Method for preparing 4-vinylphenol through catalytic pyrolysis of gramineous biomass

A vinyl phenol, catalytic pyrolysis technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low heating rate, high production cost, low yield of 4-vinylphenol, etc. To achieve the effect of inhibiting pyrolysis reaction, lowering reaction energy barrier and improving selectivity

Active Publication Date: 2017-08-15
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent application number 200610042200.9 discloses a preparation method of 4-vinylphenol, which uses p-hydroxybenzaldehyde and malonic acid as raw materials, reacts in an alkaline catalyst and an aprotic polar organic solvent to obtain 4-vinylphenol phenol; this method not only requires high reaction conditions and reaction equipment, but also has a long reaction cycle and high production costs
[0004] Another document, China Patent Application No. 201110134872.3, reports a method for preparing 4-vinylphenol from biomass. Although this technology uses biomass pyrolysis to prepare 4-vinylphenol, the pyrolysis reaction time is longer and the temperature rises The rate is low, all have certain inhibition to the generation of 4-vinylphenol, make the productive rate of 4-vinylphenol in the organic liquid product that this method obtains is lower; The formation of other pyrolysis products other than 4-vinylphenol is effectively suppressed, so that the purity of 4-vinylphenol in the liquid product is also low, resulting in the difficulty and cost of 4-vinylphenol separation and purification.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Bagasse (0.1-0.3 mm in particle size) was used as the grass biomass raw material, soaked in 1.5% calcium hydroxide aqueous solution for 10 minutes, filtered, then dried the soaked raw material at 110 °C for 5 hours as the experimental raw material, hydrogenated The calcium loading was 0.9%.

[0020] Using a pyrolysis reaction device, the above-mentioned experimental raw materials (pretreated bagasse) and raw bagasse (unpretreated bagasse) were pyrolyzed at 250°C, the heating rate was greater than 800°C / s, and nitrogen atmosphere for 35s to obtain liquid products. Productive rate is 33.5% and 22.9%, wherein the content of 4-vinylphenol is analyzed by gas chromatography, calculates that the productive rate of 4-vinylphenol is 6.7% and 2.1%, and productive rate improves 219.0%; 4-vinylphenol The content of phenol in the organic liquid product (excluding water) is 38.9% and 30.4%, and the selectivity is increased by 28.0%.

Embodiment 2

[0022] Use bagasse (0.1-0.3 mm in particle size) as the gramineous biomass raw material, immerse it in 2.0% calcium hydroxide aqueous solution for 10 minutes and filter it, then dry the soaked raw material at 110°C for 10 hours as the experimental raw material, and oxidize The calcium loading was 1.2%.

[0023] Using a pyrolysis reaction device, the above-mentioned experimental raw materials (pretreated bagasse) and raw bagasse (unpretreated bagasse) were pyrolyzed at 270°C, the heating rate was greater than 1000°C / s, and nitrogen atmosphere for 40s to obtain liquid products. Productive rate is 36.7% and 34.6%, and the content of wherein 4-vinylphenol is analyzed by gas chromatography, calculates that the productive rate of 4-vinylphenol is 6.5% and 5.6%, and productive rate improves 16.1%; 4-vinylphenol The content of phenol in the organic liquid product (excluding water) is 33.4% and 29.7%, and the selectivity is increased by 12.5%.

Embodiment 3

[0025] Use bagasse (0.1-0.3mm in particle size) as the gramineous biomass raw material, soak it in 6.0% calcium hydroxide aqueous solution for 10 minutes and filter it, then dry the soaked raw material at 110°C for 5 hours as the experimental raw material, and oxidize The calcium loading was 4.2%.

[0026] Using a pyrolysis reaction device, the above-mentioned experimental raw materials (pretreated bagasse) and raw bagasse (unpretreated bagasse) were pyrolyzed at 290°C, the heating rate was greater than 800°C / s, and nitrogen atmosphere for 30s to obtain liquid products. The productive rate is 38.1% and 35.8%, and the content of 4-vinylphenol is analyzed by gas chromatography, calculates that the productive rate of 4-vinylphenol is 6.1% and 5.4%, and productive rate improves 13.0%; 4-ethylene The content of base phenol in the organic liquid product (excluding water) is 29.4% and 27.2%, and the selectivity is increased by 8.1%.

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Abstract

The invention belongs to the field of utilization of biomass energy, and concretely relates to a method for preparing 4-vinylphenol through catalytic pyrolysis of gramineous biomass. The method comprises the following steps: loading an alkaline catalyst onto gramineous biomass used as a raw material in an impregnation manner, carrying out catalytic pyrolysis at 230-350 DEG C in an inert atmosphere, and condensing the obtained pyrolysis gas to obtain a liquid product rich in the 4-vinylphenol. The yield of the 4-vinylphenol and the selectivity of the 4-vinylphenol in the organic liquid product are high. The method for preparing the 4-vinylphenol overcomes the defects of low content of the 4-vinylphenol in obtained bio-oil, poor selectivity and high separation and extraction cost of existing gramineous biomass pyrolysis liquefaction technologies, and has a very good application prospect.

Description

technical field [0001] The invention belongs to the field of utilization of biomass energy, and in particular relates to a method for preparing 4-vinylphenol by catalytic pyrolysis of gramineous biomass. Background technique [0002] 4-Vinylphenol is a colorless crystal with a phenol-like chemical and drug smell, and has a musty and meaty aroma. When diluted, it has a sweet and vanilla bean extract aroma. It is widely used in synthetic resins, inks , synthetic rubber, flavor formula, petroleum processing and pharmaceutical industries. [0003] Chinese patent application number 200610042200.9 discloses a preparation method of 4-vinylphenol, which uses p-hydroxybenzaldehyde and malonic acid as raw materials, reacts in an alkaline catalyst and an aprotic polar organic solvent to obtain 4-vinylphenol base phenol; this method not only requires high reaction conditions and reaction equipment, but also has a long reaction cycle and high production costs. [0004] Another document...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/00C07C39/20
CPCC07C37/004C07C39/20
Inventor 陆强叶小宁王昕郭浩强潘保霏董长青杨勇平
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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