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Catalyst for converting ethyl levulinate into gamma-valerolactone and preparation method thereof

A technology of ethyl levulinate and catalyst, applied in the field of heterogeneous catalyst and preparation thereof, can solve the problems of easy deactivation, low catalyst activity, harsh reaction conditions and the like

Active Publication Date: 2019-12-31
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved in the present invention is that the EL catalytic hydrodealcoholization synthesis GVL reaction has harsh reaction conditions, the catalyst activity is not high and is easy to deactivate, and a catalyst with high activity and reusability and its preparation method are provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 0.16g hafnium tetrachloride, 0.080g terephthalic acid and 0.0054g 2-sulfonic acid terephthalic acid monosodium salt and dissolve in a polytetrafluoroethylene reactor containing 27mL dimethylformamide to obtain a mixed solution , stirred for 30 minutes, and added dropwise 3ml of acetic acid, and continued to stir for 10 minutes. The molar ratio of hafnium tetrachloride, terephthalic acid, 2-sulfonic acid terephthalic acid monosodium salt and dimethylformamide in the mixed solution was 1: 0.96:0.04:700; the above mixed solution was sealed and placed in an oven for crystallization at 80°C for 10 hours to obtain a solid. Cool to room temperature, filter the obtained solid with dimethylformamide, and dry; put the obtained filter cake into 100 mL methanol solution, stir for 24 hours; wash with methanol, filter with suction, and dry the obtained solid at 60°C for 6 hours to obtain SO 3 H-MOF(Hf); take the dried SO 3 Put 0.2 g of H-UiO-66 sample in a beaker, add 20 mL o...

Embodiment 2

[0024] Weigh 0.16g of hafnium tetrachloride, 0.050g of terephthalic acid and 0.054g of 2-sulfonic acid terephthalic acid monosodium salt and dissolve in a polytetrafluoroethylene reactor containing 27mL of dimethylformamide to obtain mixed solution, stirred for 30min, and 3ml of acetic acid was added dropwise, and continued to stir for 10min, the molar ratio of hafnium tetrachloride, terephthalic acid, 2-sulfonic acid terephthalic acid monosodium salt and dimethylformamide in the mixed solution was 1:0.6:0.4:700; the above mixed solution was sealed and placed in an oven for crystallization at 120°C for 24 hours to obtain a solid. Cool to room temperature, filter the obtained solid with dimethylformamide, and dry; put the obtained filter cake into 100 mL methanol solution, stir for 24 hours; wash with methanol, filter with suction, and dry the obtained solid at 120°C for 12 hours to obtain SO 3 H-MOF(Hf); take the dried SO3 Put 0.2 g of H-UiO-66 sample in a beaker, add 20 mL o...

Embodiment 3

[0027] Weigh 0.16g of hafnium tetrachloride and 0.134g of 2-sulfonic acid terephthalic acid monosodium salt and dissolve it in a polytetrafluoroethylene reactor containing 27mL of dimethylformamide to obtain a mixed solution, stir for 30min, and drop Add 3ml of acetic acid and continue to stir for 10 minutes. The molar ratio of hafnium tetrachloride, 2-sulfonic acid terephthalic acid monosodium salt and dimethylformamide in the mixture is 1:1:700; Crystallized in an oven at 200°C for 40h to obtain a solid. Cool to room temperature, filter the obtained solid with dimethylformamide, and dry; put the obtained filter cake into 100mL methanol solution, stir for 24h; wash with methanol, filter with suction, and dry the obtained solid at 150°C for 20h to obtain SO 3 H-MOF(Hf); take the dried SO 3 Put 0.2 g of H-UiO-66 sample in a beaker, add 20 mL of deionized water, and, under constant stirring, dissolve 0.7 mL of RuCl with a concentration of 0.15 mol / L 3 The solution was slowly ...

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Abstract

The invention provides a catalyst for conversion of ethyl levulinate into gamma-valerolactone and a preparation method of the catalyst. The catalyst comprises two parts, namely, sulfonic acid functionalized hafnium-based-metal organic framework material SO3H-MOF (Hf) and noble metal Ru nano-particles, wherein the noble metal Ru accounts for 0.5%-5% of the total weight of the catalyst, and the sulfonic acid group SO3H accounts for 0-20% of the total weight of the catalyst. The preparation method comprises the steps as follows: adding hafnium tetrachloride, terephthalic acid and monosodium 2-sulfoterephthalate to a mixed solution of dimethylformamide and acetic acid, and performing crystallizing, washing and drying to obtain the sulfonic acid functionalized hafnium-based-metal organic framework material SO3H-MOF (Hf); then, adding a RuCl3 solution dropwise to obtain a catalyst precursor, performing reduction on the catalyst precursor with sodium borohydride, and performing aftertreatment on the catalyst precursor with hydrochloric acid to obtain the catalyst. The catalyst has better catalytic activity, selectivity and reusability when used for conversion of ethyl levulinate into gamma-valerolactone.

Description

technical field [0001] The invention relates to a heterogeneous catalyst and a preparation method thereof, in particular to a catalyst for converting ethyl levulinate into gamma-valerolactone and a preparation method thereof. Background technique [0002] Biomass is a renewable resource abundant in nature. With the depletion of fossil resources, the preparation of fuels and chemicals from biomass has attracted people's attention. The conversion of biomass to fuels and chemicals usually goes through biomass platform molecular steps. Among many biomass platform molecules, γ-valerolactone (GVL) is a very potential compound with broad application prospects and has attracted extensive attention from academia and industry. A variety of catalytic systems have been developed for the preparation of GVL from levulinic acid (LA), but most of them are based on the separation and purification of LA from cellulose acid hydrolysis mixture. If LA is separated from the hydrolyzate, due to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07D307/33
CPCB01J31/1691B01J31/2239B01J2531/0213B01J2531/49C07D307/33
Inventor 张富民林真真
Owner ZHEJIANG NORMAL UNIVERSITY
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