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Method for preparing and separating p-hydroxybenzaldehyde, vanillin and syringaldehyde from lignin

A technology of p-hydroxybenzaldehyde and syringaldehyde, which is applied to the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as lack of industrial application, difficulty in recycling, secondary pollution, etc., and achieve improvement Comprehensive utilization rate, large economic and social significance, and the effect of high-efficiency catalytic activity

Inactive Publication Date: 2011-07-06
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the catalysts used for the catalytic oxidation of lignin mainly include noble metal catalysts and transition metal-based catalysts. The former is limited in practical application due to its high cost, and the latter mainly includes copper sulfate and some salts of transition metal ions. Among them Copper sulfate has attracted much attention due to its high activity, but it is difficult to recycle and easily produce secondary pollution, so it has not been used in industry so far.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment one: a kind of method utilizing lignin to prepare and separate p-hydroxybenzaldehyde, vanillin, syringaldehyde comprises the following process steps:

[0026] (1), preparation of LaFe 0.9 Cu 0.1 o 3 catalyst:

[0027] a, lanthanum nitrate in molar ratio: ferric nitrate: copper nitrate=1: 0.9: 0.1 takes by weighing nitrate;

[0028] B, dissolving nitrate in water makes nitrate solution, the mass concentration of nitrate total amount in aqueous solution is 20%;

[0029] C, in nitrate solution, add citric acid and make complexing agent solution, the mol ratio of metal ion total amount in citric acid and nitrate solution is 1: 1.5;

[0030] d. Add dropwise ammonia water with a concentration of 10% to the complexing agent solution to adjust the pH value of the complexing agent solution to 5, and stir and heat the complexing agent solution after adding ammonia water to obtain a wet gel; the heating temperature is 80°C , the stirring speed is 200 rpm, and the s...

Embodiment 2

[0040] Embodiment two: a kind of method utilizing lignin to prepare and separate p-hydroxybenzaldehyde, vanillin, and syringaldehyde comprises the following process steps:

[0041] (1) Preparation of LaCo 0.1 Cu 0.9 o 3 catalyst:

[0042] a, lanthanum nitrate by molar ratio: cobalt nitrate: copper nitrate=1: 0.1: 0.9 takes by weighing nitrate;

[0043] B, dissolving nitrate in water makes nitrate solution, the mass concentration of nitrate total amount in aqueous solution is 30%;

[0044] C, in nitrate solution, add citric acid and make complexing agent solution, the mol ratio of metal ion total amount in citric acid and nitrate solution is 1: 2;

[0045] d. Add dropwise ammonia water with a concentration of 30% in the complexing agent solution to adjust the pH value of the complexing agent solution to 6, and stir and heat the complexing agent solution after adding ammonia water to obtain a wet gel; the heating temperature is 100°C , the stirring speed is 500 rpm, and the...

Embodiment 3

[0055] Embodiment three: a kind of method utilizing lignin to prepare and separate p-hydroxybenzaldehyde, vanillin, and syringaldehyde comprises the following process steps:

[0056] (1) Preparation of LaMn 0.5 Cu 0.5 o 3 catalyst:

[0057] a, lanthanum nitrate by molar ratio: ferric nitrate: copper nitrate=1: 0.5: 0.5 takes by weighing nitrate;

[0058] B, dissolving nitrate in water makes nitrate solution, the mass concentration of nitrate total amount in aqueous solution is 25%;

[0059] C, in nitrate solution, add citric acid and make complexing agent solution, the mol ratio of metal ion total amount in citric acid and nitrate solution is 1: 1.8;

[0060] d. Add dropwise ammonia water with a concentration of 20% to the complexing agent solution to adjust the pH value of the complexing agent solution to 5, and stir and heat the complexing agent solution after adding ammonia water to obtain a wet gel; the heating temperature is 90°C , the stirring speed is 300 rpm, and ...

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Abstract

The invention relates to a method for preparing and separating p-hydroxybenzaldehyde, vanillin and syringaldehyde from lignin, which comprises the following steps: (1) preparing a Lab[1-x]Cu[x]O[3] perovskite type composite oxide catalyst; and (2) carrying out centrifugal separation on a crude aromatic aldehyde product, acidifying, carrying out vacuum drying, and extracting with trichloromethane to obtain a mixture of p-hydroxybenzaldehyde, vanillin and syringaldehyde; dissolving the mixture of p-hydroxybenzaldehyde, vanillin and mixture in anhydrous alcohol, adding ammonia water to form a precipitate, filtering, and regulating the pH value of an alcohol solution of the filtered solid with a sulphuric acid solution, thereby obtaining a crude syringaldehyde product; and concentrating the filtered liquid while depressurizing to obtain a solid, rectifying in a nitrogen atmosphere, and respectively collecting fractions at different temperatures, thereby obtaining the vanillin and p-hydroxybenzaldehyde. The invention increases the comprehensive utilization ratio of the wood fibers, lowers the cost of the wood fiber fuel alcohol, and has great economic and social meanings.

Description

technical field [0001] The invention relates to a method for preparing and separating p-hydroxybenzaldehyde, vanillin and syringaldehyde by utilizing lignin, and belongs to the technical field of biomass chemical industry. Background technique [0002] In order to alleviate the dual pressure of energy and environment in the future, countries all over the world attach great importance to the development and utilization of renewable resources, especially biomass resources. Biomass resources, as an ideal substitute for fossil resources such as petroleum and coal, have attracted widespread attention around the world. Biomass resources can be used as energy and processed into chemicals. Therefore, how to effectively convert biomass resources into energy and chemicals is one of the current research hotspots. Plant biomass is an important component of biomass resources, and its main components are cellulose, hemicellulose and lignin. Among them, cellulose and hemicellulose are the...

Claims

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Application Information

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IPC IPC(8): C07C45/32C07C47/565C07C47/58B01J23/83B01J23/889
Inventor 邓海波
Owner JIANGNAN UNIV
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