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Preparation of sulfonic acid modified polystyrene microspheres and method for catalyzing conversion of furfuryl alcohol into ethyl levulinate by using sulfonic acid modified polystyrene microspheres

A technology of polystyrene microspheres and polystyrene, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of large mass transfer resistance, poor catalyst stability, and poor thermal stability. Achieve the effect of easy recycling, stable structure and uniform size

Inactive Publication Date: 2021-11-02
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the shedding of active sites during the reaction will lead to poor stability of the catalyst, high mass transfer resistance and poor thermal stability.

Method used

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  • Preparation of sulfonic acid modified polystyrene microspheres and method for catalyzing conversion of furfuryl alcohol into ethyl levulinate by using sulfonic acid modified polystyrene microspheres
  • Preparation of sulfonic acid modified polystyrene microspheres and method for catalyzing conversion of furfuryl alcohol into ethyl levulinate by using sulfonic acid modified polystyrene microspheres
  • Preparation of sulfonic acid modified polystyrene microspheres and method for catalyzing conversion of furfuryl alcohol into ethyl levulinate by using sulfonic acid modified polystyrene microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Embodiment 1 prepares sulfonic acid group polystyrene microsphere catalyst

[0069] (1) After weighing 0.6g of benzoyl peroxide and dissolving it in 15g of styrene, mix it with 35mL of ethanol, 50mL of ethylene glycol methyl ether and 1.8g of PVP (130W) solution, and react at 80°C for 24h after passing through nitrogen to obtain 3um polystyrene seed microspheres (3-PS);

[0070] (2) Dissolve 0.25g of sodium dodecylbenzenesulfonate (SDS) in 80mL of water, then add 1.05g of butyl phthalate (DBP), and mix uniformly through ultrasonic to form emulsion A; 0.5g (1 ) prepared seed microspheres were dispersed in 7.5mL water to form a dispersion; and the dispersion was added to the emulsion, and stirred at room temperature (200rpm) for 20h to obtain a mixed solution A;

[0071] Add 3g of styrene (St), 5g of divinylbenzene (DVB), 8g of toluene and 0.1g of benzoyl peroxide (BPO) into 80mL of aqueous solution, and ultrasonically mix to form emulsion B; add emulsion B to the mixing...

Embodiment 2

[0079] Embodiment 2 catalytically prepares ethyl levulinate

[0080] (1) Weigh 1mmol furfuryl alcohol, 0.075g PS-SO 3 H catalyst and 4mL ethanol are added in the 25mL reactor with magneton;

[0081] (2) The above reactor was placed in an oil bath at 120° C. and stirred for 2 hours, and cooled to room temperature after the reaction was completed.

[0082] Take 1 mL of the reacted solution and use gas phase (GC) to measure the conversion rate of furfuryl alcohol and the yield of ethyl levulinate. The conversion rate of furfuryl alcohol was 99.7%, and the yield of ethyl levulinate was 94.1%.

Embodiment 3

[0083] Embodiment 3 catalytically prepares ethyl levulinate

[0084] (1) Weigh 1mmol furfuryl alcohol, 0.075g PS-SO 3 H and 4mL of ethanol were added to a 25mL reactor with magnets;

[0085] (2) Place the above reactor in an oil bath at 120° C. and stir for 1.5 h. After the reaction is completed, cool to room temperature. Take 1 mL of the reacted solution and use GC to measure the conversion rate of furfuryl alcohol and the yield of ethyl levulinate.

[0086] The amount of microspheres in step (1) was changed from 0.075 g to 0.025, 0.05 and 0.10 respectively, and other conditions were unchanged; 1 mL of the reaction solution was taken to measure the conversion rate of furfuryl alcohol and the yield of ethyl levulinate by GC. The result is as Figure 7 Shown, PS-SO 3 When the amount of catalyst H was 0.025, 0.05, 0.075 and 0.10 g, the yields of ethyl levulinate obtained were 87.32%, 92.55%, 94.7% and 86%, respectively.

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Abstract

The invention discloses preparation of sulfonic acid modified polystyrene microspheres and a method for catalyzing conversion of furfuryl alcohol into ethyl levulinate by using the sulfonic acid modified polystyrene microspheres, and belongs to the technical field of heterogeneous catalysis. The sulfonic acid functionalized polystyrene microsphere catalyst is prepared in a specific emulsion polymerization swelling mode, synthesis steps are simple, raw materials are cheap and easy to obtain, the specific surface area is large, and the raw materials are easy to recover; meanwhile, the catalyst can also be used for catalytic reaction, furfuryl alcohol is reduced into ethyl levulinate in a high-selectivity mode, the catalytic performance cannot be reduced after repeated use, and the requirement for green and sustainable development is met.

Description

technical field [0001] The invention relates to the preparation of sulfonic acid-modified polystyrene microspheres and a method for catalyzing the conversion of furfuryl alcohol into ethyl levulinate, belonging to the technical field of heterogeneous catalysis. Background technique [0002] Biomass energy is a kind of renewable energy, which has attracted widespread attention due to its characteristics of recyclability, wide distribution, and cleanliness. As a kind of biomass energy, levulinic acid ester has a wide range of applications in many fields. Catalysts traditionally used for the synthesis of levulinate are strong Acidic mineral acids (HCl, H 2 SO 4 and HF), although they are cheap, they have the disadvantages of polluting the environment, corroding equipment, and being difficult to separate from the product. At present, from the perspective of environmental protection and economy, the use of heterogeneous catalytic system to synthesize levulinate is not only e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J35/10B01J35/08C08F257/02C08F212/08C08F212/36C08F2/26C08F8/36C08J9/00C07C67/00C07C69/716C08L51/00
CPCB01J31/063C08F257/02C08F2/26C08F8/36C08J9/00C07C67/00C08J2351/00B01J35/51B01J35/633B01J35/647B01J35/615C08F212/08C08F212/36C07C69/716
Inventor 胡爱云丁健王海军刘晓庆
Owner JIANGNAN UNIV
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