Method for preparing p-coumarate by catalyzing lignin depolymerization through hierarchical pore molecular sieve loaded molybdenum oxide

A coumaric acid ester and molecular sieve technology, which is applied in molecular sieve catalysts, catalyst activation/preparation, chemical instruments and methods, etc., can solve the problems of difficult separation and recycling of catalysts, low lignin conversion rate, harsh reaction conditions, etc. High utilization value, high yield and high selective depolymerization, simple operation effect

Active Publication Date: 2021-03-16
SOUTH CHINA UNIV OF TECH
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Problems solved by technology

However, this technology uses lignin hydrogenation to realize lignin depolymerization. In the reaction process, it is necessary to use relatively expensive hydrogen to provide hydrogen source, and the reaction conditions are relatively harsh. The reaction temperature reaches 280°C and the hydrogen pressure reaches 8MPa.
[0006] In recent years, Li et al. (Z.M.Li, X.H.Li, Selective catalytic tailoring of the Hunit in herbaceous lignin for methyl p-hydroxycinnamate production overmetal-based ionic liquids, Green Chem., 2018, 20, 3743-3752) utilized homogeneous catalysts Metal-based ionic liquids [Bmim][FeCl 4 ] catalyzed the depolymerization of organic solvent-based bagasse lignin, under the optimal reaction conditions of reaction temperature 145°C, reaction time 6h, and nitrogen pressure 0.5MPa, a chemical with methyl p-coumarate as the main product was obtained, p-coumarin Acid methyl ester yield is 7.1wt.%, selectivity 70.5%, but this technology adopts homogeneous catalyst, and catalyst is difficult to separate and recycle, and industrial application is limited
Chinese invention patent application 201911410781.0 uses commercially available copper chloride, copper sulfate, and copper bromide as catalysts to catalyze the depolymerization of lignin into chemicals whose main product is methyl p-coumarate, but the conversion rate of lignin is low

Method used

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  • Method for preparing p-coumarate by catalyzing lignin depolymerization through hierarchical pore molecular sieve loaded molybdenum oxide
  • Method for preparing p-coumarate by catalyzing lignin depolymerization through hierarchical pore molecular sieve loaded molybdenum oxide
  • Method for preparing p-coumarate by catalyzing lignin depolymerization through hierarchical pore molecular sieve loaded molybdenum oxide

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Effect test

Embodiment 1

[0039] Embodiment 1: the preparation of 5wt.%Mo / ZSM-5 catalyst

[0040] The preparation of the molybdenum oxide catalyst 5wt.% Mo / ZSM-5 supported by the hierarchical porous molecular sieve is realized by a two-step method:

[0041] (1) Preparation of HZSM-5 carrier: use tetraethylorthosilicate as silicon source, tetrapropylammonium hydroxide as template, sodium metaaluminate as aluminum source, mix silicon source and template, and disperse in In water, stir for 3 hours until the silicon source is completely hydrolyzed, then add amino acid, stir for 2 hours until the dispersion is uniform, and then evaporate the water to the specified water-to-silicon ratio (mol(H 2 O): mol (SiO 2 )=9:1), the molar ratio of each active ingredient is 1.0SiO 2 : 0.003Al 2 o 3 : 0.015Na 2 O: 0.45TPAOH: 0.4L-lysine: 9H 2 The initial gel of O. Put the initial gel into a stainless steel hydrothermal reaction kettle lined with polytetrafluoroethylene, crystallize in an oven at 90°C for 48h, the...

Embodiment 2

[0046] Embodiment 2: the preparation of 2.5wt.%Mo / ZSM-5 catalyst

[0047] The preparation of molybdenum oxide catalyst 2.5wt.%Mo / ZSM-5 supported by hierarchical pore molecular sieves is achieved by a two-step method:

[0048] (1) Preparation of HZSM-5 carrier: use tetraethylorthosilicate as silicon source, tetrapropylammonium hydroxide as template, sodium metaaluminate as aluminum source, mix silicon source and template, and disperse in In water, stir for 6 hours until the silicon source is completely hydrolyzed, then add amino acid, stir for 4 hours to disperse evenly, then evaporate the water to the specified water-to-silicon ratio (mol(H 2 O): mol (SiO 2 )=9:1; ), the molar ratio of each active ingredient obtained is 1.0SiO 2 : 0.003Al 2 o 3: 0.015Na 2 O: 0.45TPAOH: 0.4L-lysine: 9H 2 The initial gel of O. Put the initial gel into a stainless steel hydrothermal reaction kettle with polytetrafluoroethylene lining, crystallize in an oven at 70°C for 60 hours, then move ...

Embodiment 3

[0051] Embodiment 3: the preparation of 10wt.%Mo / ZSM-5 catalyst

[0052] The preparation of the molybdenum oxide catalyst 10wt.% Mo / ZSM-5 supported by the hierarchical porous molecular sieve is realized by a two-step method:

[0053] (1) Preparation of HZSM-5 carrier: use tetraethylorthosilicate as silicon source, tetrapropylammonium hydroxide as template, sodium metaaluminate as aluminum source, mix silicon source and template, and disperse in In water, stir for 3 hours until the silicon source is completely hydrolyzed, then add amino acid, stir for 2 hours until the dispersion is uniform, and then evaporate the water to the specified water-to-silicon ratio (mol(H 2 O): mol (SiO 2 )=9:1; ), the molar ratio of each active ingredient obtained is 1.0SiO 2 : 0.003Al 2 o 3 : 0.015Na 2 O: 0.45TPAOH: 0.4L-lysine: 9H 2 The initial gel of O. Put the initial gel into a stainless steel hydrothermal reaction kettle lined with polytetrafluoroethylene, crystallize in an oven at 90°C...

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Abstract

The invention discloses a method for preparing p-coumarate by catalyzing lignin depolymerization through hierarchical pore molecular sieve loaded molybdenum oxide. The method comprises the following steps: by taking lignin as a raw material, adding a reaction medium and a hierarchical pore molecular sieve loaded molybdenum oxide catalyst, replacing with nitrogen, pressurizing to 0.1-1MPa, heatingto 120-160 DEG C, reacting for 2-10 hours while stirring, removing the catalyst after the reaction, and catalytically degrading the lignin into p-coumarate. By regulating and controlling the catalyststructure, the reaction medium and the reaction condition factors, high-yield and high-selectivity depolymerization of lignin is achieved, p-coumarate serving as a high-added-value chemical is obtained, and the purpose of high-valued utilization of lignin is achieved. The heterogeneous catalyst is used, the process is simple, reaction conditions are mild, lignin can be selectively converted to obtain the target product p-coumarate, and the yield and selectivity of p-coumarate can reach up to 11.78 wt.% and 85.24 wt.% respectively.

Description

technical field [0001] The present invention relates to lignin depolymerization, in particular to a method for preparing p-coumaric acid ester by molybdenum oxide supported by multi-stage pore molecular sieves by catalyzing lignin depolymerization, which belongs to the high-efficiency utilization technology of agricultural and forestry waste and the high-value utilization of renewable resources field. Background technique [0002] Utilizing the only renewable resource that contains fixed carbon—biomass to prepare high value-added chemicals can reduce the dependence of modern chemical industry on fossil resources and alleviate the development bottleneck caused by the dwindling reserves of fossil resources. At the same time, the use of "carbon-neutral" biomass resources can help alleviate a series of environmental problems such as the greenhouse effect caused by the excessive use of fossil resources. As the most abundant natural phenolic polymer macromolecule in nature, ligni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/48B01J37/02B01J35/10B01J37/10C07C67/31C07C69/732
CPCB01J29/48B01J37/0201B01J35/1019B01J35/1038B01J37/10C07C67/31B01J2229/186C07C69/732
Inventor 李雪辉张慧敏龙金星李立霞
Owner SOUTH CHINA UNIV OF TECH
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