Vanadium-phosphorus-oxide (VPO) catalyst and application in preparation of crylic acid (ester) by reacting acetic acid (ester) with formaldehyde

A methyl acrylate and catalyst technology, applied in the direction of carboxylate preparation, physical/chemical process catalyst, carboxylate preparation, etc., to achieve the effect of less by-products and high catalytic efficiency

Inactive Publication Date: 2014-05-28
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the reaction of producing acrylic acid from acetic acid (methyl acetate) is still in the laboratory stage, and the catalyst activity (conversion rate), selectivity and catalyst stability are mainly improved.

Method used

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  • Vanadium-phosphorus-oxide (VPO) catalyst and application in preparation of crylic acid (ester) by reacting acetic acid (ester) with formaldehyde
  • Vanadium-phosphorus-oxide (VPO) catalyst and application in preparation of crylic acid (ester) by reacting acetic acid (ester) with formaldehyde
  • Vanadium-phosphorus-oxide (VPO) catalyst and application in preparation of crylic acid (ester) by reacting acetic acid (ester) with formaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 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 concentration of 85% by mass was added, and then refluxed for 6 hours. Filter the resulting dark blue suspension mixture, wash the solid with acetone, and dry at 100°C for 24 hours to obtain the precursor of the VPO catalyst. Raise the temperature from room temperature to 400°C at a rate of 2°C / min in an alkane / air atmosphere, then keep at this temperature for 15 hours, take the activated lower layer catalyst, press it into tablets, and crush it to obtain 20-40 mesh particles for activity testing .

[0022] Take 5g of the above-mentioned catalyst, and carry out continuous reaction of acetic acid and formaldehyde in a fixed-bed reactor, the reaction temperature is 360°C, the reaction pressure is normal pressure, the reaction carrier gas is nitrogen, and the reaction mater...

Embodiment 2

[0024] 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 concentration of 85% by mass was added, and then refluxed for 6 hours. The obtained dark blue suspension mixture was filtered, the solid was washed with acetone, and dried at 100°C for 24 hours to obtain the precursor of the VPO catalyst. The dried precursor was loaded into a self-made quartz groove with a volume ratio of 1.5% In a butane / air atmosphere, the temperature was raised from room temperature to 400°C at a rate of 2°C / min, and then kept at this temperature for 15 hours. The activated middle layer catalyst was taken and crushed to obtain 20-40 mesh particles for activity testing. .

[0025] Get above-mentioned catalyst 5g, carry out the continuous reaction of acetic acid and formaldehyde to produce acrylic acid in fixed-bed reactor, reaction temperature 340 ℃, r...

Embodiment 3

[0027]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 concentration of 85% by mass was added, and then refluxed for 6 hours. The obtained dark blue suspension mixture was filtered, the solid was washed with acetone, and dried at 100°C for 24 hours to obtain the precursor of the VPO catalyst. The dried precursor was loaded into a self-made quartz groove with a volume ratio of 1.5% In a butane / air atmosphere, the temperature was raised from room temperature to 400°C at a rate of 2°C / min, and then kept at this temperature for 15 hours. The activated upper layer catalyst was taken and crushed to obtain 20-40 mesh particles for activity testing. .

[0028] Get above-mentioned catalyzer 5g, carry out acetic acid and formaldehyde to produce the continuous reaction of acrylic acid in fixed-bed reactor, reaction temperature 340 ℃, re...

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Abstract

The invention discloses a vanadium-phosphorus-oxide (VPO) catalyst for preparing crylic acid or methyl acrylate by condensing acetic acid or methyl acetate with formaldehyde. A preparation method of the vanadium-phosphorus-oxide (VPO) catalyst comprises the following steps: reducing pentavalent vanadium (vanadium pentoxide) through monobenzyl alcohol or a mixed alcohol of benzyl alcohol / isobutyl alcohol, adding a polyethylene glycol (PEG6000) surfactant into an alcohol medium, then adding phosphoric acid, adjusting a ratio of P (phosphorus) / V (vanadium) to be 1.05 to prepare a catalyst precursor, and activating the catalyst precursor in pure nitrogen, pure air and 1.5%( volume fraction) butane-air mixture atmosphere. Since the PEG is added and / or the types of prepared medium alcohols and different precursor activation atmospheres are changed in the preparation process of the catalyst, a crystal phase shape and crystallinity, reaction reactivity of lattice oxygen, ratio of V<5+> / V<4+> on the surface of the catalyst can be significantly modulated, thus significantly modulating reaction behavior of the catalyst. The catalyst for preparing crylic acid (ester) by condensing acetic acid (methyl ester) with formaldehyde is high in catalytic efficiency, and by-products are few; a greatest generation rate of (crylic acid plus acrylic ester) can reach 32.1micromoles / gcat<-1> / min<-1>.

Description

technical field [0001] The invention relates to a VPO catalyst and its application in the reaction of acetic acid (methyl acetate) and formaldehyde to produce acrylic acid (acrylate). Background technique [0002] The production of acrylic acid has experienced the cyanohydrin method, the acrylonitrile hydrolysis method, the enone method, the Reppe method and the two-step oxidation method of propylene successively. The main methods currently used are acrylonitrile hydrolysis and propylene two-step oxidation. The acrylonitrile hydrolysis method is that acrylonitrile is first hydrolyzed by sulfuric acid to generate acrylamide, and then the corresponding acrylic acid is generated under acidic conditions. A large amount of low-value ammonium sulfate and other shortcomings, so now only a few companies use this production method. The two-step oxidation of propylene is currently the most widely used method for preparing acrylic acid in industry, accounting for about 85% of the tot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198C07C57/04C07C51/353C07C69/54C07C67/343
Inventor 季伟捷孙博姚瑶苏秦秦怡生
Owner NANJING UNIV
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