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CO (carbon monoxide)-promoted method for directly oxygenizing hydroxylated aromatic compound by molecular oxygen

A technology for oxidation and hydroxylation of aromatic hydrocarbons and molecular oxygen, which is applied to the preparation of organic compounds, molecular sieve catalysts, chemical instruments and methods, etc., to achieve the effects of large-scale production, environmental friendliness, and light waste treatment burden

Inactive Publication Date: 2012-10-17
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a new method for the direct hydroxylation of aromatic hydrocarbons to produce phenolic compounds, to overcome the existing problems in the existing aromatic hydrocarbon hydroxylation process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Weigh 0.664 g H 2 PtCl 6 ·9H 2 O, 0.420 g PdCl 2 , 0.508 g RhCl 3 , 0.646 g RuCl 3 ·3H 2 O, 0.670 g H 2 IrCl 6 ·6H 2 O or 0.390 g AgNO 3 Put them into 6 100 mL beakers, and add 5 g ZrO 2 And 20 mL of water, under 80 o Carefully evaporate the water in the C water bath, the resulting sample is at 100 o Bake in oven C for 12 hours, transfer the solid into the crucible at 350 o Roast in a muffle furnace under C for 2 hours, then in 5% H 2 / Ar airflow 300 o After roasting at C for 2 hours. The catalyst is prepared after cooling, expressed as Pt / ZrO 2 -Im, Pd / ZrO 2 -Im, Rh / ZrO 2 -Im, Ru / ZrO 2 -Im, Ir / ZrO 2 -Im or Ag / ZrO 2 -Im.

Embodiment 2

[0015] Example 2: Weigh 0.664 g H 2 PtCl 6 ·9H 2 O or 0.420 g PdCl 2 Put them into 2 100 mL beakers, and then add 5 g TiO 2 And 40 mL of 0.25M NaOH in ethylene glycol solution. After stirring for 1 hour at room temperature, the temperature is increased to 140 o C continue to stir for 3 hours, filter the precipitate, wash 3 times with distilled water, at 100 o After drying for 12 hours at C, the catalyst is prepared after cooling, expressed as Pt / TiO 2 -CD or Pd / TiO 2 -CD.

Embodiment 3

[0016] Example 3: 0.104 g HAuCl 4 ·4H 2 O, 0.5 L of water into a 1 L beaker, 80 o Under the condition of stirring at C, add 0.2 M sodium hydroxide solution until the pH is about 7, and then add 5 g CeO 2 , 80 o Continue to stir for 2 hours at C, filter the precipitate and wash with distilled water until there is no Cl - At 100 o Dry for 12 hours at C, and finally at 300 o Roast in a muffle furnace under C for 4 hours. The catalyst is prepared after cooling, expressed as Au / CeO 2 -DP.

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PUM

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Abstract

The invention belongs to the technical field of the catalytic synthesis, and particularly discloses a CO (carbon monoxide)-promoted method for directly oxygenizing a hydroxylated aromatic compound by molecular oxygen. The method provided by the invention uses an aromatic compound as a substrate, uses a combined catalyst consisting of a supported precious metal catalyst and a heteroatom zeolite containing Ti, V, Cu or Fe or a polyoxometalate, and uses the mixed liquid of water and an organic solvent as a solvent; the CO (carbon monoxide) and O2 (oxygen) are put into the reaction system; and, under the promotion of the CO (carbon monoxide), the molecular oxygen directly oxygenizes the hydroxylated aromatic compound to prepare a corresponding phenol compound. The equipment and the process used by the method provided by the invention are simple; the separation of the target product is relatively easy; the reaction conditions are moderate; the system is environment-friendly; and thus the method is a green process route.

Description

technical field [0001] The invention belongs to the technical field of catalytic synthesis, and in particular relates to a method for direct hydroxylation of aromatic compounds. Background technique [0002] Hydroxylation products of aromatic compounds are important compounds in the chemical and pharmaceutical fields. For example: Methyl p-hydroxybenzoate is a preservative additive in medicine, food, spices, and film, and it is also a strong bactericide. However, at present, most of the hydroxylation products of aromatic compounds are prepared through multi-step reaction methods, the process is complicated, the equipment requirements are high, and it is not good for production. Phenol, one of the hydroxylation products of aromatic hydrocarbons, is a very important bulk organic chemical raw material, and has broad applications in the fields of pharmaceutical intermediates, pesticides, spices, dyes, auxiliaries, and resins. At present, the main production method of phenol is...

Claims

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Application Information

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IPC IPC(8): C07B41/02C07C37/58C07C39/04C07C39/07C07C43/23C07C41/26C07C39/28C07C65/03C07C51/367C07C39/14B01J29/89B01J29/03B01J29/70B01J29/46B01J29/83B01J31/38
CPCY02P20/52
Inventor 曹勇倪吉于磊刘永梅
Owner FUDAN UNIV
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