A supported zirconium vanadate catalyst for the direct oxidation of benzene by oxygen to prepare phenol and its preparation method

A zirconium vanadate and catalyst technology, which is applied in the field of preparation of new catalysts, can solve the problems of many reaction steps, low yield, and no reports, and achieve the effects of simple preparation method, high catalytic activity and good stability

Active Publication Date: 2020-11-13
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of producing phenol in most factories is mainly the cumene method, which has the following five deficiencies: ① many reaction steps; ② low yield (about 5%); ③ large energy consumption; ④ serious environmental pollution ; ⑤ The cost will fluctuate with the market price of by-product acetone
So far, the supported zirconium vanadate catalyst prepared by co-precipitation method from zirconium and vanadium, and the research on the supported zirconium vanadate catalyst for the direct oxidation of benzene to phenol by oxygen has not been reported

Method used

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  • A supported zirconium vanadate catalyst for the direct oxidation of benzene by oxygen to prepare phenol and its preparation method
  • A supported zirconium vanadate catalyst for the direct oxidation of benzene by oxygen to prepare phenol and its preparation method
  • A supported zirconium vanadate catalyst for the direct oxidation of benzene by oxygen to prepare phenol and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 0.354g of ammonium metavanadate into 30ml of DMF, stir for 3h, and impregnate it at 25°C to obtain a mixed solution A. 0.529g of ZrCl 4 Dissolve in 20ml of DMF, and add the solution dropwise to the mixed solution A, and continue to stir for 5h, then wash the obtained mixture with DMF until the filtrate is colorless and transparent, then dry to obtain zirconium vanadate.

Embodiment 2

[0021] Add 5g of activated carbon and 0.354g of ammonium metavanadate to 30ml of DMF, stir for 6h, and impregnate it at 25°C, add 0.529g of ZrCl 4 Dissolve in 20ml of DMF, and add the solution dropwise to the mixed solution in step 1 and continue to stir for 18 hours, then wash the obtained mixture with DMF until the filtrate is colorless and transparent, then dry to obtain the activated carbon-supported zirconium vanadate catalyst . From figure 2 Can see NH 4 The presence of Cl peaks, indicating that ZrCl 4 and NH 4 VO 3 The reaction produces NH 4 Cl. The broad peak at 26-30° indicates that the catalyst is in an amorphous structure. The V-Zr complex also exists in an amorphous structure. Therefore, we can assume that ZrCl 4 and NH 4 VO 3 Amorphous vanadium-zirconium compounds were formed by co-precipitation. XPS analysis can infer the chemical valence states of Zr and V before and after the reaction. Depend on image 3 It can be seen that Zr 3d 5 / 2 and Zr 3d ...

Embodiment 3

[0024] 5g MWCNTs and 0.354g ammonium metavanadate were added to 30ml of DMF, stirred for 4h, and impregnated at 25°C, and 0.529g of ZrCl 4 Dissolve in 20ml of DMF, and add the solution dropwise to the mixed solution in step 1 and continue to stir for 18 hours, then wash the obtained mixture with DMF until the filtrate is colorless and transparent, then dry to obtain MWCNTs supported zirconium vanadate catalyst .

[0025] The prepared catalyst was used for benzene hydroxylation reaction, 150mg catalyst, 1mL benzene (0.84g), 3mL acetonitrile, 0.7g ascorbic acid were added to react in a 10mL autoclave, and 3MPa O 2 , reacted under magnetic stirring, the reaction temperature was 80°C, kept for 5h, and the yield of phenol was 8.9%.

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Abstract

The invention discloses a preparation method of a supported zirconium vanadate catalyst used for preparing phenol by directly oxidizing benzene. The method includes: adding a supporter and ammonium metavanadate in DMF (dimethyl formamide) by stirring for 3-6 hours to be steeped; then, dissolving ZrCl4 in DMF, dropwise adding a solution to the above mixture by stirring continuously, washing the obtained mixture with DMF till a filtrate is colorless and transparent, and performing drying to obtain the supported zirconium vanadate catalyst. The catalyst is applied to the field of chemical engineering, and oxygen can be catalyzed to oxidize benzene directly to phenol; the preparation method of the catalyst has the advantages of simpleness, greenness, high catalytic activity, high yield, good stability, no corrosion to reaction equipment, easy separation for circulation after reaction and the like.

Description

technical field [0001] The invention belongs to the technical field of novel catalyst preparation, and in particular relates to a supported zirconium vanadate catalyst used for oxygen direct oxidation of benzene to prepare phenol and a preparation method thereof. Background technique [0002] Phenol is an important chemical intermediate. 90% of phenol is used in the synthesis of phenolic resins. It is also used in the synthesis of medicines, pesticides, paints, dyes, explosives, petroleum additives, paint removers, wood preservatives, spices, etc. field plays an important role. At present, the method of producing phenol in most factories is mainly the cumene method, which has the following five deficiencies: ① many reaction steps; ② low yield (about 5%); ③ large energy consumption; ④ serious environmental pollution ; ⑤ The cost will fluctuate with the market price of by-product acetone. Therefore, in recent years, countries all over the world have devoted themselves to the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J23/22B01J37/02B01J37/03C07C39/04C07C37/58
CPCB01J23/002B01J23/22B01J27/24B01J37/0201B01J37/035B01J2523/00C07C37/58B01J2523/31B01J2523/48B01J2523/55C07C39/04Y02P20/52Y02P20/584
Inventor 王伟涛李娜马养民唐皓杨秀芳
Owner SHAANXI UNIV OF SCI & TECH
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