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amorphous co x mn y the w 4 Preparation method and application of activated carbon composite catalytic material

A technology for catalytic materials and composite materials, 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 the effect of high catalytic efficiency and wide industrial application prospects.

Active Publication Date: 2022-04-22
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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  • amorphous co  <sub>x</sub> mn  <sub>y</sub> the w  <sub>4</sub> Preparation method and application of activated carbon composite catalytic material
  • amorphous co  <sub>x</sub> mn  <sub>y</sub> the w  <sub>4</sub> Preparation method and application of activated carbon composite catalytic material
  • amorphous co  <sub>x</sub> mn  <sub>y</sub> the w  <sub>4</sub> Preparation method and application of 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 100 mL of water, cobalt chloride and manganese chloride salt are prepared into a solution with a concentration of 2.0 mol / L and 3.0 mol / L respectively; then 0.02 mol of activated carbon is added to fully Ultrasound; Next, add 100 mL of 5.0mol / L sodium tungstate solution quickly (1min) under stirring to form a large amount of flocculent precipitate; finally, quickly (1min) move to a freeze dryer, after 12h of freeze drying , and finally the 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 ...

Embodiment 2

[0039] The amorphous Co x mn y WO 4 The specific preparation process of the activated carbon composite material is as follows: first, in 100 mL of water, the cobalt nitrate and manganese nitrate salts are prepared into a solution with a concentration of 3.5 mol / L and 2.0 mol / L respectively; then 0.02 mol of activated carbon is added and fully ultrasonicated; Next, 3.5 mol / L 100mL sodium tungstate solution was quickly added (1min) under stirring to form a large amount of flocculent precipitates; finally, it was quickly (1min) transferred to a freeze dryer, and after 24 hours of freeze drying, the non- Crystalline 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 a...

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 100 mL of water, the cobalt acetate and manganese acetate salts are prepared into a solution with a concentration of 2.5 mol / L and 1.5 mol / L respectively; then 0.03 mol of activated carbon is added and fully ultrasonicated; Next, 5.0 mol / L 100mL sodium tungstate solution was quickly added (1min) under stirring to form a large amount of flocculent precipitates; finally, it was quickly (1min) transferred to a freeze dryer, and after 24 hours of freeze drying, the non- Crystalline 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 a...

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Abstract

The invention discloses amorphous Co x mn y WO 4 / preparation method and application of activated carbon composite catalytic material, wherein the method steps of catalytic material preparation are as follows: S11: preparation of dispersion liquid: under room temperature, fully dissolve inorganic metal cobalt salt, manganese salt in water, then add activated carbon in the solution, And the dispersion liquid of cobalt salt, manganese salt and activated carbon was prepared by ultrasonic treatment; S12: amorphous Co x mn y WO 4 / Preparation of activated carbon composite material: At room temperature, add sodium tungstate solution to the dispersion liquid in S11 while stirring at a speed of 200-500r / min to form a mixed solution, and keep stirring for 10-30min, and the reacted product After filtration and cleaning, the amorphous Co was obtained after vacuum freeze-drying. x mn y WO 4 / Activated carbon composite catalytic material. The invention can realize the conversion rate of ethylbenzene exceeding 80%, and the selectivity of the acetophenone product exceeding 90%, which are much higher than the traditional catalytic 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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Patent Type & Authority Patents(China)
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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