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Process for preparing phenolic compounds

A phenolic compound and catalyst technology, which is applied in the field of doped ceria as a catalyst, can solve the problems of reducing the selectivity and difficulty of phenolic compounds, and achieve the effects of cheap catalyst, simple preparation and wide source.

Active Publication Date: 2019-02-26
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the preparation of phenolic compounds by the lignin route reduces the dependence on petrochemical phenols, there are still some difficulties
Lignin depolymerization is usually achieved by hydrogenation route, which easily causes excessive hydrogenation of benzene ring and reduces the selectivity of phenolic compounds

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 50g of cerium nitrate and a certain amount of stannous chloride dihydrate and dissolve them in 4L of water, adopt 25wt% sodium carbonate aqueous solution as a precipitating agent, adjust the system pH=10, centrifuge the gained precipitate, wash until neutral, dry, Calcined at 500°C for 3h to get 2wt% Sn-CeO 2 . Sn-CeO 2 Fill the 14-25 mesh catalyst into a reaction tube with an inner diameter of 7mm and fill it with a 15cm bed. The speed is 0.03mL·min -1 , nitrogen as the carrier gas, the flow rate is 30mL·min -1 , reacted at 350°C for 12h, and separated the liquid after the reaction, and the oil phase and water phase obtained were analyzed by chromatography respectively. The conversion of acetic acid was 85% and the overall selectivity to phenolic compounds was 80%.

Embodiment 2

[0021] Weigh 50g of cerium nitrate and a certain amount of praseodymium nitrate hexahydrate and dissolve them in 4L of water, use 25wt% sodium carbonate aqueous solution as the precipitating agent, adjust the pH of the system to 10, centrifuge the resulting precipitate, wash until neutral, dry, and set at 500°C Roast for 3h to get 2wt% Pr-CeO 2 . Pr-CeO 2 Fill the 14-25 mesh catalyst into a reaction tube with an inner diameter of 8mm and fill it with a 25cm bed. Under normal pressure, the reaction solution prepared with acetic acid and formaldehyde at a molar ratio of 1:5 is used as the raw material, and the feed rate is 0.03mL min -1 , nitrogen as the carrier gas, the flow rate is 30mL·min -1 , reacted at 350°C for 12h, and separated the liquid after the reaction, and the oil phase and water phase obtained were analyzed by chromatography respectively. The conversion of acetic acid was 100%, and the overall selectivity to phenolic compounds was 83%.

Embodiment 3

[0023] Weigh 50g of cerium nitrate and a certain amount of lanthanum nitrate hexahydrate and dissolve them in 4L of water, use 10wt% sodium hydroxide solution as a precipitating agent, adjust the pH of the system to 11, centrifuge the resulting precipitate, wash until neutral, dry, 500 ℃ roasting for 3h, that is, 5wt% La-CeO 2 . La-CeO 2 Fill the 14-25 mesh catalyst into a reaction tube with an inner diameter of 10mm and fill it with a 30cm bed. The speed is 0.03mL·min -1 , nitrogen as the carrier gas, the flow rate is 30mL·min -1 , reacted at 350°C for 12h, and separated the liquid after the reaction, and the oil phase and water phase obtained were analyzed by chromatography respectively. The conversion of acetic acid was 90% and the overall selectivity to phenolic compounds was 93%.

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Abstract

The present invention relates to a method for preparing phenolic compounds. The method adopts acetic acid, formaldehyde, or acetic acid, formaldehyde and methanol as reactants, and prepares phenolic compounds under the catalysis of doped ceria. 550°C, after the reaction, the product composition was determined by mass spectrometry and quantified by chromatography. The reaction conversion rate of the method of the present invention is high, the maximum conversion rate of the reaction reaches 100%, and the total selectivity of phenolic compounds reaches 95%; in addition, the present invention selects doped ceria as the catalyst, and the catalyst is cheap, simple to prepare and high in efficiency , can be regenerated by roasting to remove carbon deposits, and has potential application prospects.

Description

technical field [0001] The invention relates to a method for preparing phenolic compounds, in particular to a method for catalyzing the preparation of phenolic compounds by using acetic acid, formaldehyde, or acetic acid, formaldehyde and methanol as reactants and doped cerium dioxide as a catalyst. Background technique [0002] Phenolic compounds are an important class of organic chemical raw materials. Phenol is one of the important derivatives of propylene, mainly used in the production of phenolic resin, caprolactam, bisphenol A, adipic acid, aniline, alkylphenol, salicylic acid, etc.; methylphenol is mainly used in phenolic resin, electrical insulating paint, Dyes, surfactants and lubricant additives, etc. In addition, phenolic compounds play a major role in the life activities of the human body and plants, such as anti-oxidation and anti-virus. [0003] At present, the main sources of phenolic compounds are petrochemical crude oil and plants. Crude oil is distilled ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/07C07C37/20
CPCC07C37/20C07C39/07
Inventor 王峰王业红徐杰张健张志鑫张晓辰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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