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Method for preparing levulinic acid from steam explosion produced straw short fiber by adding polymerization inhibitor and performing solid acid catalysis

A technology of solid acid catalysis and levulinic acid, which is applied in the preparation of carboxylates, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of limiting the yield of levulinic acid, improve the overall utilization rate, and reduce production Cost, the effect of reducing distillation energy consumption

Inactive Publication Date: 2012-09-19
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In addition, the process of preparing levulinic acid will be accompanied by some side reactions, which mainly include the oxidative decomposition of cellulose itself and the oxidative polymerization of intermediates such as glucose and hydroxymethylfurfural during the reaction process. Through these side reactions reaction, cellulose is degraded to produce some insoluble humic acid substances, which limits the improvement of the yield of levulinic acid catalyzed by cellulose

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: get the dried rice straw and grind and cut it, carry out steam explosion treatment under the condition of 1.5MPa, 6min, mechanically comb, sieve and collect short fiber components between 40-80 mesh, in the cellulase addition: 4FPU / g substrate, solid-to-liquid ratio 1:20, temperature 45°C, after pre-enzymolysis for 2 hours, weigh 5.0g short fiber and put it into the reaction kettle, add 0.5% polymerization inhibitor p-hydroxyanisole, add 100ml Distilled water, after mixing, add 2.5% solid acid catalyst S to the reaction kettle 2 o 8 2- / ZrO 2 -SiO 2 -Sm 2 o 3 , covered and sealed, and the reactor was heated from room temperature to 160°C within 30 minutes to catalyze the preparation of levulinic acid under stirring. After 5 minutes of reaction, it was cooled and filtered, and the content of levulinic acid was determined to be 14.0% by high-pressure liquid phase method.

Embodiment 2

[0025] Embodiment 2: Get the dried rice straw and grind and cut it, carry out steam explosion treatment under the condition of 2MPa, 4min, mechanically comb, sieve and collect short fiber components between 40-80 mesh, take 4.0g short fiber and put it into In the reaction kettle, add 1.0% polymerization inhibitor p-hydroxyanisole, add 120ml distilled water, add 2.0% solid acid catalyst S to the reaction kettle after mixing 2 o 8 2- / ZrO 2 -SiO 2 -Sm 2 o 3 , Covered and sealed, under stirring, the reactor was heated from room temperature to 180°C within 10 minutes to catalyze the preparation of levulinic acid, and after 8 minutes of reaction, it was cooled and filtered, and the content of levulinic acid was determined to be 13.1% by high-pressure liquid phase method.

Embodiment 3

[0026]Embodiment 3: get the dried rice straw and grind and cut it, carry out steam explosion treatment under the condition of 0.5MPa, 7min, mechanically comb, sieve and collect short fiber components between 40-80 mesh, in the cellulase addition: 3FPU / g substrate, solid-to-liquid ratio 1:17, temperature 50°C, after pre-enzymolysis for 6 hours, weigh 4.0g short fiber and put it into the reaction kettle, add 1.5% polymerization inhibitor p-hydroxyanisole, add 180ml Distilled water, after mixing, add 1.5% solid acid catalyst S to the reaction kettle 2 o 8 2- / ZrO 2 -SiO 2 -Sm 2 o 3 , Covered and sealed, under stirring, the reactor was heated from room temperature to 220°C within 20 minutes to catalyze the preparation of levulinic acid. After 20 minutes of reaction, it was cooled and filtered, and the content of levulinic acid was determined to be 18.0% by high-pressure liquid phase method.

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PUM

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Abstract

The invention discloses a method for preparing levulinic acid from steam explosion produced straw short fiber by adding polymerization inhibitor and performing solid acid catalysis. The method comprises the steps of using the straw short fiber which is produced by the steam explosion, performing hydrolysis to the straw short fiber tissue by using solid acid catalyst instead of liquid acid to obtain intermediate products such as hexose and the like, then dehydrating the hexose to obtain hydroxymethyl furfural, and finally performing ring opening and hydration to hydroxymethyl furfural to obtain the levulinic acid. The polymerization inhibitor of p-hydroxyanisole is added after optimization of conditions and pre-enzymolysis. The yield of levulinic acid reaches 25.2%, and the yield is 68.7 % of the theoretical yield. The reaction condition of the method is mild, and the catalyst shows high activity. The product does not contain inorganic acid, so that the product does not produce a lot of waste residue and corrode equipment. The catalyst can be separated from raw materials and the product easily, and accords with today's chemical industry green development direction. And also, the whole straw is no longer low-value used. Instead, the long fiber and the short fiber of the straw are separated to carry out stratified multistage directional transformation to achieve the diversification of straw products and high-value utilization of resource.

Description

technical field [0001] The invention belongs to the field of resource utilization of lignocellulosic biomass raw materials, and in particular relates to a method for refining levulinic acid from straws. Background technique [0002] Levulinic acid (also known as 4-oxopentanoic acid, levotranic acid or valeric acid) is an important chemical raw material, and its structure is: CH 3 COCH 2 CH 2 COOH, which contains a carbonyl group and a carboxyl group in its molecule, has both the reaction characteristics of ketone and acid, and has good reactivity. It can perform various reactions such as esterification, substitution, redox, and polymerization. Its 4-position carbon The atom is an asymmetric carbon atom, so chiral synthesis and resolution are also possible. Taking advantage of these characteristics, levulinic acid can be widely used in chiral reagents, bioactive materials, polymers, adsorbents, lubricants, coatings, batteries, inks, electronic products and other fields. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/185C07C51/00C12P7/40
CPCY02P20/584
Inventor 陈洪章马力通于彬
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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