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A kind of method for preparing 4-ethyl-2-methoxyphenol by catalytic pyrolysis of biomass

A methoxyphenol, catalytic pyrolysis technology, applied in chemical instruments and methods, physical/chemical process catalysts, ether preparation and other directions, can solve the problems of complex extraction process steps, many waste liquids that are difficult to handle, no economy, and the like, To achieve the effect of simple composition, low requirements for equipment and reaction conditions, and lower production costs

Active Publication Date: 2016-10-12
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of method for preparing 4-ethyl-2-methoxyphenol by catalytic pyrolysis of biomass

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Weigh 0.50g 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 mixed solution under stirring until the pH value reaches 10, and then continue Stir at room temperature for 12h. After the stirring, the solid was filtered, dried at 100°C for 3h, and then reduced at 280°C for 3h (programmed temperature: 2°C / min) in an atmosphere of hydrogen (6% hydrogen, nitrogen as protective gas). 8.01 g of Pd / MCM-41 were obtained with a Pd loading of 2%.

[0027] Take 2g of the above catalyst, grind it to a particle size of less than 0.5mm, take 10g of larch wood as a raw material, grind it to a particle size of less than 0.3mm, mix the two mechanically, and quickly pyrolyze them at 290°C for 20s under a nitrogen atmosphere to obtain a liquid product Yield 36.5%, analyze wherein the content of 4-ethyl-2-methoxyphenol by gas chromatography, ca...

Embodiment 2

[0029] Take 5g of the catalyst in the above example 1, grind it to a particle size of less than 0.5mm, take 10g of spruce wood as a raw material, grind it to a particle size of less than 0.3mm, mix the two mechanically and rapidly pyrolyze them at 330°C under a nitrogen atmosphere 15s, the obtained liquid yield was 42.8%, and 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 1.25g 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 drip ammonia water (25%) into the mixed solution under stirring until the pH value reaches 9, and then continue Stir at room temperature for 12h. After the stirring, the solid was filtered, dried at 100°C for 3h, and then reduced at 280°C for 3h (programmed temperature: 2°C / min) in an atmosphere of hydrogen (6% hydrogen, nitrogen as protective gas). 8.05 g of Pd / SBA-15 with a Pd loading of 5% was obtained.

[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, mix the two mechanically, and rapidly pyrolyze them at 300°C for 15s under a nitrogen atmosphere to obtain a liquid product Yield 36.2%, analyze wherein the content of 4-ethyl-2-methoxyphenol by gas chromatography, calc...

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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 using a palladium series catalyst to catalyze and pyrolyze biomass. Background technique [0002] 4-Ethyl-2-methoxyphenol, also known as 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 is an edible spice that can be used according to the national standard (GB2760-2011). Natural products mainly exist in distillates of various woods, or in Tolu and Peru balsam, tomato, coffee, brandy, rum, whiskey, and are very important natural aroma components. 4-Ethyl-2-methoxyphenol is mainly used as a flavoring agent and flavoring agent for preparing various sauce-flavored and strong-flavored wine flavors, soy sauce, meat, and fruit products. [0005] At present, th...

Claims

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Application Information

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Patent Type & Authority Patents(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)
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