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Preparation method and application of amorphous CoxMnyWO4/activated carbon composite catalytic material

A technology of catalytic materials and composite materials, which is applied in the field of preparation of amorphous CoxMnyWO4/activated carbon composite catalytic materials, can solve the problems of complex preparation process and high cost of raw materials, and achieve high catalytic efficiency and wide industrial application prospects

Active Publication Date: 2021-09-17
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These catalysts generally have the following shortcoming and deficiency, such as higher raw material cost, complex preparation process, etc., and the conversion rate of ethylbenzene is often lower than 65%, and the selectivity of acetophenone is often lower than 85%.

Method used

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  • Preparation method and application of amorphous CoxMnyWO4/activated carbon composite catalytic material
  • Preparation method and application of amorphous CoxMnyWO4/activated carbon composite catalytic material
  • Preparation method and application of amorphous CoxMnyWO4/activated carbon composite catalytic material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The amorphous Co x mn y WO 4 The specific preparation process of the activated carbon composite material is as follows: firstly, in 100mL water, cobalt chloride and manganese chloride salt are prepared into a solution with a concentration of 2.0mol / L and 3.0mol / L respectively; then 0.02mol activated carbon is added, fully ultrasonicated ; Next, add 100mL of 5.0mol / L sodium tungstate solution quickly (1min) under stirring to form a large number of flocculent precipitates; finally, quickly (1min) move to a freeze dryer, after freeze-drying for 12h, finally Amorphous Co 0.4 mn 0.6 WO 4 / activated carbon composite.

[0036] The specific surface area of ​​the activated carbon is 1900m 2 / g; pore volume 1.0cm 3 / g; pore size 2.0nm; carbon content 96%; density 0.38g / cc; iodine adsorption value 2100mg / g.

[0037] Add 0.5 g of the above catalyst and 100 mL of ethylbenzene into the reflux device of a three-necked flask, use air as an oxidant, and react at 120 °C under no...

Embodiment 2

[0039] The amorphous Co x mn y WO 4 The specific preparation process of the activated carbon composite material is as follows: firstly, in 100mL water, cobalt nitrate and manganese nitrate salt are prepared into a solution, the concentration is 3.5mol / L and 2.0mol / L respectively; then add 0.02mol activated carbon, fully ultrasonic; Next, quickly (1min) add 3.5mol / L 100mL sodium tungstate solution under stirring to form a large number of flocculent precipitates; finally, quickly (1min) move to a freeze dryer, after freeze drying for 24 hours, finally obtain an amorphous State Co 1 mn 0.57 WO 4 / activated carbon composite.

[0040] The specific surface area of ​​the activated carbon is 1800m 2 / g; pore volume 1.1cm 3 / g; pore size 2.1nm; carbon content 96.5%; density 0.39g / cc; iodine adsorption value 2000mg / g.

[0041] Add 0.8 g of the above catalyst and 100 mL of ethylbenzene into the reflux device of a three-necked flask, use air as an oxidant, and react at 130 °C under...

Embodiment 3

[0043] The amorphous Co x mn y WO 4 The specific preparation process of the activated carbon composite material is as follows: first, in 100mL water, the cobalt acetate and manganese acetate salts are prepared into a solution, the concentrations are 2.5mol / L and 1.5mol / L respectively; then 0.03mol activated carbon is added and fully ultrasonicated; then Next, quickly (1min) add 5.0mol / L 100mL sodium tungstate solution under stirring to form a large number of flocculent precipitates; finally, quickly (1min) move to a freeze dryer, after freeze drying for 24 hours, finally obtain an amorphous State Co 0.5 mn 0.3 WO 4 / activated carbon composite.

[0044] The specific surface area of ​​the activated carbon is 2000m 2 / g; pore volume 1.2cm 3 / g; pore size 2.2nm; carbon content>98%; density 0.40g / cc; iodine adsorption value 2100mg / g.

[0045] Add 1.4 g of the above catalyst and 100 mL of ethylbenzene into the reflux device of a three-necked flask, use air as the oxidant, a...

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Abstract

The invention discloses a preparation method and application of an amorphous CoxMnyWO4 / activated carbon composite catalytic material. The preparation method of the catalytic material comprises the following steps: S11, preparation of a dispersion liquid: fully dissolving inorganic metal cobalt salt and manganese salt in water at room temperature, then adding activated carbon into the solution, and performing ultrasonic treatment to prepare a dispersion liquid of cobalt salt, manganese salt and activated carbon; and S12, preparation of the amorphous CoxMnyWO4 / activated carbon composite material: at room temperature, adding a sodium tungstate solution into the dispersion liquid in the S11 in a stirring state at the rotating speed of 200-500r / min to form a mixed solution, continuously stirring the solution for 10-30 minutes, filtering and cleaning the reacted product, and performing vacuum freeze drying to obtain the amorphous CoxMnyWO4 / activated carbon composite catalytic material. According to the method, the conversion rate of ethylbenzene can exceed 80%, and the selectivity of acetophenone products exceeds 90%, which is greatly higher than that of a traditional catalysis method.

Description

technical field [0001] The invention relates to the technical field of preparation of acetophenone, in particular to amorphous Co x mn y WO 4 Preparation method and application of activated carbon composite catalytic material. Background technique [0002] Acetophenone is an important intermediate in organic synthesis and is widely used in industries such as dyes, spices, and medicine. Traditionally, the industrial production of acetophenone is prepared by Friedel-Crafts acylation reaction, that is, the synthesis of benzene and acetyl chloride in the presence of aluminum trichloride. However, the conditions of the reaction are harsh, and strong acid is generated after the reaction, which easily causes corrosion of production equipment and environmental pollution. [0003] With the development of the petrochemical industry and the development of selective oxidation catalytic technology, the catalytic oxidation of ethylbenzene to acetophenone has become a very active field...

Claims

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Application Information

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IPC IPC(8): B01J23/889B01J37/03B01J37/32C07C45/33C07C49/78
CPCB01J23/8892B01J23/002B01J37/031B01J37/32C07C45/33B01J2523/00C07C49/78B01J2523/69B01J2523/72B01J2523/845
Inventor 陈祥迎汪清李平范磊张忠洁童庆军
Owner HEFEI UNIV OF TECH
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