Method for preparing levulinic acid by catalyzing bamboo shoot shells through functional ionic liquid

A technology of levulinic acid and ionic liquid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate and other directions, can solve the problems of unrecoverable acid liquid, no reuse, high reaction temperature, etc. Hydrolysis reaction rate and reaction efficiency, promoting reaction rate and quality, and the effect of strong transformation specificity

Inactive Publication Date: 2013-04-10
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main disadvantage of the scheme described in the above-mentioned documents is that the used acid solution cannot be recycled, the reaction temperature is high, and the reaction time is long
[0006] On the other hand, the shells of bamboo shoots have always been worthless waste
In the south of my country, where bamboo is abundant, hundreds of thousands of tons of bamboo shoot shells are either discarded to the field for fertilization or landfill; there is no case of reuse; there is nothing about the preparation of levulinic acid from bamboo shoot shells catalyzed by functional ionic liquids research report

Method used

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  • Method for preparing levulinic acid by catalyzing bamboo shoot shells through functional ionic liquid
  • Method for preparing levulinic acid by catalyzing bamboo shoot shells through functional ionic liquid
  • Method for preparing levulinic acid by catalyzing bamboo shoot shells through functional ionic liquid

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Experimental program
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Effect test

Embodiment 1

[0039] Bamboo shoot shells (bamboo shoots, Phyllostachys Praecox f.preveynalis, origin Taihuyuan Town, Lin’an, Zhejiang Province) were dried in an oven at 75°C to a moisture content of 9.1%, crushed to a particle size of less than 830 μm, and the functional ionic liquid was [C 2 mim]HSO 4 , The solid-liquid ratio of bamboo shoot shells and functional ionic liquid is 3:100; ultrasonic dissolution, ultrasonic working conditions are: ultrasonic power 1500W, working gap ratio 3s:5s, time 30min. Microwave reaction promotes catalytic conversion. Microwave working conditions are: microwave power 1200W, temperature setting 120°C, reflux cycle 2mL / min, helium protection and saturation for 20min, flow rate 3mL / min, stirring speed 120r / min, and reaction time 120min.

[0040] After the reaction, wash with 2 times the volume of water and centrifuge to obtain the levulinic acid aqueous solution and the functional ionic liquid respectively; then use an ultrafiltration system to remove the ma...

Embodiment 2

[0043] Bamboo shoot shells (bamboo shoots, Phyllostachys Praecox f.preveynalis, origin Taihuyuan Town, Lin’an, Zhejiang Province) were dried in an oven at 75°C to a moisture content of 10%, and crushed to a particle size of less than 830 μm. The functional ionic liquid was [C 4 mim]HSO 4 , the solid-liquid ratio of bamboo shoot shells and functional ionic liquid is 3:100; ultrasonic dissolution, ultrasonic working conditions are: ultrasonic power 1500W, working gap ratio 3s:5s, time 40min. Microwave reaction promotes catalytic conversion. Microwave working conditions are: microwave power 1200W, temperature setting 120°C, reflux cycle 2mL / min, helium protection, flow rate 3mL / min, stirring speed 120r / min, reaction time 130min.

[0044] After the reaction, wash with 2 times the volume of water and centrifuge to obtain the levulinic acid aqueous solution and the functional ionic liquid respectively; then use an ultrafiltration system to remove the macromolecular organic matter wi...

Embodiment 3

[0047] Bamboo shoot shells (bamboo shoots, Phyllostachys Praecox f.preveynalis, origin Taihuyuan Town, Lin’an, Zhejiang Province) were dried in an oven at 75°C to a moisture content of 11%, crushed to a particle size of less than 380 μm, and the functional ionic liquid was [C 6 mim]HSO 4 , the solid-liquid ratio of bamboo shoot shells and functional ionic liquid is 5:100, adding 0.7% tin dichloride by reactant weight; ultrasonic dissolution, ultrasonic working conditions are: ultrasonic power 1500W, working gap ratio 2s:5s, time 30min. Microwave reaction promotes catalytic conversion. Microwave working conditions are: microwave power 1200W, temperature setting 120°C, reflux cycle 2mL / min, helium protection and saturation for 20min, flow rate 3mL / min, stirring speed 120r / min, and reaction time 100min. The reactants were determined by gas chromatography.

[0048] After the reaction, wash with 2 times the volume of water and centrifuge to obtain the levulinic acid aqueous soluti...

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Abstract

The invention relates to a method for catalyzing to convert wood fibers of bamboo shoot shells into a modular compound levulinic acid in an environment-friendly way by adopting medium recyclable functional ionic liquid. The method aims to prepare the levulinic acid from the bamboo shoot shells serving as raw materials, and has the characteristics of recyclable acid liquid, wide raw material sources, strong sustainability and conversion specificity, high reaction rate and high efficiency. The technical scheme is that: the method for preparing the levulinic acid by catalyzing the bamboo shoot shells through the functional ionic liquid comprises the following steps of: 1) drying and crushing the bamboo shoot shells, and mixing the crushed bamboo shoot shells and the functional ionic liquid in a reaction kettle; 2) promoting dissolution by using impulse ultrasound; 3) performing microwave heating and reflux circulating; 4) washing by using water, and separating washing liquid to separately obtain aqueous solution of levulinic acid and the functional ionic liquid; and 5) ultra-filtering, evaporating and drying the aqueous solution of levulinic acid to obtain refined levulinic acid, performing elution and vacuum drying on the functional ionic liquid, and recycling the functional ionic liquid or refrigerating the functional ionic liquid for later use.

Description

technical field [0001] The invention belongs to the field of recycling and green conversion and utilization of bamboo shoot waste of Linte food, and relates to a method for using a green chemical catalyst and a functional ionic liquid with a repeatable medium to greenly catalyze the conversion of bamboo shoot shell wood fiber into a modular compound levulinic acid. Background technique [0002] Levulinic acid (LA), also known as 4-oxopentanoic acid, has a wide range of uses and can be used to synthesize hundreds of products such as resins, plastics, and medicines, and can be used to manufacture liquid fuels. It is an important new type of biomass-based resource A green modular compound, this chemical has a molecular weight of 116.12. [0003] Cellulose is a renewable resource with the most content in nature in biomass, and is a natural biological macromolecule polysaccharide. The utilization and research of cellulose resources is an important content of current green chemis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/185C07C51/00
CPCY02P20/582
Inventor 周存山余筱洁张有做杨虎清王允祥
Owner JIANGSU UNIV
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