Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing alkyl levulinate by regulating water content

A technology of alkyl levulinate and water content, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of not deeply exploring the influence of water, etc., and achieves simple and easy implementation and reaction. Simple steps and few by-products

Active Publication Date: 2020-04-07
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although water was added to the initial reaction solution, the effect of water content on alkyl levulinate was not investigated in depth.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing alkyl levulinate by regulating water content
  • Method for preparing alkyl levulinate by regulating water content
  • Method for preparing alkyl levulinate by regulating water content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The preparation of embodiment 1 methyl levulinate:

[0047] Mix 10 grams of furfuryl alcohol, 75 grams of methanol, 2 grams of water and 1 gram of Amberlyst-15, react at a temperature of 80 ° C, and control the stirring speed at 300 rpm, and the reflux temperature of 20 ° C. After 6 hours of reaction, wait for the temperature Cool down to room temperature, remove the catalyst by filtration, and remove the methanol in the reaction mixture by distillation under reduced pressure at 35°C to obtain light yellow methyl levulinate, which is analyzed by high performance liquid chromatography, the conversion rate of furfuryl alcohol and the selection of methyl levulinate The properties were 100% and 97.52%, respectively, and the yield was 97.52%.

Embodiment 2

[0048] The preparation of embodiment 2 ethyl levulinate:

[0049] After mixing 5 grams of furfuryl alcohol, 500 grams of ethanol, 1 gram of water and 250 grams of ZSM-5, react at a temperature of 40 ° C, and control the stirring speed at 1000 rpm, the reflux temperature of 5 ° C, and wait for 0.5 hours after the reaction The temperature is lowered to room temperature, the catalyst is removed by filtration, and the ethanol in the reaction mixture is distilled off under reduced pressure at 40°C to obtain pale yellow ethyl levulinate, which is analyzed by high performance liquid chromatography, the conversion rate of furfuryl alcohol and the concentration of ethyl levulinate. The yields were 100% and 95.35%, respectively, and the yield was 95.35%.

Embodiment 3

[0050] The preparation of embodiment 3 ethyl levulinate:

[0051] After mixing 10 grams of furfuryl alcohol, 30 grams of 75% (volume percentage, the same below) ethanol, 280 grams of cyclohexane and 20 grams of Amberlyst-15, the temperature was reacted at 60 ° C, and the stirring speed was controlled to be 500 rpm, condensed and refluxed The temperature is 20 DEG C. After reacting for 5 hours, the temperature drops to room temperature, and the catalyst is removed by filtration. The ethanol in the reaction mixture is distilled off under reduced pressure at 40 DEG C. to obtain pale yellow ethyl levulinate, which is analyzed by high performance liquid chromatography. The conversion rate of furfuryl alcohol and the yield of ethyl levulinate were 100% and 96.36%, respectively, and the yield was 96.36%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing alkyl levulinate by regulating water content. The method comprises the following steps: at least mixing furfuryl alcohol, alkyl alcohol and an acidic catalyst to form a reaction system, carrying out a reaction under the conditions of continuous stirring and reflux condensation, regulating the content of water in the reaction system to enable a mol ratio of the furfuryl alcohol to the water to be 1: (0.1-5), and carrying out aftertreatment to obtain alkyl levulinate. The structural formula of the alkyl levulinate is as shown in the specification. In the structural formula, R is any one selected from the group consisting of -CH3, -C2H5, -C3H7, -C4H9 and -C5H11. Compared with the prior art, the method provided by the invention has the advantagesthat the alkyl levulinate is prepared by regulating the water content; process is simple and feasible; conditions are mild; cost is low; few byproducts are produced; maximum yield reaches 99.8%; and the problem of low yield of alkyl levulinate in conventional synthesis methods is solved.

Description

technical field [0001] The invention relates to a method for preparing alkyl levulinate, in particular to a method for preparing alkyl levulinate by regulating water content, and belongs to the field of organic synthesis. Background technique [0002] Alkyl levulinate is a potential green biomass-based platform compound with a wide range of applications. It can be used in chemical industries such as food flavor additives, pharmaceuticals, solvents and plasticizers, and can also be used as a new type of liquid fuel additive. [0003] Alcoholysis of furfuryl alcohol to prepare alkyl levulinate is a common and widely used industrial preparation method. In the prior art, furfuryl alcohol is used as raw material in the method for converting furfuryl alcohol into alkyl levulinate, acid is used as catalyst, and anhydrous alkyl alcohol is used as solvent. But according to the theoretical calculation result, the generation of alkyl levulinate will be inhibited if no water is added i...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/313C07C69/716
CPCC07C67/08C07C67/313C07C69/716
Inventor 张亚杰方雯婷马中森陈金波陆贻超
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI