VPO catalyst, preparation method and uses thereof

A catalyst, vanadium pentoxide technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, chemical instrument and method, etc., to achieve high catalytic efficiency

Active Publication Date: 2018-04-13
SHANGHAI HUAYI NEW MATERIAL +1
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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 formal...

Method used

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  • VPO catalyst, preparation method and uses thereof
  • VPO catalyst, preparation method and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 4.8g of vanadium pentoxide and 72ml of benzyl alcohol were refluxed at 140°C for 6 hours, and 2.1g of PEG6000 was added to the reaction medium. After 1 hour, 6.45g 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, the solid was washed with acetone, and dried at 100°C for 24 hours to obtain the VPO precursor. The dried precursor was pressed into tablets and crushed to obtain 20-40 mesh particles, which were filled with an inner diameter of 10mm The in-line activation tube was used to heat up from room temperature to 400°C at a rate of 2°C / min in a 20ml / min volume ratio of 0.2% n-butane / air atmosphere for 15 hours to prepare acrylic acid ( ester) VPO catalyst.

[0021] Get above-mentioned catalyst 5g to carry out the continuous reaction of acetic acid and formaldehyde in fixed-bed reactor, reaction temperature is 360 ℃, reaction pressure is normal pressure, r...

Embodiment 2

[0023] 4.0g of vanadium pentoxide and 60ml of benzyl alcohol were refluxed at 140°C for 6 hours, and 1.75g ​​of PEG6000 was added to the reaction medium. After 1 hour, 5.37g 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, the solid was washed with acetone, and dried at 100°C for 24 hours to obtain the VPO precursor. The dried precursor was pressed into tablets and crushed to obtain 20-40 mesh particles, which were filled with an inner diameter of 10mm The in-line activation tube was used to heat up from room temperature to 400°C at a rate of 2°C / min in a 20ml / min volume ratio of 0.2% n-butane / air atmosphere for 15 hours to prepare acrylic acid ( ester) VPO catalyst.

[0024]Get above-mentioned catalyzer 5g and carry out the continuous reaction of acetic acid and formaldehyde in fixed-bed reactor, temperature of reaction is 360 ℃, and reaction pressure is normal ...

Embodiment 3

[0026] 4.0g of vanadium pentoxide and 88ml of benzyl alcohol were refluxed at 110°C for 6 hours, and 2.67g of PEG6000 was added to the reaction medium. After 1 hour, 6.84g of concentrated phosphoric acid with a mass percent concentration of 85% was added and refluxed for 4 hours to obtain The dark blue suspension mixture was filtered, the solid was washed with acetone, and dried at 100°C for 24 hours to obtain the VPO precursor. The dried precursor was pressed into tablets and crushed to obtain 20-40 mesh particles, which were filled with an inner diameter of 10mm The in-line activation tube was used to heat up from room temperature to 440°C at a rate of 2°C / min in a 20ml / min volume ratio of 1.5% n-butane / air atmosphere for 5 hours to prepare acrylic acid ( ester) VPO catalyst.

[0027] Get above-mentioned catalyzer 5g and carry out the continuous reaction of acetic acid and formaldehyde in fixed-bed reactor, temperature of reaction is 340 ℃, and reaction pressure is normal pr...

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PUM

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Abstract

The invention relates to a VPO catalyst for preparing acrylic acid or methyl acrylate through condensation of acetic acid and formaldehyde. The preparation method comprises: reducing pentavalent vanadium (vanadium pentoxide) through benzyl alcohol, adding a polyethylene glycol (PEG 6000) surfactant to the alcohol medium, adding phosphoric acid to prepare a catalyst precursor, and activating with butane gas through activators with different pipe diameters (10-48 mm) at different activation temperatures (400-440 DEG C) under different butane concentrations (0-1.5 vol.%) and different flow rate (20-60 ml/min) to prepare the catalyst. According to the present invention, the catalyst precursor is activated through the method, such that the sample morphology and the crystal phase composition ofthe catalyst, and the V<5+>/V<4+>ratio can be regulated and changed so as to significantly change the reaction behavior of the catalyst; and the prepared catalyst has advantages of high catalytic efficiency and less by-products, wherein the highest yield of the target product (acrylic acid and methyl acrylate) can reach 80.9%.

Description

technical field [0001] The invention relates to a VPO catalyst and its application in the reaction of acetic acid and formaldehyde to produce 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 prepare acrylic acid. The route of produ...

Claims

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Application Information

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IPC IPC(8): B01J27/198C07C51/353C07C57/04
CPCB01J27/198B01J37/08B01J37/16C07C51/353C07C57/04
Inventor 季伟捷冯新振刘军马建学庄岩
Owner SHANGHAI HUAYI NEW MATERIAL
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