Method for preparation of levulinate by solid acid catalyst catalyzed sugar conversion
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A technology of catalyst catalyzing sugar and solid acid catalyst, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor catalytic effect, low catalyst loading rate, etc. Yield effect
Inactive Publication Date: 2017-11-17
CHINA UNIV OF MINING & TECH
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[0005] The purpose of the present invention is to provide a method for the preparation of levulinic acid ester by solid acid catalyzed sugar conversion with a high loading capacity, so as to solve the problems of low loading rate and poor catalytic effect of existing catalysts for preparing levulinic acid ester
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[0023] In the method for preparing levulinic acid ester of the present invention, sugar, catalyst, alcohol and cyclohexane are placed in a reaction kettle, reacted at a set temperature and a set time, and after the reaction is completed, the filtrate is taken out and filtered to obtain levulinic acid acid ester solution.
[0024] The concrete steps of preparation levulinate method:
[0025] a, sugar, solid acid catalyst, alcohol and hexanaphthene are placed in the reaction kettle and stirred evenly;
[0026] b. Seal the reaction kettle, set the temperature, and the rotation speed is 300r / min. When the temperature reaches the set value, it will react under the condition of the set time;
[0027] c. After the reaction time is up, quickly cool down to room temperature, open the reaction kettle, take out the filtrate of the product, and filter to obtain the levulinic acid ester solution.
[0028] The sugar is any one of glucose, fructose or sucrose.
[0029] Described alcohol i...
Embodiment 1
[0035] Get 0.5g solid acid catalyst Zr(SO 4 ) 2 / SiO 2 , 1.0 g of glucose, 30 ml of methanol and 10 ml of cyclohexane were placed in a reaction kettle at a reaction temperature of 200° C. for 30 minutes. After the reaction, the reactants were taken out and filtered to obtain a filtrate containing methyl levulinate. At this time, the yield of methyl levulinate was 35.82%.
Embodiment 2
[0037] Get 0.4g solid acid catalyst Zr(SO 4 ) 2 / SiO 2 , 2.0 g of fructose, 32 ml of absolute ethanol and 15 ml of cyclohexane were placed in a reaction kettle at a reaction temperature of 190° C. and reacted for 40 minutes. After the reaction was completed, the reactant was taken out and filtered to obtain a filtrate containing ethyl levulinate. At this time, the yield of ethyl levulinate was 41.12%.
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Abstract
Belonging to levulinate preparation methods, the invention provides a method for preparation of levulinate by solid acid catalyst catalyzed sugar conversion. The method includes: using sugar as the raw material, taking solid acid Zr(SO4)2/SiO2 as the catalyst, employing alcohol-cyclohexane as the reaction system, carrying out reaction under the circumstances of a reaction temperature of 170-220DEG C, a sugar dosage of 1.0-3.0g, an alcohol dosage of 20-50ml and a cyclohexane dosage of 10-20ml for 30-70min, and then performing filtering to obtain residue and a solution containing levulinate. The solid acid catalyst participating in the reaction has the advantages of high catalytic activity, no corrosion to equipment and no pollution to the environment, etc., and is in line with the development direction of green chemistry, thus providing a reliable path for biomass conversion to prepare high-value-added products. Compared with the prior art, the method provided by the invention mainly has the advantages that: 1. the active component Zr(SO4)2 is easily combined with the carrier SiO2; 2. catalysts with different loading capacities can be prepared according to needs; and 3. the solid acid catalyst can be recovered for recycling.
Description
technical field [0001] The invention relates to a method for preparing levulinate, in particular to a method for preparing levulinate by catalyzing sugar conversion with a solid acid catalyst. Background technique [0002] Levulinate, also known as pentaruvate, 4-ketovalerate or 4-oxopentanoate, the common ones mainly include methyl levulinate, ethyl levulinate and butyl levulinate, etc. Short-chain fatty esters, they are a kind of colorless transparent or yellow liquid with aromatic smell, easily soluble in most organic solvents such as ethanol, ether and chloroform, are a kind of very potential new energy chemicals, have a wide range of industrial Value. For example, its properties are similar to those of biodiesel, and it can be used as a blended fuel for transportation such as petrochemical diesel and biodiesel. After adding it, it can effectively improve combustion cleanliness, and has excellent lubricating ability, flash point stability and low temperature fluidity. ...
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