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Method for preparing 4-ethyl phenol by selective lignin hydrogenolysis

A ‐ethylphenol and lignin technology, applied in the field of biomass energy utilization, can solve the problem of high cost of precious metals, and achieve the effect of simple preparation method, wide source and low price

Active Publication Date: 2017-10-10
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The nickel catalyst used in the method overcomes the disadvantage of high cost of precious metals in the existing process, and has a good hydrogenolysis effect on lignin, and the catalyst preparation method is simple, easy to recycle, and has no pollution to the environment

Method used

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  • Method for preparing 4-ethyl phenol by selective lignin hydrogenolysis
  • Method for preparing 4-ethyl phenol by selective lignin hydrogenolysis
  • Method for preparing 4-ethyl phenol by selective lignin hydrogenolysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The method for preparing 4-ethylphenol by selective catalytic conversion of lignin comprises the steps:

[0028] Weigh 203.3g of MgCl with a purity of 99% 2 ·6H 2 The solid of O was added to a 500ml beaker, fully dissolved with 200ml of deionized water, then poured into a 1000ml round bottom flask, and 100ml (25%) of NH 3 ·H 2 O while stirring vigorously. A white precipitate was formed and aged for 12 hours, filtered, and the filtrate was treated with Ag(NO 3 ) 2 The solution was detected, and the solid part was carefully washed several times with deionized water until no obvious precipitation was formed. The solid part was placed in an oven at 120°C for one night, and then calcined in a muffle furnace at 850°C for 4 hours to obtain a white powder that is the catalyst carrier MgO.

[0029] Weigh 1.818g of Ni(NO 3 ) 2 ·6H 2 O was dissolved in 2.25ml of deionized water, and after being completely dissolved, it was added to 1g of the prepared carrier MgO. After s...

Embodiment 2

[0040] Take by weighing 339.2g purity and be 99% Zr(NO 3 ) 4 ·5H 2 The solid of O was added to a 500ml beaker, fully dissolved with 200ml of deionized water, then poured into a 1000ml round bottom flask, and 100ml (25%) of NH 3 ·H 2 O while stirring vigorously. A white precipitate was formed and aged for 12 hours, filtered, and the filtrate was treated with Ag(NO 3 ) 2 The solution was detected, and the solid part was carefully washed several times with deionized water until no obvious precipitation was formed. Take the solid part and place it in an oven at 120°C for one night, and then calcinate it in a muffle furnace at 850°C for 4 hours to obtain a white powder that is the catalyst carrier ZrO 2 .

[0041] Weigh 1.818g of Ni(NO 3 ) 2 ·6H 2 O was dissolved in 2.25ml of deionized water, and after it was completely dissolved, it was added to 1g of carrier ZrO prepared in step 1). 2 middle. After soaking for 12 hours, dry it in a drying oven at 110°C for 12 hours, a...

Embodiment 3

[0045] Weigh 101.7g of MgCl with a purity of 99% 2 ·6H 2 The solid of O was added to a 500ml beaker, fully dissolved with 200ml of deionized water, then poured into a 1000ml round bottom flask, and 72ml (25%) of NH 3 ·H 2 O while stirring vigorously. A white precipitate was formed and aged for 12 hours, filtered, and the filtrate was treated with Ag(NO 3 ) 2 The solution was detected, and the solid part was carefully washed several times with deionized water until no obvious precipitation was formed. The solid part was placed in an oven at 120°C for one night, and then calcined in a muffle furnace at 850°C for 4 hours to obtain a white powder that is the catalyst carrier MgO.

[0046] Weigh 1.818g of Ni(NO 3 ) 2 ·6H 2 O was dissolved in 2.25ml of deionized water, and after being completely dissolved, it was added to 1g of the prepared carrier MgO. After soaking for 24 hours, dry it in a 110°C drying oven for 18 hours, and finally calcinate the dried solid in a muffle ...

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Abstract

The invention discloses a method for preparing 4-ethyl phenol by selective lignin hydrogenolysis. According to the method, lignin, nickel-based catalysts and reaction solvents are added into a reactor, the reactor is sealed and filled with hydrogen, the internal pressure of the reactor is controlled to be 0-4MPa, and reaction is performed for 1-5 hours at the temperature of 210-290 DEG C. After reaction, reaction liquid is filtered to obtain a liquid product containing the 4-ethyl phenol and recovered catalysts. The nickel-based catalysts comprise carriers and nickel metal loaded on the carriers. Generation of the 4-ethyl phenol in the hydrogenolysis process of lignin can be greatly promoted by the catalysts, formation of carbon deposits and other phenol products in the lignin depolymerization process is inhibited, and the generated 4-ethyl phenol is high in selectivity. The yield of the 4-ethyl phenol reaches 6.31%, the content of the 4-ethyl phenol in the organic liquid product is 38.83%, and the yield and selectivity simultaneously reach the current highest level.

Description

technical field [0001] The invention relates to 4-ethylphenol, in particular to a method for preparing 4-ethylphenol by selective catalytic hydrogenolysis of lignin with a nickel-based catalyst, which belongs to the field of utilization of biomass energy. Background technique [0002] As the only renewable resource that contains fixed carbon, the production of high value-added chemicals from biomass can reduce the dependence of modern chemical industry on fossil resources, and alleviate the development bottleneck caused by the decreasing reserves of fossil resources. However, lignin, as an important component that is not effectively utilized in biomass, has attracted widespread attention. [0003] Generally, more than 100 kinds of phenolic products can be obtained through depolymerization of lignin such as pyrolysis, hydrogenation, hydrogenolysis and oxidation, but the selectivity is generally very low, and 4‐ethylphenol is generally only used as one of them in a very small ...

Claims

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Application Information

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IPC IPC(8): C07C37/00C07C39/06B01J23/755
CPCB01J23/755B01J23/78C07C37/004C07C39/06Y02P20/52
Inventor 龙金星赵伟杰李雪辉徐志祥马宏卫
Owner SOUTH CHINA UNIV OF TECH
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