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Adsorption separation method of aromatic aldehydes in lignin oxidation liquid

A technology of oxidizing liquid and adsorption separation, which is applied in chemical instruments and methods, separation/purification of carbonyl compounds, preparation of organic compounds, etc., to achieve high efficiency, easy regeneration, and good selectivity.

Active Publication Date: 2017-10-31
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

p-Hydroxybenzaldehyde, vanillin and syringaldehyde can be preliminarily separated from the lignin oxidation solution by using the adsorption of attapulgite, which has not been reported yet

Method used

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  • Adsorption separation method of aromatic aldehydes in lignin oxidation liquid
  • Adsorption separation method of aromatic aldehydes in lignin oxidation liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: Adsorption and separation of aromatic aldehydes according to the following steps

[0019] (1) Preparation of lignin oxidation solution: the corncob acid hydrolysis residue is added to the stainless steel reactor, and then NaOH and CuSO are added 4 , Make NaOH concentration 10%, catalyst CuSO 4 The concentration is 2%, oxygen gas is 1.0MPa, the stirring speed is 100rpm, the temperature is raised to 160°C, and the temperature is kept for 180 minutes and then cooled to room temperature. The pH value of the reaction solution is adjusted to 5 with 10% sulfuric acid to obtain the lignin oxidation solution;

[0020] (2) Attapulgite adsorption and separation of aromatic aldehydes: The attapulgite was burned in a muffle furnace at 500°C for 4 hours and then cooled to room temperature; then the attapulgite was added to the lignin oxidation solution at a liquid-solid ratio of 50:1. Place on a shaker, 200r / min, 30°C shaking for 1 min, then filter, take the filter cake; mix the...

Embodiment 2

[0022] Example 2: Adsorption and separation of aromatic aldehydes according to the following steps

[0023] (1) Preparation of lignin oxidation solution: add the residue of enzymatic hydrolysis of corn stalk into a stainless steel reactor, and then add NaOH and CuSO 4 , Make NaOH concentration 5%, catalyst CuSO 4 The concentration is 0.5%, oxygen is fed into 0.5MPa, the stirring speed is 300rpm, the temperature is raised to 200°C, the temperature is kept for 60 minutes and then cooled to room temperature, the pH value of the reaction solution is adjusted to 6 with 10% hydrochloric acid to obtain the lignin oxidation solution;

[0024] (2) Attapulgite adsorption and separation of aromatic aldehydes: The attapulgite is burned in a muffle furnace at 700°C for 4 hours and then cooled to room temperature; then the attapulgite is added to the lignin oxidation solution at a liquid-solid ratio of 100:1, Place on a shaker, 200r / min, 30°C shaking for 10min, then filter, take the filter cake; ...

Embodiment 3

[0025] Example 3: Adsorption and separation of aromatic aldehydes according to the following steps

[0026] (1) Preparation of lignin oxidation solution: the acid hydrolysis residue of wheat straw stalk is put into a stainless steel reactor, and then NaOH and CuSO are added. 4 , Make NaOH concentration 8%, catalyst CuSO 4 The concentration is 1%, oxygen gas is 0.8MPa, the stirring speed is 200rpm, the temperature is increased to 180°C, and the temperature is kept for 120 minutes and then cooled to room temperature. The pH value of the reaction solution is adjusted to 5.5 with 10% phosphoric acid to obtain the lignin oxidation solution;

[0027] (2) Attapulgite adsorption and separation of aromatic aldehydes: The attapulgite is burned in a muffle furnace at 600°C for 4 hours and then cooled to room temperature; then the attapulgite is added to the lignin oxidation solution at a liquid-solid ratio of 75:1. Place on a shaker, 200r / min, 30℃ shaking for 5min, then filter, take the filter...

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Abstract

The invention discloses a method for adsorptive separation of aromatic aldehyde in lignin oxidized liquid.Lignocellulose rich in lignin is adopted as a raw material, and after a wet process catalytic oxidation reaction, the lignin oxidized liquid is prepared; the pH value of the lignin oxidized liquid is adjusted to be slightly acidic, and attapulgite is adopted for adsorptive separation of the aromatic aldehyde compound in the lignin oxidized liquid; finally eluent is used for eluting the aromatic aldehyde compound adsorbed on the attapulgite away, and preliminary separation of the aromatic aldehyde compound from a lignin catalytic oxidation degradation product is achieved.Adsorption is achieved through the attapulgite, p-hydroxy benzaldehyde, vanillic aldehyde and syringaldehyde with commercial value are preliminarily separated from the lignin catalytic oxidation degradation product, and the separation and extraction process of the lignin degradation product is simplified.

Description

Technical field [0001] The invention belongs to the technical field of biomass chemical industry, and specifically relates to a method for adsorption and separation of aromatic aldehydes in lignin oxidation liquid. Background technique [0002] The lignin in lignocellulosic raw materials can be degraded into low molecular weight chemicals such as vanillin, benzene, phenol and their homologs through solvolysis. The low-molecular products of lignin after oxidative degradation include p-hydroxybenzaldehyde, vanillin, syringaldehyde, guaiacol, acetvanillone and acetyl syringone, among which three main aromatic aldehydes account for more than 90%. However, their physical and chemical properties are very similar, and separation is very difficult. Applying the principle of the reaction of sodium bisulfite and aldehyde compounds to produce water-soluble sodium bisulfite adducts, the aldehyde compounds in the reactants are separated from other components, but they also need to be further...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/32C07C45/79C07C47/565C07C47/58C07C47/575
CPCC07C45/32C07C45/79C07C47/565C07C47/58C07C47/575
Inventor 吴真胡磊贺建龙朱安峰穆飞虎
Owner HUAIYIN TEACHERS COLLEGE
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