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Catalyst suitable for catalyzing selective hydrogenation of phenol to prepare cyclohexanone as well as preparation and application of catalyst

A technology for catalyzing phenol and selectivity, applied in the field of catalysis, can solve the problems of large-scale industrial application limitations, high reaction temperature and pressure, and low product selectivity, and achieve easy industrial scale-up production and application, mild preparation process, and simple preparation process Effect

Active Publication Date: 2022-02-01
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, the reaction of phenol hydrogenation to cyclohexanone reported in a large number of literatures has problems such as high reaction temperature and pressure, excessive catalyst dosage and low product selectivity. And it is also easy to produce by-products such as cyclohexanol and cyclohexane
Although the literature (Science, 2009,326:1250-1252) has reported that catalysts Pd / C and AlCl 3 Under mild reaction conditions (50°C, 1.0MPa H 2 ), the selectivity of cyclohexanone is above 99.9%, but AlCl as a Lewis acid additive 3 It will be hydrolyzed to generate highly corrosive HCl, which has problems such as corrosion of equipment and environmental pollution, and large-scale industrial applications are limited

Method used

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  • Catalyst suitable for catalyzing selective hydrogenation of phenol to prepare cyclohexanone as well as preparation and application of catalyst
  • Catalyst suitable for catalyzing selective hydrogenation of phenol to prepare cyclohexanone as well as preparation and application of catalyst
  • Catalyst suitable for catalyzing selective hydrogenation of phenol to prepare cyclohexanone as well as preparation and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Preparation of 5.0wt% Pd / ZrHP catalyst and evaluation of its catalytic activity.

[0033] The preparation method comprises the following steps:

[0034] (1) Weigh 5.156g ZrOCl 2 ·8H 2 O in a 250mL round bottom flask, add 100mL of distilled water and stir until completely dissolved, then slowly add 5.53g of 85wt% H 3 PO 4 solution, and stirred evenly at room temperature; then placed in a FCMCR-3S microwave reactor (Kerui Instruments) and heated for 20 minutes at a power of 600W; after cooling to room temperature, the resulting white precipitate was separated from the solid and liquid, and the solid was washed with distilled water to neutrality; dry in a vacuum oven at 80°C for 12h, and grind the solid particles; finally place it in a muffle furnace and roast at 200°C for 4h (heating rate 2°C / min) to obtain zirconium hydrogen phosphate ( ZrHP) carrier.

[0035] (2) Disperse 0.4 g of the prepared zirconium hydrogen phosphate (ZrHP) carrier in 100 mL of ethylene glycol...

Embodiment 2

[0041] Preparation methods of Pd / ZrHP catalysts with different Pd loadings and their catalytic activity evaluation.

[0042] The preparation method comprises the following steps:

[0043] (1) The microwave synthesis of the zirconium hydrogen phosphate (ZrHP) carrier is the same as the step (1) in Example 1.

[0044] (2) The basic steps of preparing the Pd / ZrHP catalyst by microwave reduction method are the same as in Example 1 step (2), the difference is that adding different metering concentrations is the chloropalladium acid solution of 0.01g-Pd / mL to make the Pd in ​​the catalyst The loading amounts of the two were 3.0wt%, 5.0wt%, 7.0wt%, 9.0wt%, respectively.

[0045] Catalytic activity evaluation: Add 10mmol phenol, 20mL cyclohexane and 0.1g of catalyst into a stainless steel autoclave equipped with a thermocouple and a polytetrafluoroethylene liner, and mix well; then fill the reaction kettle with H 2 And replace it three times to empty the air in the reactor, and then...

Embodiment 3

[0049] Reactivity of 5.0 wt% Pd / ZrHP catalysts for selective hydrogenation of phenol under different hydrogen pressures.

[0050] Adopt the catalyst of embodiment 1, catalytic activity evaluation is the same as embodiment 2, difference is that the hydrogen pressure that is charged in the reactor is respectively 0.5MPa, 1.0MPa, 1.5MPa, 2.0MPa. Table 3 shows the reactivity of 5.0wt% Pd / ZrHP catalysts for the selective hydrogenation of phenol under different hydrogen pressures.

[0051] table 3

[0052]

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Abstract

The invention discloses a catalyst suitable for catalyzing selective hydrogenation of phenol to prepare cyclohexanone and a preparation method of the catalyst. The catalyst comprises a porous solid acid zirconium hydrogen phosphate carrier with a layered structure and noble metal Pd nanoparticles loaded on the carrier, wherein the mass fraction of Pd in the catalyst is 1-10%. The preparation method comprises the following steps: uniformly mixing phosphoric acid and ZrOCl2.8H2O in water, conducting heating for 20-30 minutes under the microwave power of 550-650W, taking a solid, conducting washing, conducting drying, and conducting roasting at 190-210 DEG C to obtain zirconium hydrogen phosphate; and dispersing the zirconium hydrogen phosphate in a reducing organic solvent, adding a palladium precursor solution into the reducing organic solvent, uniformly conducting mixing, conducting heating and reducing for 4-8 minutes under the microwave power of 550-650W, taking a solid, conducting washing, and conducting drying to obtain the catalyst. The invention also discloses application of the catalyst in catalyzing selective hydrogenation of phenol to prepare cyclohexanone.

Description

technical field [0001] The invention relates to the technical field of catalysis, in particular to a catalyst suitable for catalyzing the selective hydrogenation of phenol to prepare cyclohexanone and its preparation and application. Background technique [0002] Cyclohexanone is the main intermediate for the preparation of nylon, caprolactam and adipic acid, and is also a commonly used solvent in the preparation of industrial products such as paints, pesticides, dyes, rubber, and lubricating oil. [0003] The production process of cyclohexanone mainly includes cyclohexane oxidation method and phenol hydrogenation method. Compared with the traditional cyclohexane oxidation method, the phenol hydrogenation method has gradually become the main way to produce cyclohexanone due to its advantages such as simple process, low energy consumption, and less pollution. [0004] So far, the reaction of phenol hydrogenation to cyclohexanone reported in a large number of literatures has ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J35/00B01J37/16B01J37/34C07C45/00C07C49/403
CPCB01J27/1856B01J37/346B01J37/16C07C45/006C07C2601/14B01J35/394B01J35/393C07C49/403
Inventor 王紫璇侯昭胤陈平
Owner ZHEJIANG UNIV
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