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Synthesizing method of Ag@SiO2 supported mesoporous niobium phosphate catalyst and application of Ag@SiO2 supported mesoporous niobium phosphate catalyst in 5-hydroxymethylfurfural preparation

A niobium phosphate catalyst, hydroxymethyl furfural technology, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry and other directions, can solve the problems of difficult catalyst recovery, difficult sample handling, high toxicity and other problems

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

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Problems solved by technology

[0004] Although the application performance of metal salt catalysts and Lewis acids is good, there are disadvantages such as high toxicity, difficult sample handling in the later stage, and difficulty in catalyst recovery.

Method used

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  • Synthesizing method of Ag@SiO2 supported mesoporous niobium phosphate catalyst and application of Ag@SiO2 supported mesoporous niobium phosphate catalyst in 5-hydroxymethylfurfural preparation
  • Synthesizing method of Ag@SiO2 supported mesoporous niobium phosphate catalyst and application of Ag@SiO2 supported mesoporous niobium phosphate catalyst in 5-hydroxymethylfurfural preparation
  • Synthesizing method of Ag@SiO2 supported mesoporous niobium phosphate catalyst and application of Ag@SiO2 supported mesoporous niobium phosphate catalyst in 5-hydroxymethylfurfural preparation

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Embodiment 1

[0022] Embodiment 1: a kind of Ag@SiO2 supports the synthesis method of mesoporous niobium phosphate catalyst, comprises the following steps:

[0023] (1) Ag@SiO 2 Synthesis of nanoparticles: Weigh 0.85 g (0.005 mol) of AgNO 3 Place in 200 mL of secondary water, dissolve evenly in a water bath at 23°C, add 80 mL of PEG 200 and stir for 20 min, then take 1.135 g of sodium borohydride and place it in 200 mL of secondary water to fully dissolve and slowly add the above Stir the solution while adding it dropwise, and quickly adjust the stirring speed to 400r / min after the sodium borohydride solution is added dropwise, so that the solution at this time is vigorously stirred for 15 minutes. Bare nanosilver particles are produced. Then slowly drop 60mL of TEOS into the nano-silver aqueous solution, adjust the temperature of the water bath to 50°C and stir for 2 h to obtain Ag@SiO 2 Aqueous solution, sealed and kept at room temperature for use.

[0024] (2) Preparation of niobium ...

Embodiment 2

[0028] Embodiment 2: a kind of Ag@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 5:95, stir evenly and add crushed Ag@SiO 2 Load mesoporous niobium phosphate catalyst, the mass ratio of catalyst to glucose is: 60:0.36, then place the round-bottomed flask in a heater with a temperature of 160°C, install a condensing reflux device and pass tap water, and carry out heating and reflux reaction for 120min. 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 88.23%.

[0029] The calculation of the detection and yield of product 5-hydroxymethylfurfural is as follows:

[0030] ...

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Abstract

The invention relates to a synthesizing method of a Ag@SiO2 supported mesoporous niobium phosphate catalyst and application of the Ag@SiO2 supported mesoporous niobium phosphate catalyst in 5-hydroxymethylfurfural preparation. The synthesizing method is characterized in that niobium oxide phosphate NbOPO4 serving as the solid acid source is allowed to have reaction with core-shell quantum dots Ag@SiO2 by utilizing the synergistic effect of nano silver and niobium oxide phosphate and the bonding effect of SiO2 and NbOPO4 to prepare the mesoporous solid acid catalyst Ag@SiO2-NbOPO4. On the basisof the mesoporous solid acid catalyst Ag@SiO2-NbOPO4, renewable glucose is used as the raw material to prepare 5-hydroxymethylfurfural through a water / gamma-valerolactone double-phase system under optimal preparation conditions that reaction temperature is 160 DEG C, reaction time is 120 minutes, the use amount of the Ag@SiO2 supported mesoporous niobium phosphate catalyst is 0.06g, the volume ratio of water to valerolactone is 5:95 and the use amount of glucose is 0.36mg, the yield of the 5-hydroxymethylfurfural can reach 88.23%, and an evident effect is achieved.

Description

technical field [0001] The present invention relates to a kind of Ag@SiO 2 Synthesis method of supported mesoporous niobium phosphate catalyst and its application in preparation of 5-hydroxymethylfurfural. Background technique [0002] 5-Hydroxymethylfurfural (5-HMF), as an important platform compound, can undergo oxidation, hydrogenation, condensation and other reactions through the convertible functional group aldehyde group, hydroxyl group or furan ring of conjugated diene in its molecule. It is widely used in the preparation of various high value-added chemical products and related derivatives. 5-Hydroxymethylfurfural and its derivatives can be used to replace petroleum fuels, manufacture various polymer materials, synthesize drugs and pesticides, and produce resinous plastics. At present, most researchers usually prepare 5-hydroxymethylfurfural through the dehydration of various types of acid-catalyzed monosaccharides (including fructose and glucose) and carbohydrates...

Claims

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Application Information

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