Method for preparing phenolic chemicals through thermo-chemical conversion of industrial lignin

An industrial lignin and thermochemical conversion technology, which is applied in the field of industrial lignin thermochemical conversion to prepare phenolic chemicals, can solve the problems of high equipment requirements, constant, high energy consumption, etc., and achieve simple recovery process and wide sources , the effect of reducing production costs

Inactive Publication Date: 2011-09-07
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The experimental results prove that although the lignin liquefaction yields obtained by different liquefaction methods are different, the yields and chemica...

Method used

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  • Method for preparing phenolic chemicals through thermo-chemical conversion of industrial lignin
  • Method for preparing phenolic chemicals through thermo-chemical conversion of industrial lignin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A component:

[0043] Acid-precipitated lignin from papermaking black liquor 100g

[0044] Aluminosilicate 5 g

[0045]Tetrahydronaphthalene 7 g

[0046] B component:

[0047] Glycerin 300 g

[0048] Dry the acid-precipitated lignin in the papermaking black liquor in an oven at 60°C for 8 hours to remove residual moisture, then mix it with other components of the above-mentioned A component and B component in the reactor, and reflux at 230°C for reaction After 1 hour, a heat conversion liquefied product was obtained.

[0049] Pour 60 parts of a mixture of dioxane and water with a volume ratio of 1:3 into the above thermochemical liquefaction product. Stir evenly and then centrifuge (5000 rev / min), and get the upper layer and the lower layer after standing and stratifying; the lower layer is glycerol solvent, which is recycled after vacuum distillation; the upper layer is phenolic chemicals and di The mixture of dioxane / water was removed by rotary evaporation to ob...

Embodiment 2

[0052] A component:

[0053] 100 grams of alkali lignin in papermaking black liquor

[0054] Aluminosilicate 4 g

[0055] Phenol 3 g

[0056] B component:

[0057] Glycerin 450 g

[0058] Dry the alkali lignin in the above weight parts of papermaking black liquor in an oven at 80°C for 8 hours to remove residual moisture, mix it with other components in the reactor, and react at 200°C for 0.5 hour to obtain thermal conversion liquefied product.

[0059] Pour 80 parts of a mixture of dioxane and water with a volume ratio of 1:6 into the above thermochemical liquefaction product. Stir evenly and then centrifuge (5000 rev / min), and get the upper layer and the lower layer after standing and stratifying; the lower layer is glycerol solvent, which is recycled after vacuum distillation; the upper layer is phenolic chemicals and di The mixture of dioxane / water was removed by rotary evaporation to obtain phenolic chemicals.

[0060] According to the GC-MS internal standard quant...

Embodiment 3

[0062] A component:

[0063] 100 grams of lignosulfonate in papermaking black liquor

[0064] Silicophosphoric acid 3 g

[0065] Phenol 5 g

[0066] B component:

[0067] Glycerin 400 g

[0068] Dry the lignosulfonate in the papermaking black liquor in an oven at 60°C for 8 hours to remove residual moisture, then mix it with other components in component A and component B in the reactor, and react at 230°C After 1 hour, a heat conversion liquefied product was obtained.

[0069] Pour 100 parts of a mixture of dioxane and water with a volume ratio of 1:10 into the above thermochemical liquefaction product. Stir evenly and then centrifuge (5000 rev / min), and get the upper layer and the lower layer after standing and stratifying; the lower layer is glycerol solvent, which is recycled after vacuum distillation; the upper layer is phenolic chemicals and di The mixture of dioxane / water was removed by rotary evaporation to obtain phenolic chemicals.

[0070] According to the GC...

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Abstract

The invention provides a method for preparing phenolic chemicals through the thermo-chemical conversion of industrial lignin. The method is as follows: under the common functions of solid acid catalyst and hydrogen supply solvent, industrial lignin performs atmospheric thermo-chemical conversion in high boiling point organic reaction medium to prepare homogeneous low molecular weight organic matter with rich phenolic compounds such as phenol, methoxyphenol, dimethoxyphenol and 2-methoxy-4-methylphenol, and the organic reaction medium is recycled through the technologies such as vacuum distillation. The method has simple process, good stability and low production cost; and the yield of the prepared phenolic compounds is more than 54%. The method plays an important role in the high-valued comprehensive utilization of the renewable resource, namely ndustrial lignin; and the converted phenolic chemicals can be used to synthesize phenolic resin, prepare high efficiency cement water-reducing agent and further separate, purify and prepare bio-chemicals. Particularly, by adopting the method, the lignin in papermaking black liquid and preparation residue of biological fuel ethanol prepared from cellulose can be converted to phenolic chemicals; and the method has wide application prospect.

Description

technical field [0001] The invention relates to a method for preparing phenolic chemicals from lignin, in particular to a method for preparing phenolic chemicals through industrial lignin thermochemical conversion. Background technique [0002] Lignin is one of the components of plant fiber raw materials, its content is second only to cellulose, and it is a natural aromatic polymer with a three-dimensional network structure. There are active groups such as hydroxyl, carbonyl, aromatic, methoxy, and conjugated double bonds in lignin molecules, which can realize various chemical reactions. However, the utilization of lignin is not very sufficient at present. [0003] The method of thermochemical conversion of lignin into phenolic chemicals is a technology that can realize the thermochemical conversion of lignin under normal pressure and the action of a catalyst to prepare chemical raw materials. It has the advantages of no need for pressure-resistant equipment, relatively lo...

Claims

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Application Information

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IPC IPC(8): C07C37/54C07C39/04C07C39/06C07C41/01C07C43/23
CPCY02P20/52
Inventor 武书彬隋鑫金
Owner SOUTH CHINA UNIV OF TECH
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