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Method for separating formic acid and levulinic acid from hydrate molten salt

A technology for the separation of levulinic acid and separation methods, which is applied in the separation/purification of carboxylic acid compounds, chemical instruments and methods, and the preparation of organic compounds. Separation, separation of difficult separation methods and other problems, to achieve good self-catalysis ability, promote the production rate, and enhance the effect of protonation performance

Pending Publication Date: 2022-04-12
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent CN110963908A discloses a method for preparing levulinic acid based on cellulose hydrolysis of molten salt hydrate. Converting cellulose in MIBK / LiCl can obtain a levulinic acid yield of more than 91.2%, but due to the higher boiling point of levulinic acid High, good solubility in hydrate molten salt, difficult to separate by conventional separation methods
In this patent, it is difficult to separate the complexing agent and co-solvent, etc., and waste water is generated
[0010] In the prior art, when biomass is converted into levulinic acid, every molecule of levulinic acid is accompanied by a molecule of formic acid, and it is difficult to effectively separate the levulinic acid and formic acid contained in the biomass conversion liquid

Method used

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  • Method for separating formic acid and levulinic acid from hydrate molten salt
  • Method for separating formic acid and levulinic acid from hydrate molten salt
  • Method for separating formic acid and levulinic acid from hydrate molten salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) After the cellulose hydrolyzate is concentrated, the concentrated cellulose hydrolyzate is obtained, and 33g CaCl is added in 30.0g of the cellulose concentrated hydrolyzate 2 React with 14.8g of n-butanol at 60°C for 3.0 hours, wherein the concentrated cellulose hydrolyzate consists of 11.6g of levulinic acid, 2.0g of formic acid, 16.0g of water and 0.4g of other biomass hydrolysis by-products;

[0044] (2) After the reaction is completed, the temperature is lowered to 30° C., sedimentation and separation are carried out, and the organic phase is separated, and the mass of the organic phase is 28.1 g;

[0045] (3) the organic phase obtains butyl levulinate and butyl formate respectively through distillation, and the productive rate of butyl formate is 81.0wt.%, and the productive rate of butyl levulinate is 71.1wt.%; Chromatographic analysis, see the results Figure 5 , the two main peaks are as follows: 1, 8.57: butyl formate; 2, 21.587: butyl levulinate;

[004...

Embodiment 2

[0048] (1) After the cellulose hydrolyzate is concentrated, the concentrated cellulose hydrolyzate is obtained. Add 16.7g LiCl and 14.8g n-butanol to 30.0g of the cellulose concentrated hydrolyzate, and react at 80°C for 5.0h. Among them, the composition of the cellulose concentrated hydrolyzate 5.8g of levulinic acid, 2.0g of formic acid, 21.8g of water and 0.4g of other biomass hydrolysis by-products;

[0049] (2) After the reaction is completed, the temperature is lowered to 40° C., sedimentation separates the layers, and the organic phase is separated, and the mass of the organic phase is 22.4 g;

[0050] (3) The organic phase was distilled to obtain butyl levulinate and butyl formate respectively, the productive rate of butyl formate was 83.2wt.%, and the productive rate of butyl levulinate was 72.7wt.%.

[0051] (4) Butyl levulinate and butyl formate are hydrolyzed to obtain levulinic acid and formic acid respectively.

Embodiment 3

[0053] (1) After the cellulose hydrolyzate is concentrated, the cellulose concentrated hydrolyzate is obtained, and CaBr is added in 30.0 g of the cellulose concentrated hydrolyzate 2 49.0 g and 29.6 g of n-butanol were reacted at 90°C for 2.5 hours, wherein the cellulose concentrated hydrolyzate consisted of 11.6 g of levulinic acid, 4.6 g of formic acid, 13.3 g of water and 0.5 g of other biomass hydrolysis by-products;

[0054] (2) After the reaction is completed, the temperature is lowered to 40° C., sedimentation separates the layers, and the organic phase is separated, and the mass of the organic phase is 45.5 g;

[0055] (3) The organic phase was distilled to obtain butyl levulinate and butyl formate respectively, the productive rate of butyl formate was 81.0wt.%, and the productive rate of butyl levulinate was 73.1wt.%.

[0056] (4) Butyl levulinate and butyl formate are hydrolyzed to obtain levulinic acid and formic acid respectively.

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a method for separating formic acid and levulinic acid from hydrate molten salt. The method comprises the following steps: reacting under the coexistence of levulinic acid, formic acid and alcohol in hydrate molten salt, respectively reacting formic acid and levulinic acid with alcohol to generate formate and levulinic acid ester, and carrying out ester exchange on formate and levulinic acid to generate levulinic acid ester and formic acid, after the reaction is finished, the reaction liquid contains levulinic acid ester, formate, levulinic acid, formic acid and alcohol, separating the reaction liquid to obtain an organic phase, distilling the organic phase to respectively obtain levulinic acid ester and formate, and hydrolyzing to respectively obtain levulinic acid and formic acid. The method is simple in technological process, low in energy consumption and easy to separate, and the product can be spontaneously separated from the hydrate molten salt, so that the subsequent purification cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for separating formic acid and levulinic acid in hydrate molten salts. Background technique [0002] Biomass conversion to produce chemicals is the most promising high-value utilization method of biomass, which can partially replace fossil resources. Among the chemicals produced from biomass conversion, levulinic acid is considered as a high value-added chemical. Levulinic acid can be used to synthesize 1,4-pentanediol, 2-butanone, 2-methyltetrahydrofuran, 3-hydroxypropionic acid, 5-nonanone, angelica lactone, bisphenolic acid, glycerol ketal ester oligomerization substances, levulinate, succinic acid, valeric acid and valeric acid salts, gamma-valerolactone and delta-aminolevulinic acid, etc. Due to its high performance, high flash point and good fluidity, it can be used as gasoline and diesel additives and has attracted much attention. [0003] Levulinic a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/00C07C51/44C07C51/493C07C53/02C07C59/185C07C67/08C07C67/54C07C69/06C07C67/03C07C69/716
Inventor 崔洪友王景华王建刚张远李志合王鸣易维明
Owner SHANDONG UNIV OF TECH
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