Synthesis method of ZnO@SiO2 supported mesoporous niobium phosphate catalyst and application thereof in preparation of 5-hydroxymethylfurfural

A technology of niobium phosphate catalyst and hydroxymethyl furfural, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problem of low yield of 5-hydroxymethyl furfural

Active Publication Date: 2019-10-08
LUSHAN COLLEGE OF GUANGXI UNIV OF SCI & TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the yield of many preparations of 5-hydroxymethylfurfural is not high, so it is particularly important to design and synthesize a catalyst with high catalytic e...

Method used

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  • Synthesis method of ZnO@SiO2 supported mesoporous niobium phosphate catalyst and application thereof in preparation of 5-hydroxymethylfurfural
  • Synthesis method of ZnO@SiO2 supported mesoporous niobium phosphate catalyst and application thereof in preparation of 5-hydroxymethylfurfural
  • Synthesis method of ZnO@SiO2 supported mesoporous niobium phosphate catalyst and application thereof in preparation of 5-hydroxymethylfurfural

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Embodiment 1

[0021] Example 1: A ZnO@SiO 2 The synthetic method of supported mesoporous niobium phosphate catalyst comprises the following steps:

[0022] (1) Preparation of nano-zinc oxide: Accurately weigh 2.195g of zinc acetate dihydrate (Zn(CH 3 COO) 2 2H 2 O), and it was uniformly dissolved in 100mL CH 3 CH 2OH, and fully stirred at 65°C for 20min to obtain a homogeneous solution; then take sodium hydroxide (0.4g) and dissolve it in 100mLCH 3 CH 2 OH, and fully dissolved at 50°C; the Zn(CH 3 COO) 2 2H 2 The O solution was cooled to 50°C, and 5 mL of polyethylene glycol 200 (PEG200) was added. After stirring for 10 min, the sodium hydroxide ethanol solution was quickly added to the Zn(CH 3 COO) 2 2H 2 In the O solution, the nanometer zinc oxide solution is obtained after reacting for 10 minutes;

[0023] (2) ZnO@SiO 2 Preparation of core-shell quantum dots: Accurately take 200 μL of concentrated ammonia water and 100 mL of absolute ethanol, and mix them evenly to obtain NH...

Embodiment 2

[0027] Embodiment 2: a kind of ZnO@SiO as described in embodiment 1 2 The application of the supported mesoporous niobium phosphate catalyst in the preparation of 5-hydroxymethylfurfural, weigh 0.04g glucose and place it in a 50mL beaker and add 20mL water to ultrasonically dissolve it completely. Add γ-valerolactone and glucose solution at a ratio of 1:9, stir evenly and add crushed ZnO@SiO 2 Load mesoporous niobium phosphate catalyst, the mass ratio of catalyst to glucose is: 120:0.24, then place the round-bottomed flask in a heater with a temperature of 140°C, install a condensing reflux device and pass tap water, and carry out heating and reflux reaction for 80 minutes. After taking out the reaction flask, filter it with a suction filter bottle while it is hot, and the liquid obtained by suction filtration is 5-hydroxymethylfurfural solution, and the yield is 84.96%.

[0028] The calculation of the detection and yield of product 5-hydroxymethylfurfural is as follows:

[...

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Abstract

The invention relates to a synthesis method of a ZnO@SiO2 supported mesoporous niobium phosphate catalyst and application thereof in preparation of 5-hydroxymethylfurfural. The synthesis method comprises the following steps: reacting diammonium hydrogen phosphate with niobium tartrate to generate niobium phosphate; reacting the niobium phosphate with a core-shell quantum dot ZnO@SiO2; after carrying out aging reaction for 24 h, centrifuging and drying, and calcining for 5 h at the temperature of 500 DEG C to synthesize a NbOPO4-ZnO@SiO2 solid acid catalyst; in a biphasic reaction system of water and gamma-valerolactone, taking glucose as a raw material, and preparing 5-hydroxymethylfurfural by catalytic hydrolysis of NbOPO4-ZnO@SiO2. The optimal preparation process conditions are as follows: the reaction time is 80 min, the reaction temperature is 140 DEG C, the use amount of the catalyst is 0.12 g, the use amount of the glucose is 0.24 mg, and the volume ratio of the water to the gamma-valerolactone is 1:9, and the yield of the 5-hydroxymethylfurfural is significantly increased by the process and is 84.96%.

Description

technical field [0001] The invention relates to a ZnO@SiO 2 Synthesis method of supported mesoporous niobium phosphate catalyst and its application in preparation of 5-hydroxymethylfurfural. Background technique [0002] 5-Hydroxymethylfurfural (5-hydroxymethylfurfural, 5-HMF) contains a molecule of furan ring, aldehyde group and hydroxymethyl group respectively, and can prepare various derivatives through oxidation, hydrogenation, condensation and other reactions. It is a kind of Important pharmaceutical and chemical intermediates. In recent years, with the development of technology for preparing 5-hydroxymethylfurfural from biomass resources, the research on the synthesis of 5-hydroxymethylfurfural from monosaccharides (such as glucose and fructose) has been deepened, and acid-catalyzed fructose is the It is an ideal and efficient way to prepare 5-hydroxymethylfurfural, but the limited source of fructose and high cost are not conducive to its large-scale and commercial a...

Claims

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Application Information

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IPC IPC(8): B01J27/195C07D307/46
CPCB01J27/195C07D307/46
Inventor 罗应李彦青李利军李红金程昊孔红星
Owner LUSHAN COLLEGE OF GUANGXI UNIV OF SCI & TECH
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