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A method for preparing 4-vinylphenol by catalytic pyrolysis of gramineous biomass

A vinylphenol, 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 and the like, To achieve the effect of inhibiting pyrolysis reaction, reducing reaction energy barrier and improving selectivity

Active Publication Date: 2020-07-28
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 Patents(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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