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Novel supported heteropolyacid catalyst and application thereof in preparation of levulinate

An acid catalyst, supported technology, applied in the preparation of carboxylate, molecular sieve catalyst, preparation of organic compounds, etc., can solve the problem of unsatisfactory effect, no technical solution report of levulinate catalyst, unfavorable product separation and catalyst recovery, etc. problems, to achieve the effect of easy recovery and recycling, improved acidity and recyclability, and stable properties

Active Publication Date: 2021-03-12
BEIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There have been reports on the preparation of levulinic acid esters from heteropolyacids as catalysts, and reports on the preparation of molecular sieves, especially zeolite molecular sieves, for the preparation of levulinic acid esters, but there is no preparation of levulinic acid with heteropolyacid-loaded molecular sieves as biomass conversion Report on the Technical Scheme of Ester Catalyst
Heteropolyacids with Keggin structure—H 3 PW 12 o 40 has a strong Acidity plays a big role in catalyzing biomass alcoholysis, fructose dehydration, and alcoholysis of HMF, but it is a homogeneous catalyst in the medium, which is not conducive to product separation and catalyst recovery
Zeolite molecular sieve Sapo-18 has Acidic and strong Lewis acidity, its Lewis acidity can catalyze the isomerization of glucose into fructose, but a single molecular sieve is not ideal in the reaction of preparing levulinate from biomass

Method used

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  • Novel supported heteropolyacid catalyst and application thereof in preparation of levulinate
  • Novel supported heteropolyacid catalyst and application thereof in preparation of levulinate
  • Novel supported heteropolyacid catalyst and application thereof in preparation of levulinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh molecular sieve Sapo-18 and polyacid compound H respectively by mass ratio 10:1 3 PW 12 o 40 It is 20ml water that the adsorption saturation of molecular sieve is measured by equal volume impregnation method, and polyacid compound H 3 PW 12 o 40 Pour it into the reactor, add 20ml of water, stir to dissolve, then add the polyacid solution dropwise to the Sapo-18 powder, stir while adding, stir for 60min after dissolving, let the reaction system stand for 24h, and precipitate light Gray solid, filtered and dried, put the solid in a muffle furnace, and calcined at 550 ° C for 4 hours to obtain 10% H 3 PW 12 o 40 / Sapo-18 catalyst.

[0032]Corn stalk powder 0.1g, 0.4g 10% H 3 PW 12 o 40 Put the catalyst of Sapo-18 into a high-pressure reactor, add 15ml of methanol solution, and heat and stir. The reaction temperature is 190°C, and the reaction time is 6h. After the reaction is finished, the reaction mixture is filtered after cooling, the clear liquid conta...

Embodiment 2

[0034] Weigh molecular sieve Sapo-18 and polyacid compound H respectively by mass ratio 10:2 3 PW 12 o 40 It is 20ml water that the adsorption saturation of molecular sieve is measured by equal volume impregnation method, and polyacid compound H 3 PW 12 o 40 Pour into the reactor, add 20ml of water, stir to dissolve, then add the polyacid solution dropwise to the Sapo-18 powder, stir while adding, stir for 60min after dissolving, let the reaction system stand for 24h, precipitate out Gray solid, filtered and dried, put the solid in a muffle furnace, and calcined at 550 ° C for 4 hours to obtain 20% H 3 PW 12 o 40 / Sapo-18 catalyst.

[0035] Corn stalk powder 0.1g, 0.3g 20% ​​H 3 PW 12 o 40 Put the catalyst of Sapo-18 into a high-pressure reactor, add 15ml of methanol solution, and heat and stir. The reaction temperature is 190°C, and the reaction time is 6h. After the reaction is finished, the reaction mixture is filtered after cooling, the clear liquid contains me...

Embodiment 3

[0037] Weigh molecular sieve Sapo-18 and polyacid compound H respectively by mass ratio 10:3 3 PW 12 o 40 ; Count more as compound H 3 PW 12 o 40 Pour it into the reactor, add 20ml of water according to the equal volume impregnation method, stir to dissolve, then add the polyacid solution dropwise to the Sapo-18 powder, stir while adding, stir for 60min after dissolving, and let the reaction system stand Set aside for 24 hours, a light gray solid is precipitated, filtered and dried, the solid is placed in a muffle furnace, and calcined at 550 ° C for 4 hours to obtain 30% H 3 PW 12 o 40 / Sapo-18 catalyst.

[0038] Corn stalk powder 0.1g, 0.4g 20% ​​H 3 PW 12 o 40 Put the catalyst of Sapo-18 into a high-pressure reactor, add 15ml of methanol solution, and heat and stir. The reaction temperature is 190°C, and the reaction time is 6h. After the reaction is finished, the reaction mixture is filtered after cooling, the clear liquid contains methyl levulinate, and the pr...

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Abstract

The invention belongs to the technical field of catalyst preparation and application, and particularly relates to a novel solid supported heteropolyacid catalyst. Meanwhile, the invention also relatesto application of the supported catalyst in preparation of levulinate. According to the invention, H3PW12O40 / Sapo-18 catalyst is prepared by loading a molecular sieve and the heteropolyacid accordingto different proportions, the strong acidity of the heteropolyacid can be loaded on the surface of the molecular sieve, the acidity of the catalyst is enhanced, the supported heteropolyacid catalystwith the optimal acidity and Lewis acidity proportion is obtained by regulating the loading capacity of the heteropolyacid, and a synergistic effect is achieved, the catalytic effect is greatly improved. Meanwhile, the conversion of the heteropolyacid catalyst from a homogeneous phase to a heterogeneous phase is also realized, and the green and sustainable use of the catalyst is realized.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation and application, and in particular relates to a new solid-loaded heteropolyacid catalyst. At the same time, the invention also relates to the application of the supported catalyst in the preparation of levulinate. Background technique [0002] Biomass resources have the characteristics of low cost, renewable, extensive resources, and environmental friendliness. The use of biomass resources to produce related chemicals is of great significance to the realization of sustainable development. For example, an important platform chemical, levulinic acid, is mainly used in the production of various biochemicals such as solvents, resins, plasticizers, polymers, herbicides, pharmaceuticals, etc. through esterification, substitution, and redox , flavorings and biofuels, which can be obtained from cellulose-rich biomass resources. [0003] Cellulose is the most abundant high-molecular carbohyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J31/26B01J29/85C07C69/716C07C67/00
CPCB01J27/188B01J29/85C07C67/00B01J2229/186C07C69/716Y02P20/584
Inventor 段喜鑫周瑜时君友
Owner BEIHUA UNIV