Method of preparing levulinic acid via hemicellulose

A technology of hemicellulose and levulinic acid, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of increased energy consumption by multi-stage hydrolysis, difficult separation of subsequent products, safety and environmental protection. hidden dangers and other problems, to achieve the effects of easy separation, recycling, and catalytic effect.

Inactive Publication Date: 2019-03-01
ZHEJIANG HUAKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent with the publication number CN108675928A discloses a method for directly preparing levulinate from furfural, by using furfural as raw material and lower alkanol as the reaction medium, the combination of loaded molecular sieve ZrO2 / MCM and ion exchange resin Amberlyst-15 As a catalyst to prepare levulinate, the disadvantage of this technology is that the raw materials used are highly toxic, and there are hidden dangers in terms of safety and environmental protection
The Chinese patent of publication number CN104311411A discloses the method technology of preparing levulinic acid by multi-stage acid hydrolysis, uses inorganic acid as catalyst, adopts multi-stage hydrolysis, hydrolyzes cellulose component, prepares levulinic acid product, the shortcoming of this technology is: preparation There are many by-products in the product, the operation is complicated, the energy consumed by multi-stage hydrolysis is increased, the cost is high, the subsequent products are difficult to separate, and the purity is reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The first method of synchronous saccharification and fermentation of the present invention to prepare cellulosic ethanol, this embodiment comprises the following steps:

[0044] (11) Screen 200 mesh hemicellulose.

[0045] (12) Weigh 100 g of the hemicellulose prepared in step (11), and prepare a hemicellulose solution with a concentration of 15% with a two-phase solvent.

[0046] (13) Add the prepared hemicellulose liquid to the reaction kettle, and add 5% formic acid, acetic acid and ferric chloride mixed solution, 1% tin porous carbon-based solid acid catalyst, and 0.5% Raney nickel-alumina in sequence -ZSM5 catalyst, 0.3% Au-ZrO 2 - SBA15 catalyst.

[0047] (14) Stir at a constant speed of 100r / min. At the same time, adjust the temperature of the solution in the reactor at 110°C and maintain it for 0.5h; then adjust the temperature of the solution in the reactor at 160°C and maintain it for 3.0h; then adjust The temperature of the solution in the reaction kettle ...

Embodiment 2

[0051] The second method of synchronous saccharification and fermentation of the present invention for preparing cellulosic ethanol, this embodiment comprises the following steps:

[0052] (21) Screen 400 mesh hemicellulose.

[0053] (22) Weigh 100 g of the hemicellulose prepared in step (1), and prepare a hemicellulose solution with a concentration of 25% with a two-phase solvent.

[0054] (23) Add the prepared hemicellulose liquid to the reaction kettle, and add 10% formic acid, acetic acid and ferric chloride mixed solution, 5% tin porous carbon-based solid acid catalyst, and 1.0% Raney nickel-alumina in sequence -ZSM5 catalyst, 0.8% Au-ZrO 2 - SBA15 catalyst.

[0055] (24) Stir at a constant speed of 150r / min. At the same time, adjust the temperature of the solution in the reactor at 125°C and maintain it for 2.0 hours; then adjust the temperature of the solution in the reactor at 180°C and maintain it for 6.0 hours; then adjust The temperature of the solution in the re...

Embodiment 3

[0059] The third method for preparing cellulosic ethanol by synchronous saccharification and fermentation of the present invention, this embodiment includes the following steps:

[0060] (31) Screen 300 mesh hemicellulose.

[0061] (32) Weigh 100 g of the hemicellulose prepared in step (1), and prepare a hemicellulose solution with a concentration of 20% with a two-phase solvent.

[0062] (33) Add the prepared hemicellulose solution into the reaction kettle, and then add 8% formic acid, acetic acid and ferric chloride mixed solution, 3% tin porous carbon-based solid acid catalyst, and 0.8% Raney nickel-alumina -ZSM5 catalyst, 0.5% Au-ZrO 2 - SBA15 catalyst.

[0063] (34) Stir at a constant speed of 130r / min. At the same time, adjust the temperature of the solution in the reactor at 120°C and maintain it for 1.0h; then adjust the temperature of the solution in the reactor at 170°C and maintain it for 4.5h; then adjust The temperature of the solution in the reaction kettle is...

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Abstract

The invention relates to a method of preparing levulinic acid via hemicellulose. The method comprises the steps of screening hemicellulose which is 200-400 mesh, preparing hemicellulose liquid havinga concentration of 15-25% with a dual-water-phase solvent, adding the prepared hemicellulose liquid into a reactor, adding 5-10% of a mixed solution of formic acid, acetic acid and iron chloride, 1-5%of a tin porous carbon-based solid acid catalyst, 0.5-1.0% of Raney nickel-alumina-ZSM5 catalyst, and 0.3-0.8% of Au-ZrO2-SBA15 catalyst, stirring while temperatures are controlled in different periods of time, introducing hydrogen for a period of time, holding the set temperature for a period of time, and preparing to obtain levulinic acid solution. few byproducts occur to the preparation of levulinic acid; subsequent separation and purification are simple; the yield of levulinic acid is increased; one-step preparation of levulinic acid by hemicellulose is achieved.

Description

technical field [0001] The invention relates to a method for preparing levulinic acid from hemicellulose. Background technique [0002] Levulinic acid is one of the important products produced by biomass hydrolysis, and it is also an important platform compound and chemical raw material. In industry, levulinic acid is difficult to be directly produced by organic synthesis, and is usually obtained through biomass conversion. [0003] At present, there are two main production routes of levulinic acid: the first one is the synthetic route of furfuryl alcohol catalytic hydrolysis. Using pentosan as raw material, it is first converted into furfural by cracking, and then furfural is hydrogenated to generate furfuryl alcohol. Under acid catalysis, furfuryl alcohol generates levulinic acid through hydrolysis, ring opening and rearrangement reactions. The second is: biomass direct hydrolysis synthetic approach. Using biomass six-carbon sugar as raw material, levulinic acid is di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/185C07C51/00B01J23/14B01J29/46B01J29/04
CPCC07C51/00B01J23/002B01J23/14B01J29/043B01J29/46C07C59/185
Inventor 张金建陈德水李勉程新平杨世辉黄涛丁士友
Owner ZHEJIANG HUAKANG PHARMA
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