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Method for separating and extracting ethyl levulinate from alcoholysis solution of biomass sugar

A technology of ethyl levulinate and biomass sugar, applied in the field of ethyl levulinate, can solve the problems of complex composition, coking of sugar plates, affecting the color and luster of extracting ethyl levulinate, etc., and achieve the effect of full utilization

Active Publication Date: 2015-06-10
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the composition of the reaction solution obtained by alcoholysis of sugars to produce ethyl levulinate is complex, including unreacted ethanol, remaining sugar, ethyl levulinate, pigments and other unknown components
[0008] Ethanol can be recovered by concentrating the reaction solution. This operation is relatively easy to realize, but it is more difficult to separate and purify ethyl levulinate from the concentrated solution. The main difficulties are: ① sugar alcohol hydrolysis to prepare ethyl levulinate The content of ethyl levulinate in the reaction liquid is very low, and it is difficult to extract; ②The reaction liquid contains a large amount of pigments that affect the color of the extracted ethyl levulinate; ③When high-temperature distillation collects ethyl levulinate, unreacted sugar will occur Hardening and coking, which is the most important obstacle in the industrialization of the technology of sugar reaction to produce ethyl levulinate

Method used

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  • Method for separating and extracting ethyl levulinate from alcoholysis solution of biomass sugar
  • Method for separating and extracting ethyl levulinate from alcoholysis solution of biomass sugar
  • Method for separating and extracting ethyl levulinate from alcoholysis solution of biomass sugar

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Effect test

Embodiment 1

[0021] Add 0.5g CaO to 500mL raw material solution (ethyl levulinate content is 2.46g / 100mL) to neutralize sulfuric acid as a catalyst, filter, gradually reduce and concentrate under reduced pressure at 70-100°C to remove ethanol and other low-boiling substances; then Add 15mL of dodecane and 5mL of triethyl citrate, continue to heat up to 165°C for extraction under reduced pressure and collect fractions, and finally obtain 11.6g of light yellow clear liquid (ethyl levulinate), accounting for ethyl levulinate in the raw material solution 94.3% of the ester, and the distillation residue does not appear hardened in the flask, and can be easily poured out from the flask.

Embodiment 2

[0023] Add 0.5g CaO to 500mL raw material solution (ethyl levulinate content is 2.46g / 100mL) to neutralize sulfuric acid as a catalyst, filter, gradually reduce and concentrate under reduced pressure at 50-100°C to remove ethanol and other low-boiling substances; then Add 15mL of dodecane, 15mL of tetradecane, 10mL of triethyl citrate and 5mL of triacetin, continue to heat up to 140°C for extraction under reduced pressure and collect fractions, and finally obtain a light yellow clear liquid (ethyl levulinate) 10.7g, accounted for 87% of ethyl levulinate in the raw material liquid, and the distillation residue did not appear hardened in the flask, and could be easily poured out from the flask.

Embodiment 3

[0025] Add 1.5g CaO to 500mL raw material solution (ethyl levulinate content is 2.46g / 100mL) to neutralize the sulfuric acid as a catalyst, filter, gradually reduce and concentrate under reduced pressure at 80-100°C to remove ethanol and other low-boiling substances; then Add 20mL of dodecane, 5mL of triethyl citrate and 10mL of glyceryl diacetate, continue to heat up to 150°C for extraction under reduced pressure and collect fractions, and finally obtain 10.3g of light yellow clear liquid (ethyl levulinate), accounting for the raw material 83.7% of the ethyl levulinate in the liquid, and the distillation residue does not appear hardened in the flask, and can be easily poured out from the flask.

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Abstract

The invention provides a method for separating and extracting ethyl levulinate from an alcoholysis solution of biomass sugar, and relates to ethyl levulinate. The method comprises the following steps: adding an acid removal catalyst into the alcoholysis solution of the biomass sugar, removing the acid and filtering, and then concentrating to remove substances with low boiling point to obtain a concentrated solution; adding a heat conducting agent and a cosolvent into the concentrated solution, heating and then depressurizing, distilling and collecting the distillate to obtain the ethyl levulinate. The method can be used for solving an important bottleneck problem in the process of producing the ethyl levulinate from sugar, namely the hardening of un-reacted sugar; and the ethyl levulinate can be directly extracted from the alcoholysis solution of the sugar, the left distillation residue at last can outflow easily, and the distillation residue can be used as a boiler fuel to realize sufficient utilization of the material. And no hardening of the distillation residue can be used for effectively inhibiting the coking of the un-reacted biomass.

Description

technical field [0001] The invention relates to ethyl levulinate, in particular to a method for separating and extracting ethyl levulinate from biomass sugar alcoholysis reaction liquid. Background technique [0002] Ethyl levulinate is an important chemical raw material, because ethyl levulinate itself has a faint apple fragrance, and is currently used in edible spices and fruit preservatives. In addition, ethyl levulinate is also an excellent diesel oxygenator and biodiesel diluent, which can effectively improve the low-temperature flow properties of biodiesel such as cloud point, pour point and cold filter point, with a proportion of no more than 15vol%. Mixed with biodiesel, in line with American ASTM D6751 diesel standard. [0003] Chinese patent CN101619024 discloses a production process of ethyl levulinate, which includes catalyzing the esterification of levulinic acid in a large amount of ethanol with sulfuric acid at a temperature of 80°C to 120°C to synthesize eth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/716C07C67/62C07C67/54
Inventor 孙勇林鹿唐兴
Owner XIAMEN UNIV