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Method for preparing levulinic acid alkyl ester catalyzed by biomass zinc-based solid acid

A technology catalyzed by alkyl levulinate and solid acid, which is applied in the reaction preparation of ester group and hydroxyl group, organic chemistry and other directions, can solve the problems of complex reaction steps and high cost, and achieves easy recovery, improved yield, and rich source of raw materials. Effect

Inactive Publication Date: 2018-12-28
宁波高新区诠宝绶新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The preparation of alkyl levulinate in the above inventions or prior art is mostly obtained by the direct esterification of levulinic acid and alcohol or the alcoholysis reaction of monosaccharide or polysaccharide as a substrate, but there are complicated reaction steps in the above reaction path, and the reaction High temperature is required, a large amount of excess alcohol needs to be added to the reaction system and the cost of product separation and purification is relatively high, which increases the production cost of alkyl levulinate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of method that biomass zinc-based solid acid catalysis prepares alkyl levulinate, its technical scheme is as follows:

[0019] According to the number of parts by mass, 25 parts of angelica lactone, 17 parts of fatty alcohol compound and 3 parts of biomass zinc-based solid acid are added to the high-pressure reactor, vacuumize, replace the air in the reactor with inert gas, and circulate Three times, then control the temperature at 80°C, and react for 3 hours; after the completion of the reaction, wash the crude product three times with saturated saline, then dry the organic phase with a desiccant, filter, and then distill under reduced pressure at 800pa to collect the fraction at 130°C. The purified alkyl levulinate can be obtained.

[0020] The fatty alcohol compound is isopropanol.

[0021] The inert gas is nitrogen.

[0022] Described biomass zinc-based solid acid is prepared according to the following scheme:

[0023] According to the number of parts by m...

Embodiment 2

[0027] A kind of method that biomass zinc-based solid acid catalysis prepares alkyl levulinate, its technical scheme is as follows:

[0028] According to the number of parts by mass, 20 parts of angelica lactone, 14 parts of fatty alcohol compound and 1 part of biomass zinc-based solid acid are added to the autoclave, vacuumize, replace the air in the reactor with inert gas, and circulate Three times, then control the temperature at 70°C, and react for 1h; after completing the reaction, wash the crude product three times with saturated saline, then dry the organic phase with a desiccant, filter, and then distill under reduced pressure at 500pa to collect fractions at 120°C. The purified alkyl levulinate can be obtained.

[0029] The fatty alcohol compound is ethanol.

[0030] The inert gas is argon.

[0031] Described biomass zinc-based solid acid is prepared according to the following scheme:

[0032] According to the number of parts by mass, 40 parts of biomass materials ...

Embodiment 3

[0036] A kind of method that biomass zinc-based solid acid catalysis prepares alkyl levulinate, its technical scheme is as follows:

[0037] According to the number of parts by mass, 30 parts of angelica lactone, 20 parts of fatty alcohol compound and 5 parts of biomass zinc-based solid acid are added to the high-pressure reactor, vacuumize, replace the air in the reactor with inert gas, and circulate Three times, then control the temperature at 90°C, and react for 6h; after the completion of the reaction, wash the crude product three times with saturated brine, then dry the organic phase with a desiccant, filter, and then distill under reduced pressure at 1000pa to collect the fraction at 140°C. The purified alkyl levulinate can be obtained.

[0038] The fatty alcohol compound is n-butanol.

[0039] The inert gas is nitrogen.

[0040] Described biomass zinc-based solid acid is prepared according to the following scheme:

[0041]According to the number of parts by mass, 60 ...

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Abstract

The invention relates to the field of fine chemicals, in particular to a method for preparing levulinic acid alkyl ester catalyzed by a biomass zinc-based solid acid. According to the method for preparing the levulinic acid alkyl ester catalyzed by the biomass zinc-based solid acid, the levulinic acid alkyl ester is prepared by taking angelica lactone and a fatty alcohol compound as reaction raw materials and using the biomass zinc-based solid acid as a catalyst. The method is an efficient levulinic acid alkyl ester preparation method free of byproducts. The method further has rich raw materials sources, a reagent is easy to recycle, the process flow and the production cost are simplified, and the method is green and environmentally friendly. The biomass zinc-based solid acid is taken as acatalyst, and the method for preparing levulinic acid ester is expanded.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for preparing alkyl levulinate by catalyzing a biomass zinc-based solid acid. Background technique [0002] In the last ten years, new researches on the properties and applications of alkyl levulinate have been emerging. Its applications are mainly reflected in green chemical solvents and additives. Its unique physical and chemical properties make it widely used in fine chemicals and petrochemical industries. It has been applied for a long time, and researchers have always paid attention to its preparation method. [0003] CN101052617A discloses a method for preparing esters of dicarboximidolevulinic acid and trans-4-oxo-2-pentenoic acid alkyl esters. The method comprises two reaction steps, wherein the first step of the two reaction steps is the bromination of alkyl levulinate to obtain (3 and 5)-brominated alkyl levulinate, and the The second step of the two-step reacti...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C69/716
CPCC07C67/03C07C69/716
Inventor 王琪宇王新
Owner 宁波高新区诠宝绶新材料科技有限公司
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