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Method for synthesizing levulinate

A technology of levulinic acid ester and levulinic acid, applied in the field of platform compound synthesis, to achieve the effect of high yield

Inactive Publication Date: 2018-11-13
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In view of the problems existing in the prior art, one of the purposes of the present invention is to provide a method for synthesizing levulinic acid ester by novel catalyst catalytic esterification method, improve the catalytic reaction efficiency of synthesizing levulinic acid ester by esterification method, both can Solve the problem of catalyst separation and reuse, and achieve a higher conversion rate of levulinic acid, and can be applied to alcohols with different carbon chain lengths as reactants

Method used

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  • Method for synthesizing levulinate
  • Method for synthesizing levulinate
  • Method for synthesizing levulinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A method for synthesizing ethyl levulinate, the steps are as follows:

[0037] Take 5mmol of levulinic acid, 10mL of ethanol, 0.116g of loaded PDA-SO 3 H solid acid catalyst (the mass ratio of levulinic acid to catalyst is 1:0.2) was successively added into a 100mL round-bottomed three-necked flask, and the esterification reaction took place at 70°C, 80°C, 90°C, 100°C, and 110°C for 5 hours respectively to obtain Ethyl levulinate. Among them load type PDA-SO 3 The mass ratio of the acid in the H solid acid catalyst to the PDA carrier is 96:100, and the catalyst is also coated with ferric oxide nanoparticles, and the mass ratio of the nanoparticles to the PDA carrier is 0.9:1. The conversion rate of levulinic acid is shown in Table 1.

[0038] Table 1

[0039] Esterification temperature

[0040] As can be seen from Table 1, as the esterification reaction temperature increases, the conversion rate of levulinic acid increases gradually, and when 100 DEG C, th...

Embodiment 2

[0042] A method for synthesizing n-butyl levulinate, the steps are as follows:

[0043] Take 5mmol of levulinic acid, 10mL of n-butanol, 0.116g of loaded PDA-SO 3 H solid acid catalyst (the mass ratio of levulinic acid to catalyst is 1:0.2) was successively added to a 100mL round-bottomed three-neck flask, and esterification reactions occurred at 70°C, 80°C, 90°C, and 100°C for 5 hours to obtain levulinic acid n-butyl ester. Among them load type PDA-SO 3 The mass ratio of the acid in the H solid acid catalyst to the PDA carrier is 87:100, and the catalyst is also coated with ferric oxide nanoparticles, and the mass ratio of the nanoparticles to the PDA carrier is 0.8:1. The conversion rate of levulinic acid is shown in Table 2.

[0044] Table 2

[0045] Esterification temperature

[0046] As can be seen from Table 2, as the esterification reaction temperature increases, the conversion rate of levulinic acid increases gradually, and when 90 DEG C, the conversion r...

Embodiment 3

[0048] A method for synthesizing n-octyl levulinate, the steps are as follows:

[0049] Take 5mmol of levulinic acid, 10mL of n-octanol, 0.116g of loaded PDA-SO 3 H solid acid catalyst (the mass ratio of levulinic acid to catalyst is 1:0.2) was successively added into a 100mL round-bottomed three-necked flask, and the esterification reaction occurred at 100°C, 110°C, and 120°C for 4 hours to obtain n-octyl levulinate . Among them load type PDA-SO 3 The mass ratio of the acid in the H solid acid catalyst to the PDA carrier is 77:100, and the catalyst is also coated with ferric oxide nanoparticles, and the mass ratio of the nanoparticles to the PDA carrier is 0.7:1. The conversion rate of propionic acid is shown in Table 3.

[0050] table 3

[0051] Esterification temperature

[0052] As can be seen from Table 3, as the esterification reaction temperature increases, the conversion rate of levulinic acid increases gradually, and when 110 DEG C, the conversion rate o...

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Abstract

The invention relates to a method for synthesizing levulinate. The method comprises the following step: catalyzing levulinic acid and alcohol to be subjected to esterification reaction by utilizing aloading type PDA-SO3H solid acid catalyst, so as to obtain the levulinate. According to the method provided by the invention, the loading type PDA-SO3H solid acid catalyst is used as the catalyst, canbe recycled and also can be used for more efficiently catalyzing the generation of the levulinate. The method directly takes the levulinic acid and the alcohol as raw materials and the levulinate issynthesized through one-step reaction; the selectivity of a product is higher than 99.9 percent and the yield is high; when the alcohol is enough, the conversion rate of the levulinic acid reaches 87percent or more.

Description

technical field [0001] The invention relates to the technical field of platform compound synthesis, in particular to a method for synthesizing levulinate. Background technique [0002] With the rapid development of modern economy, fossil energy is constantly being consumed, which prompts us to replace non-renewable fossil energy with renewable biomass energy. As an important platform compound, levulinic acid is mainly produced by catalytic hydrolysis of furfuryl alcohol and biomass hydrolysis, mainly including cellulose or starch as raw materials. Its downstream product, levulinate, is an important derivative of levulinic acid. It is a widely used biomass material and has great application value in spices, flavors, plasticizers, food additives, and biofuels. At this stage, it is mainly used in related fields such as food, medicine, cosmetics, plastics and fuel. Levulinic acid ester compounds have similar properties to biodiesel and can be used as additives for fossil fuels...

Claims

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Application Information

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IPC IPC(8): C07C69/716C07C67/08
CPCC07C67/08C07C69/716Y02P20/584
Inventor 王洪海刘洪丽姜艳军高丽雅李浩李春利刘文静卢一凡
Owner HEBEI UNIV OF TECH