Composite acid solid catalyst PVP-HNTs@UiO-66-SO3H and preparation method thereof

An acidic solid, catalyst technology, used in catalyst activation/preparation, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc. Insufficient performance and other problems, to achieve the effect of low cost, simple preparation process and simple preparation process

Inactive Publication Date: 2018-04-24
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] Aiming at the problems of insufficient performance of existing catalysts and low yield of HMF, the present invention provides a composite acidic solid catalyst PVP-HNTs@UiO-66-SO 3 H and its preparation method, by using polyvinylpyrrolidone (PVP) modified mesoporous material halloysite (HNTs) as a carrier, one-step synthesis of porous composite acidic solid catalyst PVP-HNTs@UiO-66-SO by solvothermal method 3 H, and adjust the acidity of the catalyst by changing the amount of loaded acidic MOF
The preparation process of this method is simple, no modifier is needed, and the porous structure of the prepared catalyst solves the problem of a single pore structure of the catalyst; the one-step synthesis of a composite acidic solid catalyst effectively solves the problem of a decrease in the thermal stability of the catalyst caused by subsequent sulfonation treatment , while effectively increasing the conversion rate of fructose to HMF

Method used

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  • Composite acid solid catalyst PVP-HNTs@UiO-66-SO3H and preparation method thereof
  • Composite acid solid catalyst PVP-HNTs@UiO-66-SO3H and preparation method thereof
  • Composite acid solid catalyst PVP-HNTs@UiO-66-SO3H and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0030] 1. PVP-HNTs@UiO-66-SO 3 The preparation method of H is characterized in that it is carried out according to the following steps:

[0031] (1) 0.1g HNTs was dispersed in 1g / mL 50mL PVP aqueous solution, and then ultrasonically dispersed to form a mixed system. The reaction system was reacted at 30° C. for 12 h under magnetic stirring. After the reaction, the obtained product was washed with deionized water, collected by centrifugation, and dried in vacuum to obtain modified PVP-HNTs.

[0032] (2) 0.025g of PVP-HNTs, 0.04g of zirconium chloride and 0.04g of 2-sulfonic acid terephthalic acid were dissolved in 20mL of N,N-dimethylformamide and weak acid mixed solution, which contained 16mL of N , N-dimethylformamide and 4mL of weak acid, and ultrasonically disperse the resulting mixture evenly. Then the dispersed mixed solution was placed in a reactor at 100° C. for 12 h. After the reaction, the obtained product was centrifuged, washed, soaked in methanol for 2 days, an...

Embodiment 2

[0050] 1. PVP-HNTs@UiO-66-SO 3 The preparation method of H is characterized in that it is carried out according to the following steps:

[0051] (1) 1g HNTs was dispersed in 2.5g / mL 250mL PVP aqueous solution, and then ultrasonically dispersed to form a mixed system. The reaction system was reacted at 60° C. for 18 h under magnetic stirring. After the reaction, the obtained product was washed with deionized water, collected by centrifugation, and dried in vacuum to obtain modified PVP-HNTs.

[0052] (2) 2.5g of PVP-HNTs, 1.4g of zirconium chloride and 1.4g of 2-sulfonic acid terephthalic acid were dissolved in 150mL of N,N-dimethylformamide and weak acid mixed solution, which contained 90mL of N , N-dimethylformamide and 60mL of weak acid, and ultrasonically disperse the resulting mixture evenly. Then the dispersed mixed solution was placed in a reaction kettle at 150° C. for 24 h. After the reaction, the obtained product was centrifuged, washed, soaked in methanol for 2 d...

Embodiment 3

[0060] 1. PVP-HNTs@UiO-66-SO 3 The preparation method of H is characterized in that it is carried out according to the following steps:

[0061] (1) 10g HNTs were dispersed in 5g / mL 500mL PVP aqueous solution, and then ultrasonically dispersed to form a mixed system. The reaction system was reacted at 90° C. for 24 h under magnetic stirring. After the reaction, the obtained product was washed with deionized water, collected by centrifugation, and dried in vacuum to obtain modified PVP-HNTs.

[0062] (2) 5g of PVP-HNTs, 2.4g of zirconium chloride and 2.7g of 2-sulfonic acid terephthalic acid were dissolved in 250mL of N,N-dimethylformamide and weak acid mixed solution, which contained 220mL of N, N-dimethylformamide and 30mL of weak acid, and the resulting mixture was dispersed uniformly by ultrasonic. Then the dispersed mixed solution was placed in a reactor at 180° C. for 36 h. After the reaction, the obtained product was centrifuged, washed, soaked in methanol for 2 days...

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Abstract

The invention belongs to the field of solid catalysts, and provides a one-step synthesized composite acid solid catalyst PVP-HNTs@UiO-66-SO3H, a preparation method thereof and an application of the catalyst. The preparation method includes steps of dissolving modified HNTs, zircon salt and 2-sulfo terephthalic acid in weakly acidic solution, uniformly dispersing obtained mixed solution under ultrasonic conditions and placing the mixed solution into a reactor for reaction; filtering, collecting and washing reacted products; soaking the washed products in low boiling point solvents, filtering the washed products and then performing vacuum drying to obtain PVP-HNTs@UiO-66-SO3H materials. The PVP-HNTs@UiO-66-SO3H has a porous structure, a large specific surface area and high heat stability, adsorption of fructose molecules is effectively promoted, and the efficiency of preparing HMF (hydroxymethyl furfural) by fructose dehydration is improved.

Description

technical field [0001] The invention belongs to the field of solid catalysts, in particular to composite acidic solid catalysts and a preparation method thereof. Background technique [0002] With the increasing energy crisis and environmental pollution, seeking a sustainable green energy has become an urgent problem to be solved. Biomass energy has become an ideal energy source to replace non-renewable energy sources such as coal, oil, and natural gas because of its wide range of sources, low price, and abundant reserves. 5-Hydroxymethylfurfural (HMF) is a biomass-based platform compound that contains active aldehyde groups, hydroxyl groups and furan rings in its structural formula derived from biomass conversion. It can be derived from numerous downstream products through further reactions. It is a key intermediate connecting biomass chemistry and petrochemistry. Biomass preparation of HMF is one of the hotspots in the study of comprehensive utilization of biomass resour...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/10B01J37/34C07D307/46
CPCC07D307/46B01J31/2213B01J37/343B01J35/60
Inventor 刘猛张云雷李春香闫永胜金佩
Owner JIANGSU UNIV
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