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Method for preparing vanillin through catalytic oxidation degradation of lignin

A catalytic oxidation and oxidative degradation technology, applied in the field of lignin degradation, can solve problems such as difficult recycling and secondary pollution, and achieve good reusability, easy recycling, and mild reaction conditions

Active Publication Date: 2016-01-13
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, copper sulfate has attracted much attention because of its good catalytic activity and low cost, but its recovery is difficult and it is easy to cause secondary pollution

Method used

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  • Method for preparing vanillin through catalytic oxidation degradation of lignin
  • Method for preparing vanillin through catalytic oxidation degradation of lignin
  • Method for preparing vanillin through catalytic oxidation degradation of lignin

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Preparation of solid catalyst heteropolyacid K 6 [Co Ⅱ W 12 O40]·16H 2 O, the steps are as follows: Na 2 WO 4 2H 2 O (19.8g) was dissolved in 40mL deionized water, adjusted to pH=7 with glacial acetic acid to obtain solution A, (CH 3 CO 2 ) 2 Co 4H 2 O (2.5g) was dissolved in 12mL deionized water to obtain solution B; put solution A in a flask, boil in an oil bath, slowly add solution B preheated at 80°C and stir to produce a black-green solution, boil for 20min Then filter while hot. The saturated CH at pH=7 3 Slowly add COOK solution (20mL) to the filtrate, stir to produce a green solid, cool to room temperature and filter, wash the solid twice with the filtrate, dissolve the solid in 40mL of 2M sulfuric acid solution, stir at 50°C for 15min, a dark blue solution is produced, filter to obtain Filtrate C, concentrate and crystallize to get K 6 [Co Ⅱ W 12 O40]·16H 2 O solid heteropolyacids.

Embodiment 2

[0034] Preparation of solid catalyst heteropolyacid K 5 [Co Ⅲ W 12 o 40 ]·20H 2 O: On the basis of Example 1, heat liquid C to boiling, and add K in batches 2 S 2 o 8 (10g), after the solution turns from blue to yellow, stop heating, and cool in an ice bath to obtain yellow needle-like crystals, filter to obtain K 5 [Co Ⅲ W 12 o 40 ]·20H 2 O solid heteropolyacids.

Embodiment 3

[0036] Preparation of solid catalyst heteropolyacid H 6 [Co Ⅱ W 12 o 40 ]·2.5H 2 O: Na 2 WO 4 2H 2 O (1.0g), CoCl 2 ·6H 2 O (0.1g), (CH 3 CO 2 ) 2 Co 4H 2 O (0.12g), 1,3-propanediamine (0.06g) were mixed and dissolved in 15mL of water, stirred for 1 hour, adjusted to pH=2 with 6M HCl, moved to a reaction kettle, and reacted at 160°C for 4 days to prepare Get H 6 [Co Ⅱ W 12 o 40 ]·2.5H 2 O solid heteropolyacid.

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Abstract

The invention discloses a method for preparing vanillin through catalytic oxidation degradation of lignin. The method comprises the steps that the lignin and a solid acid catalyst are mixed, solvent is added, oxidation degradation is performed on the lignin under the condition of the oxygen pressure ranging from 1 MPa to 3 MPa, and then single aromatic compounds taking the vanillin as the main component, wherein heteropolyacid and heteropolyacid salt of the heteropolyacid or hydrates of the heteropolyacid are adopted as the solid acid catalyst, and any one or several of K6[Co<II>W12O40], H6[Co<II>W12O40], K5[Co<III>W12O40], (NH4)[3CoMo6O24H6] and H3PW12O40 is / are adopted as the heteropolyacid. According to the method, aromatic hydrocarbon compounds are the main products, the vanillin selectivity is up to 50-70 percent, and the yield reaches 0.5-6.4 percent; the oxidation degradation reaction of the lignin is mild in condition, green and safe, and the catalyst is convenient to recycle, high in recycling rate and good in recycling performance.

Description

technical field [0001] The invention belongs to the technical field of lignin degradation, and in particular relates to a method for preparing vanillin by catalytic oxidation degradation of lignin. Background technique [0002] Lignin is the second largest natural polymer in the plant kingdom after cellulose. It is an amorphous three-dimensional network-like aromatic polymer compound mainly composed of phenylpropane-based structural units (C9), accounting for 10% of the quality of lignocellulosic biomass. 15-30%, is the only non-petroleum resource in nature that can provide renewable aromatic compounds. The phenylpropanyl C9 structural unit of lignin mainly includes guaiacyl, syringyl and p-hydroxyphenyl, which can be degraded into monoaromatic or aliphatic organic compounds under appropriate conditions, such as vanillin and syringaldehyde Wait. However, the structure of lignin is complex and the bond types such as C-C and C-O that constitute its unit structure are relativ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/51C07C45/27C07C47/58
CPCC07C45/27C07C45/51C07C47/58Y02P20/584
Inventor 应汉杰胡甜朱晨杰刘铖陈勇吴菁兰庄伟陈晓春
Owner NANJING TECH UNIV