Catalyst for one-step synthesis of alkyl cyclohexanone from alkylphenol and preparation method thereof

A technology of alkyl phenol and catalyst, applied in the field of selective hydrogenation catalyst and its preparation, can solve the problems of low conversion rate and selectivity, improve activity and selectivity, eliminate agglomeration, and facilitate large-scale industrial production Effect

Inactive Publication Date: 2009-08-12
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to provide a catalyst for the one-step synthesis of alkylcyclohexanone from alkylphenol, its active carbon carrier and auxiliary The catalytic components are used together, so that the catalyst has good catalytic activity for the one-step synthesis of alkylcyclohexanone by hydroisomerization of alkylphenol, high conversion rate of alkylphenol, and high selectivity of product alkylcyclohexanone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put the activated carbon in a pulverizer and pulverize it into powder, screen out 100-300 mesh activated carbon, add it to a nitric acid solution with a concentration of 2.5mol / L, and place it in an ultrasonic generator for ultrasonic immersion for 8 hours, then wash the activated carbon with deionized water to Neutralize and filter to obtain a pretreated activated carbon filter cake. Take 10 g of dry-based activated carbon filter cake and add it to 10 mL of an aqueous solution with a concentration of 0.05 g / mL noble metal palladium salt for loading. At 45 ° C, stir and impregnate and ultrasonicate for 2 hours, filter, and add deionized water to the filter cake to make a slurry with a volume of 100 mL. Regulate pH=11 with sodium hydroxide solution, add 10mL formaldehyde solution and carry out reduction by liquid-phase chemical reduction method, the active component precious metal palladium is evenly distributed on the surface of the activated carbon carrier with highly d...

Embodiment 2

[0028] Put the activated carbon into a pulverizer and pulverize it into powder, screen out 100-300 mesh activated carbon, add it to a nitric acid solution with a concentration of 2.5mol / L, and place it in an ultrasonic generator for ultrasonic immersion for 8 hours, then wash the activated carbon with deionized water To neutral and filtered to obtain a pretreated activated carbon filter cake. Take 10g of dry-based activated carbon filter cake and add it to 10mL of precious metal palladium salt solution with a palladium metal content of 5% for loading. At 45°C, stir and impregnate and ultrasonicate for 2 hours, filter, and add deionized water to the filter cake to make a slurry with a volume of 100mL. Regulate pH=11 with sodium hydroxide solution, add 10mL formaldehyde solution and carry out reduction by liquid-phase chemical reduction method, the active component precious metal palladium is evenly distributed on the surface of the activated carbon carrier with highly dispersed ...

Embodiment 3

[0030] Put the activated carbon in a pulverizer and pulverize it into powder, screen out 100-300 mesh activated carbon, add it to a nitric acid solution with a concentration of 2.5mol / L, and place it in an ultrasonic generator for ultrasonic immersion for 8 hours, then wash the activated carbon with deionized water to Neutralize and filter to obtain a pretreated activated carbon filter cake. Take 10g of dry-based activated carbon filter cake and add it to 10mL of precious metal palladium salt solution with a palladium metal content of 5% for loading. At 45°C, stir and impregnate and ultrasonicate for 2 hours, filter, and add deionized water to the filter cake to make a slurry with a volume of 100mL. Regulate pH=11 with sodium hydroxide solution, add 10mL formaldehyde solution and carry out reduction by liquid-phase chemical reduction method, the active component precious metal palladium is evenly distributed on the surface of the activated carbon carrier with highly dispersed n...

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Abstract

The invention relates to a catalyst for synthesizing alkyl cyclohexanone by alkyl phenol in one step and a preparation method thereof. The catalyst comprises an active carbon carrier, and nano active component palladium metal and auxiliary catalytic component alkaline metal or alkaline-earth metal loaded on the active carbon carrier. The preparation method for the catalyst comprises the following steps: after the active carbon is subjected to ultrasonic treatment by nitric acid solution, using deionized water to wash the active carbon to be neutral, adding the active carbon into palladium salt aqueous solution to be ultrasonically soaked, filtering the solution, pulping a filter cake and then reducing the filter cake, evenly distributing nano-scale granules as the active component on the surface of the active carbon carrier, filtering and washing the reactants until no chloride ions exist, then adding the filter cake into alkaline metal or alkaline-earth metal salt solution, pulping, soaking and filtering the filter cake, and drying the filter cake to form a Pd/active carbon catalyst. The preparation method is simple to operate, the palladium/carbon catalyst particles are evenly distributed and are less than 50 nanometers, the catalyst enjoys adjustability, and the catalyst is particularly suitable for the reaction of synthesizing the alkyl cyclohexanone by the alkyl phenol in one step and has high catalytic activity and ketone selectivity.

Description

technical field [0001] The invention relates to a selective hydrogenation catalyst and a preparation method thereof; in particular to a catalyst for one-step synthesis of alkylcyclohexanone from alkylphenol and a preparation method thereof. Background technique [0002] Cyclohexanone is an important chemical product widely used in modern chemical industry, especially in nylon, rubber and other fields. Alkylalkylcyclohexanone is widely used as an important fine chemical intermediate for the synthesis of monomer liquid crystals, medicines, and pesticides. The traditional method for preparing alkylalkylcyclohexanone is to convert alkylphenol into alkylcyclohexanol by catalytic hydrogenation, and then catalyze the oxidation of alkylcyclohexanol to alkylalkylcyclohexanone. This traditional preparation process has the disadvantages of complicated production steps, low product yield, high production cost, and serious environmental pollution. In recent years, with the sharp increa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/58C07C49/603C07C45/51
Inventor 曾永康张之翔曾利辉杨乔森文永忠潘丽娟
Owner XIAN CATALYST NEW MATERIALS CO LTD
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