High-yield levulinic acid ester preparation method under catalysis of solid acid

A high-yield technology for levulinic acid esters and acid catalysis, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of acid point loss and yield reduction, and achieve good reactivity.

Active Publication Date: 2013-11-27
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The used catalyst can maintain a certain activity after high temperature activation, but there is also the loss of acid points, resulting in a decrease in yield

Method used

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  • High-yield levulinic acid ester preparation method under catalysis of solid acid

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Preparation of tin-containing molecular sieve Sn-Beta:

[0032] Take 20 parts of hydrogen-type Beta molecular sieve (H-Beta) (beta molecular sieve produced by Nankai Catalyst Factory) and mix with 400 parts of 13M nitric acid solution, heat to 100°C for 20 hours; filter, wash until neutral, put in an oven at 120°C After drying, transfer to a vacuum drying oven to dry at 180°C for 5 hours to remove water to obtain dealuminated molecular sieve (deAlBeta); take 5 parts of deAlBeta and dissolve it in 100 parts of benzene, then add 10 parts of anhydrous SnCl 4 , stirred at 25°C for 24h, filtered, washed with 1000 parts of benzene to remove free SnCl 4 , 550 ° C air activation 3h, after cooling to get Sn-Beta.

Embodiment 2

[0034] SBA-15-SO 3 Preparation of H:

[0035] Stir and dissolve 4 parts of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123, M=5800) with 121 parts of 1.9M hydrochloric acid solution; heat to 40°C after complete dissolution Slowly add 6.82 parts of tetraethyl silicate dropwise, pre-hydrolyze for 150 minutes, then add dropwise 1.61 parts of mercaptopropyltrimethoxysilane, and keep stirring at 40°C for 20 hours. After the reaction, put it into 400 parts of hydrothermal reaction kettle for aging at 120°C for 24 hours; cool it, filter it with a Buchner funnel to obtain a white solid, put it into a Soxhlet extractor, and use ethanol as the extraction agent to reflux and extract for 24 hours. ℃ vacuum oven drying for 10h to obtain SBA-15-SO 3 H.

Embodiment 3

[0037] Carbon-SO 3 Preparation of H:

[0038] Take 20 parts of microcrystalline cellulose, react at 450 ° C for 5 h under the protection of argon, and obtain black activated carbon; take 4.3 parts of activated carbon and 300 parts of concentrated sulfuric acid, mix them and heat up to 120 ° C for sulfonation for 24 h; after cooling, dilute with water to 1000 parts, use Buchner funnel filtration, vacuum drying to obtain Carbon-SO 3 H.

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Abstract

The invention discloses a high-yield levulinic acid ester preparation method under catalysis of solid acid and belongs to the field of organic synthesize. The method comprises the following steps: uniformly mixing 1 part of sugar, 10-100 parts of alcohol, 0.01-0.2 part of acid B and 0.1-1 part of acid L, and performing reaction under the temperature of 130-190 DEG C for 1-20 h to obtain a levulinic acid methyl ester solution, wherein the acid L is stanniferous molecular sieve, and the acid B is SBA-15-SO3H, Carbon-SO3H or Amberlyst-15. According to the method, the carbohydrate is low in cost and easy to obtain; with the acid B and acid L which can be used repeatedly, the catalysis effect basically remains the same; the levulinic acid ester compound prepared in one step can be widely applied to industries of food additives, essence spices, chemical reaction intermediates, gasoline, diesel-dopes and the like.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a method for preparing levulinic acid ester with solid acid catalysis and high yield. Background technique [0002] In the traditional method of preparing levulinic acid, cheap water is used as solvent, but a large amount of humin is produced, resulting in low yield. Recently, researchers have begun to study the reaction behavior of sugars when alcohols (especially methanol) are used as solvents. When water is used as a solvent, the intermediate 5-hydroxymethylfuran is prone to side reactions to generate humin, which leads to a decrease in the yield of LA; while when methanol is used as a solvent, 5-hydroxymethylfuran can first react with methanol to form humin, which is not conducive to The produced intermediate thus increases the yield of levulinate. [0003] Riisager et al. (Catalysis Communications, 2011, 17:71-75.) studied under relatively mild conditions (140°C, ethanol sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/00
Inventor 郭庆祥刘海峰邓理魏续瑞廖兵庞浩
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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