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Method for preparing 4-ethyl-2-metoxyphenol by catalytic pyrolysis of biomass

A methoxyphenol, catalytic pyrolysis technology, applied in chemical instruments and methods, physical/chemical process catalysts, ether preparation, etc., can solve the problems of complex extraction process steps, waste liquid that is difficult to handle, and uneconomical, etc. It achieves the effects of simple composition, low requirements for equipment and reaction conditions, and reduced production costs

Active Publication Date: 2015-03-25
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction process of this method has many and extremely complicated steps, and various acids, alkalis and organic solvents need to be used in the extraction process, and the waste liquid is more difficult to handle.
In general, pyrolyzing biomass first to obtain conventional bio-oil (composition is extremely complex), and then extracting 4-ethyl-2-methoxyphenol from complex bio-oil is not only technically complicated, but not very economical , and the waste liquid produced is easy to pollute the environment

Method used

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  • Method for preparing 4-ethyl-2-metoxyphenol by catalytic pyrolysis of biomass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 0.50 g of palladium nitrate dihydrate (Pd(NO 3 ) 2 ·2H 2 O) Dissolve in 100mL deionized water, stir until completely dissolved, add 8.00g MCM-41 to the solution, slowly drop ammonia water (25%) into the mixture under stirring until the pH value reaches 10, then continue Stir at room temperature for 12 h. After stirring, the solid was filtered, dried at 100°C for 3h, and then reduced in a hydrogen atmosphere (6% hydrogen and nitrogen as protective gas) at 280°C for 3h (programmed temperature was 2°C / min). 8.01 g of Pd / MCM-41 were obtained with a Pd loading of 2%.

[0027] Take 2g of the above catalyst, grind to a particle size of less than 0.5mm, take 10g of larch wood as a raw material, grind to a particle size of less than 0.3mm, mechanically mix the two, and rapidly pyrolyze them for 20s at 290°C under a nitrogen atmosphere. The content of 4-ethyl-2-methoxyphenol was analyzed by gas chromatography, and the yield of 4-ethyl-2-methoxyphenol was calculated to b...

Embodiment 2

[0029] Get 5g of catalyst in above-mentioned embodiment 1, grind to particle size less than 0.5mm, take 10g spruce wood as raw material, grind to particle size less than 0.3mm, after both are mechanically mixed, rapidly pyrolyze at 330 ° C under nitrogen atmosphere 15s, the obtained liquid yield was 42.8%, the content of 4-ethyl-2-methoxyphenol was analyzed by gas chromatography, and the yield of 4-ethyl-2-methoxyphenol was calculated to be 2.3%; The content of 4-ethyl-2-methoxyphenol in the organic liquid product (excluding water) was 11.0%.

Embodiment 3

[0031] Weigh 1.25 g of palladium nitrate dihydrate (Pd(NO 3 ) 2 ·2H 2 O) Dissolve in 100mL deionized water, stir until completely dissolved, add 7.80g SBA-15 to the solution, slowly drop ammonia water (25%) into the mixture under stirring until the pH value reaches 9, then continue Stir at room temperature for 12 h. After stirring, the solid was filtered, dried at 100°C for 3h, and then reduced in a hydrogen atmosphere (6% hydrogen and nitrogen as protective gas) at 280°C for 3h (programmed temperature was 2°C / min). 8.05 g of Pd / SBA-15 were obtained with a Pd loading of 5%.

[0032] Take 2g of the above catalyst, grind it to a particle size of less than 0.5mm, take 10g of cedar wood as a raw material, grind it to a particle size of less than 0.3mm, mechanically mix the two, and rapidly pyrolyze them for 15s at 300°C under a nitrogen atmosphere. The content of 4-ethyl-2-methoxyphenol was analyzed by gas chromatography, and the yield of 4-ethyl-2-methoxyphenol was calculated...

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Abstract

The invention belongs to the field of using biomass energy and in particular relates to a method for preparing 4-ethyl-2-metoxyphenol by catalytic pyrolysis of a biomass by virtue of a palladium-series catalyst. By taking the biomass as a raw material, the method comprises the steps of; mechanically mixing the biomass and the palladium-series catalyst, and carrying out quick pyrolysis under an oxygen-free condition at 250-380 DEG C; condensing the pyrolysis gas to obtain a liquid product rich in 4-ethyl-2-metoxyphenol; and carrying out simple separation and purification on the liquid product to obtain 4-ethyl-2-metoxyphenol with higher purity. In addition, the method for preparing 4-ethyl-2-metoxyphenol by catalytic pyrolysis of the biomass provided by the invention is low in cost and takes the wide biomass as the raw material so as to reduce the production cost of 4-ethyl-2-metoxyphenol.

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-ethyl-2-methoxyphenol by catalytic pyrolysis of biomass with a palladium-based catalyst. Background technique [0002] 4-Ethyl-2-methoxyphenol, alias 4-ethylguaiacol, 2-methoxy-4-ethylphenol, CAS number: 2785-89-9, has the following structure: [0003] [0004] 4-Ethyl-2-methoxyphenol has soy sauce flavor, smoky flavor and mild barbecue flavor, and it is the edible spice that can be used according to the national standard (GB2760-2011). Natural products mainly exist in the distillates of various woods, or in turmeric and peru balsam, tomatoes, coffee, brandy, rum, and whiskey, and are very important natural aroma components. 4-Ethyl-2-methoxyphenol is mainly used for the preparation of various sauce-flavored and strong-flavored wine flavors, and as flavoring agent and flavoring agent for soy sauce, meat and fruit products. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/01
CPCB01J29/0325B01J29/043B01J2229/18C07C41/01C07C43/23
Inventor 董长青张智博陆强陈晨李文涛张芸檀勤良
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)