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Method for preparing vanillin from straw lignin under normal pressure condition

A technology of straw lignin and vanillin is applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of organic compounds, etc. Mild and controllable, the effect of solving the complex high temperature and high pressure equipment and reducing environmental pollution

Pending Publication Date: 2021-12-10
JILIN AGRICULTURAL UNIV
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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing vanillin from corn stalk lignin under normal pressure, which can effectively solve the technical problems of complex high-temperature and high-pressure equipment for preparing vanillin and harsh reaction conditions; at the same time , using corn stalk lignin as raw material, on the one hand, it can reduce the environmental pollution caused by straw burning, on the other hand, it provides a new idea for the resource utilization of straw, which has good economic and social significance

Method used

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  • Method for preparing vanillin from straw lignin under normal pressure condition
  • Method for preparing vanillin from straw lignin under normal pressure condition

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Embodiment 1

[0022] Add 2g of corn stalk alkali lignin (you can buy it directly, or extract it yourself by corn stalk alkaline process), add 50mL of 1mol / L NaOH solution, add 0.2g of CuSO 4 As a catalyst, it is catalyzed in a three-necked flask of 500ml, a magnetic stirrer is placed in the three-necked flask, a condensation device is installed on the three-necked flask, and the three-necked flask is placed on the magnetic stirrer (see figure 1 ), the number of revolutions is 250rpm, in a 90°C constant temperature water bath with H 2 o 2 Oxidation; use a syringe to add 10mL H 2 o 2 , add 10mL H after 1h 2 o 2 , the oxidation time is 2 hours. After 2 hours, the temperature of the water bath drops to 70°C. Measure an appropriate volume of 0.1mol / LH 2 SO 4 The solution was poured into a three-necked flask, refluxed for 0.5 h, and the pH of the reaction system was adjusted to acidic (pH 1-2). After the reaction, the solution in the three-necked flask was cooled to room temperature, extra...

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Abstract

The invention relates to a method for preparing vanillin from straw lignin under normal pressure condition. The method comprises the following steps: step S1, adding corn straw alkali lignin, NaOH solution and CuSO4 into three flasks, placing magnetic stirrers in the three flasks, and installing condensing devices on the three flasks; s2, placing the three flasks on magnetic stirrer devices, and oxidizing with H2O2 in a water bath at the constant temperature of 80-90 DEG C; adding H2O2 in at least two batches by using an injector during oxidation; s3, measuring an H2SO4 solution, pouring the H2SO4 solution into the three flasks, refluxing, and adjusting the pH value of a reaction system to be acidic; and S4, cooling the solution in the three flasks to room temperature, extracting by using an organic solvent, combining the extract phases, and concentrating under reduced pressure to obtain a vanillin-containing product. The method can effectively solve the technical problems of complex high-temperature and high-pressure equipment and harsh reaction conditions of the existing vanillin preparation method.

Description

technical field [0001] The invention belongs to the field of recycling and reuse of corn stalks, and in particular relates to a method for preparing vanillin from straw lignin under normal pressure. Background technique [0002] Vanillin is known as the "king of food spices" because of its unique vanilla smell and strong milky aroma, and is widely used in food, daily chemical, medicine, agriculture and other fields. [0003] Lignin has been considered as a potential biorefinery raw material for the production of value-added chemicals (including vanillin and its derivatives). 80-85% of synthetic vanillin in the market is produced from petroleum derivative guaiacol, and only 20-15 About % is produced with lignin as raw material. The preparation of vanillin from lignin usually adopts a high-pressure reaction process. For example, Liu Chao put lignin and sodium hydroxide solution into an autoclave at a certain ratio in "A New Method for Preparation of Vanillin from Lignin", and...

Claims

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Application Information

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IPC IPC(8): C07C47/58C07C45/00C07C45/80
CPCC07C45/00C07C45/80C07C47/58
Inventor 汪树生胡恒苏玉春陈光朱学军李艳慧易南琛
Owner JILIN AGRICULTURAL UNIV
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