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Composite phase VPO catalyst and preparation method and application thereof

A catalyst and composite phase technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, preparation of organic compounds, etc., to achieve high catalytic efficiency

Active Publication Date: 2019-02-01
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of preparing acrylic acid by the reaction of acetic acid and formaldehyde is still in the laboratory stage, and the performance of the catalyst is mainly improved.

Method used

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  • Composite phase VPO catalyst and preparation method and application thereof
  • Composite phase VPO catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022]4.8g of vanadium pentoxide and 72ml of benzyl alcohol were refluxed at 140°C for 5 hours, and 2.1g of PEG6000 was added to the reaction medium. After 1 hour, 6.44g of concentrated phosphoric acid with a mass percent concentration of 85% was added and refluxed for 6 hours to obtain The dark blue suspension mixture was filtered, washed with acetone, and dried at 100°C for 24 hours to obtain a VPO precursor. The precursor is loaded into an inline activation tube with an internal diameter of 50mm, and is heated from room temperature to 400°C at a rate of 2°C / min in 1.5% n-butane / air flow (90ml / min), and kept for 15 hours to obtain ( VO) 2 P 2 o 7 ; The VPO precursor was heated from room temperature to 400°C at a rate of 2°C / min in an oxygen flow of 40ml / min and kept for 15 hours to obtain δ-VOPO 4 . Will (VO) 2 P 2 o 7 and δ-VOPO 4 According to the mass ratio of 3:1, it was mixed and ball milled on an omnidirectional ball mill for 12 hours to obtain a VPO catalyst ap...

Embodiment 2

[0025] 4.8g of vanadium pentoxide and 72ml of benzyl alcohol were refluxed at 140°C for 5 hours, and 2.1g of PEG6000 was added to the reaction medium. After 1 hour, 6.44g of concentrated phosphoric acid with a mass percent concentration of 85% was added and refluxed for 6 hours to obtain The dark blue suspension mixture was filtered, washed with acetone, and dried at 100°C for 24 hours to obtain a VPO precursor. The precursor is loaded into an inline activation tube with an internal diameter of 50mm, and is heated from room temperature to 400°C at a rate of 2°C / min in 1.5% n-butane / air flow (90ml / min), and kept for 15 hours to obtain ( VO) 2 P 2 o 7 ; The VPO precursor was heated from room temperature to 400°C at a rate of 2°C / min in an oxygen flow of 40ml / min and kept for 15 hours to obtain δ-VOPO 4 . Will (VO) 2 P 2 o 7 and δ-VOPO 4 According to the mass ratio of 1:3, it was mixed and ball milled on an omnidirectional ball mill for 12 hours to obtain a VPO catalyst u...

Embodiment 3

[0028] 4.8g of vanadium pentoxide and 72ml of benzyl alcohol were refluxed at 140°C for 5 hours, and 2.1g of PEG6000 was added to the reaction medium. After 1 hour, 6.44g of concentrated phosphoric acid with a mass percent concentration of 85% was added and refluxed for 6 hours to obtain The dark blue suspension mixture was filtered, washed with acetone, and dried at 100°C for 24 hours to obtain a VPO precursor. The precursor is loaded into an inline activation tube with an internal diameter of 50mm, and is heated from room temperature to 400°C at a rate of 2°C / min in 1.5% n-butane / air flow (90ml / min), and kept for 15 hours to obtain ( VO) 2 P 2 o 7 ; The VPO precursor was heated from room temperature to 400°C at a rate of 2°C / min in an oxygen flow of 40ml / min and kept for 15 hours to obtain δ-VOPO 4 . Will (VO) 2 P 2 o 7 and δ-VOPO 4 According to the mass ratio of 1:1, they were mixed and ball milled on an omnidirectional ball mill for 4 hours to obtain a VPO catalyst...

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Abstract

Provided is a composite phase VPO catalyst; the composite phase VPO catalyst is formed by mixing two phases of (VO)2P2O7 with delta-VOPO4 or gamma-VOPO4, or two phases of delta-VOPO4 and gamma-VOPO4 at a mass ratio of 1:3-3:1. The catalyst can finely regulate and control the composition of the phases in the catalyst, thereby significantly changing the reaction behavior of the catalyst. The catalyst has high catalytic efficiency for condensation of acetic acid and formaldehyde to prepare acrylic acid (acrylate), and has fewer by-products; the highest yield of target products (acrylic acid and methyl acrylate) can reach 84.2%. The invention discloses a preparation method of the composite phase VPO catalyst.

Description

technical field [0001] The invention relates to a composite phase VPO catalyst and its application in the reaction of acetic acid and formaldehyde to prepare acrylic acid (ester). Background technique [0002] The production technology of acrylic acid is constantly developing. The industrial production process of acrylic acid has mainly experienced chlorohydrin method, cyanohydrin method, Reppe method, enone method, acrylonitrile hydrolysis method, propylene two-step oxidation method and One-step oxidation of propane. At present, the most widely used method for preparing acrylic acid in industry is the two-step oxidation of propylene, accounting for about 85% of the total output of acrylic acid. [0003] The method described above is basically based on petroleum as a raw material. Combined with the current situation of my country's energy structure rich in coal, poor in oil, and low in gas, people are actively researching and exploring new ways to produce acrylic acid. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/353C07C57/045C07C67/00C07C69/54
CPCC07C51/353C07C67/00B01J27/198C07C57/04C07C69/54
Inventor 季伟捷刘军冯新振徐志佳
Owner NANJING UNIV
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