect by centrifugation;

[0042] (c) coating the porous material obtained in step (b) with SiO 2 After drying, the functionalized conjugated microporous polymer material (SiO2@CMP-4-TEMPO) of the...

Embodiment 1

[0046] The present embodiment provides a kind of preparation method of H-CMP-4-TEMPO nanometer catalyst, and technique is as follows figure 1 shown, including the following steps:

[0047] (a) SiO 2 Nanospheres (500mg) and catalyst Pd (PPh 3 ) 2 Cl 2 (8.4mg) and CuI (2.3mg) were added to a round bottom flask, triethylamine (15mL) and toluene (15mL) were added under nitrogen atmosphere. After the solid was dispersed by sonication, it was stirred vigorously at room temperature for 1 h.

[0048] (b) Add tetrakis(4-ethynylbenzenemethane 0.12mmol, 50mg) and 2,5-dibromo-TEMPO (0.24mmol, 103.4mg) to the reaction system of step (a), charge into nitrogen protection, react The temperature was raised from room temperature to 100°C, and the stirring speed was reduced to 100rpm, and the reaction was carried out for 48h.

[0049] (c) The product obtained in step (b) was cleaned with chloroform, methanol, and acetone ultrasonically, and the product was collected by centrifugation, and ...

Embodiment 2

[0056] The present embodiment provides a kind of preparation method of H-CMP-2-TEMPO nano-catalyst, it comprises the following steps:

[0057] (a) SiO 2 Nanospheres (500mg) and catalyst Pd (PPh 3 ) 2 Cl 2 (8.4mg) and CuI (2.3mg) were added to a round bottom flask, triethylamine (15mL) and toluene (15mL) were added under nitrogen atmosphere. After the solid was dispersed by sonication, it was stirred vigorously at room temperature for 1 h.

[0058] (b) Add 1,4-diethynylbenzene (0.24mmol, 30mg) and 2,5-dibromo-TEMPO (0.24mmol, 103.4mg) to the reaction system of step (a), fill with nitrogen protection, the The reaction temperature was raised from room temperature to 100° C., and the stirring speed was reduced to 100 rpm, and the reaction was performed for 48 hours.

[0059] (c) The product obtained in the step (b) is ultrasonically cleaned with chloroform, methanol, and acetone respectively, collected by centrifugation to obtain the product, and dried at low temperature.

...

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Abstract

The invention discloses a method for preparing a TEMPO free radical functionalized hollow conjugated microporous polymer based on a SiO2 template and application. The method comprises the following steps: adding a palladium catalyst, cuprous iodide and SiO2 nano microspheres into an organic solvent, and stirring for 0.5 hour to 1.5 hours in a nitrogen protection environment to obtain a mixed solution; adding an aromatic alkyne monomer and a TEMPO free radical functionalized monomer into a mixed solution, heating to 90 DEG C and 110 DEG C, and reacting for 24 hours to 50 hours to obtain a functionalized conjugated microporous polymer material (SiO2@CMPs-TEMPO) with SiO2 coated with a TEMPO free radical functionalized porous material; drying SiO2@CMPs-TEMPO, adding the dried SiO2@CMPs-TEMPOinto a hydrofluoric acid aqueous solution, stirring for 2 hours to 4 hours, etching SiO2, cleaning, and centrifuging to obtain the TEMPO free radical functionalized hollow conjugated microporous polymer material (HCMPs-TEMPO). The TEMPO free radical functionalized hollow conjugated microporous polymer material provided by the invention can efficiently catalyze the oxidation of alcohol organic matters.

Description

technical field [0001] The invention relates to a SiO-based 2 The functionalized hollow conjugated microporous polymer nano catalyst prepared by template belongs to the technical field of nano catalyst. Background technique [0002] The catalytic oxidation reaction of alcohol plays an important role in chemical production. The catalysts used in the catalytic oxidation reaction of alcohol in chemical production, such as manganese oxide, chromium oxide, hypervalent iodine and other oxidants, may be accompanied by pollution containing heavy metal elements during use. substances, and easily peroxidize alcohols. Based on the current necessity and urgency of environmental protection, in chemical experiments and production, how to find more environmentally friendly and efficient environment-friendly catalysts has become a research focus. [0003] Conjugated microporous polymers (CMPs) are a class of organic porous materials with microporous structure, high specific surface area, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/02B01J31/06B01J35/10B01J37/00B82Y30/00B82Y40/00
CPCC08G61/02B01J31/063B01J31/06B01J35/023B01J35/10B01J37/0018B82Y30/00B82Y40/00C08G2261/1432C08G2261/124C08G2261/132C08G2261/312C08G2261/3328C08G2261/352C08G2261/413B01J2231/70
Inventor 庄金亮申妍铭
Owner GUIZHOU NORMAL UNIVERSITY
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