Method for preparation of benzene ring phenol compound from alkali lignin

A technology for alkali lignin and phenol, which is applied in the field of preparing phenol compounds, can solve the problems of reducing reaction activity and selectivity, improving reaction risk coefficient and the like, and achieves the effects of simple recovery, cheap raw materials, and easy separation of products.

Inactive Publication Date: 2016-04-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

This type of method is likely to cause the reactants to coke and polymerize over time to form carbon deposi

Method used

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  • Method for preparation of benzene ring phenol compound from alkali lignin
  • Method for preparation of benzene ring phenol compound from alkali lignin
  • Method for preparation of benzene ring phenol compound from alkali lignin

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Metal catalyst: commercial catalysts can be used, such as: the catalyst Raney nickel used in the examples is commercially purchased from Anshan Zhongli Catalyst Factory, model ZL-N311, Ni content ≥ 90%.

[0041] The impregnation method can also be used to take metal precursors of different concentrations according to different loadings, and make a self-made supported metal catalyst. Taking the preparation of Pd / C and Ru / C as an example: in the corresponding metal precursors Palladium chloride and The aqueous solution of ruthenium trichloride impregnates the active carbon carrier in a medium volume, stirs it evenly, and then dries it at 60°C, then dries it at 120°C for 12 hours, and finally reduces it in a hydrogen atmosphere at 450°C for 1 hour, and then uses O 2 1% O 2 / N 2 The metal catalyst can be obtained by passivating the mixed gas for 6 hours.

Embodiment 2-10

[0043] Weigh a total of 10 grams of phosphorylcholine or a mixed solvent and transfer it to a 75 milliliter reaction kettle, add 0.25 grams of alkali lignin and 0.05 grams of Raney nickel catalyst, replace it with hydrogen for 3 times, and fill it with a certain amount of pressure of hydrogen , the reaction temperature is raised to a certain temperature, stirred quickly at 800rpm, and the heating is stopped after 6 hours of reaction. When the temperature drops to room temperature, the vent valve is opened to reduce the pressure in the kettle to normal pressure. Extract 3 times, use gas chromatography to analyze product distribution, and remove ethyl acetate with a rotary evaporator, and weigh it as the total weight of the product.

[0044] Conversion rate X (%) calculation method:

[0045] The reaction conditions and reaction results are shown in Table 1.

[0046] Table 1

[0047]

[0048] As shown in Table 1, the reaction medium used in the reaction temperature range o...

Embodiment 11-16

[0050] Adopt the reaction condition of embodiment 2-10, only change catalyst, and reaction condition and reaction result are shown in Table 2 for details.

[0051] Table 2

[0052]

[0053] As shown in Table 2, alkali lignin can be converted to ethylphenol with high selectivity on different catalysts in the catalytic process involved in the present invention. Among them, the selectivity of ethylphenol on the Raney nickel catalyst and the Pd catalyst can reach 47% and 48%, which shows that it is better than other catalysts in the phosphorylcholine composite medium.

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Abstract

The invention relates to a method for preparation of a benzene ring phenol compound from alkali lignin. At a reaction temperature of 150DEG C-300DEG C, under a hydrogen pressure of 0.1MPa-13Mpa, under the action of a metal catalyst, in a solvent containing choline ionic liquid, alkali lignin is taken as the reaction raw material, hydrogenation degradation of alkali lignin is carried out to prepare the benzene ring phenol compound. Specifically, the solvent containing choline ionic liquid can be one of a solvent only containing choline ionic liquid, a mixed solvent composed of choline ionic liquid and an inorganic solvent, or a mixed solvent composed of choline ionic liquid and an organic solvent; and the metal catalyst is raney nickel and/or loaded metal catalyst. The method provided by the invention has the significant advantages of cheap and easily available raw materials, simple catalyst preparation process, easy recovery, easy separation of product and the like.

Description

technical field [0001] The invention relates to a method for preparing benzene-cyclophenol compounds from alkali lignin. Using choline ionic liquid, a mixed solvent composed of choline ionic liquid and inorganic solvent, or a mixed solvent composed of choline ionic liquid and organic solvent as the reaction medium, under the action of a supported metal catalyst, hydrogenation degradation Alkali lignin preparation of benzene ring phenolic compounds. Background technique [0002] Lignin is a biomass-based material second only to cellulose in nature, with an annual global output of about 50 billion tons. As a big agricultural and forestry country, China produces up to 700 million tons of agricultural and forestry waste every year. One of the main components is lignin. The wastes produced by people in daily life and the residues of some industrial production also contain lignin components. The efficient conversion of lignin into energy chemicals can not only effectively alle...

Claims

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Application Information

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IPC IPC(8): C07C39/04C07C39/06C07C37/54
CPCY02P20/54
Inventor 刘菲王爱琴张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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