Catalyst for preparing p-nitroacetophenone by oxidation of p-nitroethylbenzene and preparation method thereof

A technology of p-nitroacetophenone and p-nitroethylbenzene, which is applied in the field of catalyst and its preparation, can solve the problems of difficult separation of catalyst and product, difficulty in repeated recycling, and low catalyst efficiency

Active Publication Date: 2019-05-07
YANCHENG INST OF IND TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. It is difficult to separate the catalyst and product dispersed in the system, and it is difficult to recycle repeatedly;
[0007] 2. The efficiency of the catalyst is low, and the oxidation reaction time of p-nitroethylbenzene is long

Method used

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  • Catalyst for preparing p-nitroacetophenone by oxidation of p-nitroethylbenzene and preparation method thereof
  • Catalyst for preparing p-nitroacetophenone by oxidation of p-nitroethylbenzene and preparation method thereof
  • Catalyst for preparing p-nitroacetophenone by oxidation of p-nitroethylbenzene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take by weighing 46g anhydrous cerium trichloride zinc (CeCl 3 ) was dissolved in 250ml of deionized water. After fully dissolving evenly, stir rapidly and add 40% NaOH dropwise to adjust the pH to 12 to obtain a white slurry.

[0019] Weigh 312g manganese sulfate (MnSO 4 ) was dissolved in 1000ml of deionized water. After fully dissolving evenly, stir rapidly and add 40% NaOH dropwise to adjust the pH to 10 to obtain a pink slurry, which was oxidized to a brown slurry.

[0020] Wet grind 660g of clay, 130g of talc and the above two slurries in a ball mill until the powder is less than 320 mesh, add a binder, and go through the extrusion molding process to produce a honeycomb ceramic blank, using a box-type drying furnace at 105°C After drying for 3 hours and firing at 1280°C for 6 hours, the cylindrical honeycomb ceramic catalyst was obtained with a size (mm) of 150×150×300, a number of pores of 25×25, a wall thickness (mm) of 1.0, a pore width of 2.77, and a specific...

Embodiment 2

[0025] Weigh 52g anhydrous cerium trichloride zinc (CeCl 3 ) was dissolved in 250ml of deionized water. After fully dissolving evenly, stir rapidly and add 40% NaOH dropwise to adjust the pH to 12 to obtain a white slurry.

[0026] Weigh 268g manganese sulfate (MnSO 4 ) was dissolved in 1000ml of deionized water. After fully dissolving evenly, stir rapidly and add 40% NaOH dropwise to adjust the pH to 10 to obtain a pink slurry, which was oxidized to a brown slurry.

[0027] Wet grind 665g of clay, 145g of talc and the above two slurries in a ball mill until the powder is less than 320 mesh, add a binder, and go through the process of extrusion molding to produce a honeycomb ceramic blank, using a box-type drying furnace at 105°C After drying for 3 hours and firing at 1260°C for 6 hours, the cylindrical honeycomb ceramic catalyst was obtained with a size (mm) of 150×150×300, a number of pores of 32×32, a wall thickness (mm) of 1.0, a pore width of 3.66, and a specific surface...

Embodiment 3

[0032] Weigh 60g anhydrous cerium trichloride zinc (CeCl 3 ) was dissolved in 250ml of deionized water. After fully dissolving evenly, stir rapidly and add 40% NaOH dropwise to adjust the pH to 12 to obtain a white slurry.

[0033] Weigh 248g manganese sulfate (MnSO 4 ) was dissolved in 1000ml of deionized water. After fully dissolving evenly, stir rapidly and add 40% NaOH dropwise to adjust the pH to 10 to obtain a pink slurry, which was oxidized to a brown slurry.

[0034] Wet grind 680g of clay, 107g of talc and the above two slurries in a ball mill until the powder is less than 320 mesh, add a binder, and go through the process of extrusion molding to produce a honeycomb ceramic blank, using a box-type drying furnace at 105°C After drying for 3 hours and firing at 1260°C for 6 hours, the cylindrical honeycomb ceramic catalyst was obtained with a size (mm) of 150×150×300, a number of pores of 40×40, a wall thickness (mm) of 0.7, a pore width of 3.03, and a specific surface...

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Abstract

The invention provides a catalyst for preparing p-nitroacetophenone by oxidizing 4-nitroethylbenzene and a preparation method of the catalyst. The method comprises the steps that clay and talc serve as the main raw materials, hydroxides of cerium (+3) and manganese (+2) are subjected to wet milling in a ball mill till the particle sizes are smaller than 320 meshes, an adhesive taking MC or PVA as the main component is added, a honeycomb greenware is produced through a technological process of extrusion molding, and the catalyst is obtained through firing at 1,240 DEG C to 1,280 DEG C. The catalyst comprises active catalytic components of cerium oxide, manganese dioxide and a ceramic carrier. The honeycomb ceramic catalyst of the Ce2O3-MnO2 and ceramic carrier has the advantages of being good in catalytic effect and long in service life. The catalyst is used for preparing p-nitroacetophenone by conducting pure oxygen catalyzing on 4-nitroethylbenzene, and the yield of p-nitroacetophenone is 65% or above.

Description

Technical field: [0001] The invention provides a catalyst for preparing p-nitroacetophenone by oxidizing p-nitroethylbenzene and a preparation method thereof. Background technique: [0002] p-Nitroacetophenone (PNAP) is an important intermediate in organic synthesis, widely used in the synthesis of pharmaceuticals, pesticides and chiral intermediates. p-Nitroacetophenone was prepared by oxidation of p-nitroethylbenzene, and the ketone group was obtained by controlling the depth of direct oxidation of α-H on the side chain of aromatic hydrocarbons. Early selection of some highly oxidizing chemical oxidants, such as: KMnO 4 、H 2 o 2 and CrO3 etc. The use of oxygen as the oxidant has the dual advantages of economic cost and environmental protection compared with chemical oxidants. At present, the industrial production method of p-nitroacetophenone is: add p-nitroethylbenzene into the oxidation tower, then add cobalt stearate and manganese acetate catalysts, and feed compre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/34C07C201/12C07C205/45
Inventor 项东升孙开进朱驯
Owner YANCHENG INST OF IND TECH
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