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Imide bond grafted NHPI catalyst, preparation method and application thereof

The technology of imide and catalyst is applied in the field of NHPI catalyst grafted by imide bond and its preparation field, which can solve the problems of loss of NHPI active components, influence on catalytic effect, cleavage of graft bond, etc., and achieve recyclable The effect of utilization, good catalytic effect and high active site density

Active Publication Date: 2020-10-20
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, under the reaction conditions, because in the immobilized catalyst using amide or ester bond, the amide bond or ester bond is easily hydrolyzed in the presence of acid, so the stability of the existing immobilized NHPI catalyst is low. During the use process, the graft bond will be broken, which will cause the loss of NHPI active components and affect its catalytic effect.

Method used

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  • Imide bond grafted NHPI catalyst, preparation method and application thereof
  • Imide bond grafted NHPI catalyst, preparation method and application thereof
  • Imide bond grafted NHPI catalyst, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The synthesis route of this embodiment is as follows figure 1 Shown:

[0042] (1) Use γ-aminopropyltriethoxysilane APTES to modify SiO 2 : Add 2g SiO2 to a 250mL single-necked round bottom flask 2 , 10g γ-aminopropyltriethoxysilane APTES and 100mL tetrahydrofuran THF, move the flask into an oil bath, set up a reflux device, stir, heat the oil bath to 70°C and keep a constant temperature, stop heating and stirring after 24 hours of reaction and reflux, When the temperature dropped to room temperature, remove the reflux device, filter the reaction solution, wash the filter cake once with 60mL THF, and wash twice with 60mL absolute ethanol, and put the obtained white solid powder in an oven at 70°C for 24 hours to prepare SiO 2 -APTES.

[0043] (2) Using pyromellitic dianhydride and SiO 2 -Imidation reaction of primary amines on APTES support to prepare SiO 2 -APTES-PDMA: Take 1g pyromellitic dianhydride PDMA, 1g SiO prepared in the first step 2 -APTES and 100mL of a...

Embodiment 2

[0050] (1) Use γ-aminopropyltriethoxysilane APTES to modify SiO 2 : Add 2g SiO2 to a 250mL single-necked round bottom flask 2, 6g of γ-aminopropyltriethoxysilane APTES and 100mL of tetrahydrofuran THF, move the flask into an oil bath, set up a reflux device, stir, heat the oil bath to 80°C and keep it at a constant temperature, react and reflux for 48 hours, stop heating and stirring, When the temperature dropped to room temperature, remove the reflux device, filter the reaction solution, wash the filter cake once with 60mL THF, and wash twice with 60mL absolute ethanol, and put the obtained white solid powder in an oven at 70°C for 24 hours to prepare SiO 2 -APTES.

[0051] (2) Using 3,3',4,4'-biphenyltetracarboxylic dianhydride BDP and SiO 2 -Imidation reaction of primary amines on APTES support to prepare SiO 2 -APTES-BDP: Take 1g 3,3',4,4'-biphenyltetracarboxylic dianhydride BDP, 2g SiO prepared in the first step 2 -APTES and 100mL of dimethylacetamide DMAC were placed...

Embodiment 3

[0056] The difference between this embodiment and embodiment 2 is that in step 2, 1,4,5,8-naphthalene tetracarboxylic dianhydride NTDA and SiO 2 -Imidation reaction of primary amines on APTES support to prepare SiO 2 -APTES-NTDA, the amount of 1,4,5,8-naphthalene tetracarboxylic dianhydride NTDA used is 1g, and the product in step 3 is SiO 2 -APTES-NTDA–NOH with a grafted N-hydroxyphthalimide concentration of 0.75 mmol / g.

[0057] From Figure 6 It can be seen that NTDA and SiO 2 The asymmetric stretching vibration absorption peak of anhydride in +NTDA appears at 1774cm -1 Sample SiO after grafting reaction 2 -APTES-NTDA and SiO 2 -APTES-NTDA-NOH at 1774cm -1 Absorption peak disappears at 1666, 1712cm -1 Symmetrical and asymmetrical stretching vibration absorption peaks of imide group carbonyl appeared, 1345cm -1 The stretching vibration absorption peak of O=C-N-C=O on the imide ring appeared, indicating that NTDA and SiO 2 -APTES grafting was successful.

[0058] Fr...

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Abstract

The invention discloses an NHPI catalyst grafted by utilizing imide bonds, a preparation method and application thereof. The catalyst comprises a SiO2 carrier and N-hydroxyphthalimide grafted on the SiO2 carrier, wherein the N-hydroxyphthalimide is grafted on the SiO2 carrier through imide bonds. The preparation method of the catalyst comprises the following steps: (1) modifying the surface of a carrier SiO2 by using aminopropyltriethoxysilane to obtain a surface ammoniation carrier SiO2-APTES; (2) dissolving cyclized dianhydride and the surface ammoniation carrier SiO2-APTES in a solvent, andgrafting through imide covalent bonds to prepare grafted anhydride; and (3) carrying out imidization treatment on the grafted anhydride to prepare the grafted NHPI catalyst, wherein the catalyst canbe used as a recyclable catalyst to be applied to preparation of acetophenone. The catalyst has the advantages of no loss of active components in the catalytic reaction, good stability, high active site density and good catalytic effect, and realizes the cyclic utilization of the catalyst.

Description

technical field [0001] The invention relates to an NHPI catalyst and its preparation method and application, more specifically, to an NHPI catalyst grafted with imide bonds, its preparation method and application. Background technique [0002] Acetophenone is an important intermediate in the fields of manufacturing perfumes, soaps, resins and medicines. In industry, Friedel-Crafts (Friedel-Crafts) acylation of benzene is generally used to prepare acetophenone, but the reaction conditions of this process are relatively harsh. , the yield of acetophenone is low. With the increasing demand for acetophenone, the development of an economical and environmentally friendly production process for acetophenone has attracted widespread attention from academia and industry. At present, 1-phenylethanol oxidation method, styrene oxidation method and ethylbenzene oxidation method have been studied to synthesize acetophenone. The production of acetophenone with relatively cheap ethylbenze...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C49/78C07C45/28
CPCB01J31/0274B01J31/0275C07C45/28B01J2231/70C07C49/78Y02P20/584
Inventor 石国军徐思浩路秋婷冯亚梁雨欣
Owner YANGZHOU UNIV
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