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A kind of vpo catalyst and its application in the reaction of acetic acid (ester) and formaldehyde to produce acrylic acid (ester)

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: 2016-11-23
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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  • A kind of vpo catalyst and its application in the reaction of acetic acid (ester) and formaldehyde to produce acrylic acid (ester)
  • A kind of vpo catalyst and its application in the reaction of acetic acid (ester) and formaldehyde to produce acrylic acid (ester)
  • A kind of vpo catalyst and its application in the reaction of acetic acid (ester) and formaldehyde to produce acrylic acid (ester)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 4.8g vanadium pentoxide and 72ml benzyl alcohol were refluxed at 140°C for 6 hours, 2.1g PEG6000 was added to the reaction medium, after 1 hour, 6.45g of concentrated phosphoric acid with a mass percentage concentration of 85% was added, and then refluxed for 6 hours. The resulting 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 put into a self-made quartz tank with a volume ratio of 1.5% n-butyl In an alkane / air atmosphere, the temperature is increased from room temperature to 400°C at a heating rate of 2°C / min, and then kept at this temperature for 15 hours. The activated lower layer catalyst is compressed and crushed to obtain 20-40 mesh particles for activity testing .

[0022] Take 5g of the above catalyst and carry out the continuous reaction of acetic acid and formaldehyde in a fixed bed reactor. The reaction temperature is 360°C, the re...

Embodiment 2

[0024] 4.8g vanadium pentoxide and 72ml benzyl alcohol were refluxed at 140°C for 6 hours, 2.1g PEG6000 was added to the reaction medium, after 1 hour, 6.45g of concentrated phosphoric acid with a mass percentage concentration of 85% was added, and then refluxed for 6 hours. The resulting 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 put into a self-made quartz groove with a volume ratio of 1.5%. In a butane / air atmosphere, the temperature is increased from room temperature to 400°C at a heating rate of 2°C / min, and then kept at this temperature for 15 hours. The activated middle layer catalyst is compressed into tablets and crushed to 20-40 mesh particles for activity testing .

[0025] Take 5g of the above catalyst and carry out the continuous reaction of acetic acid and formaldehyde to produce acrylic acid in a fixed bed reactor. The reaction tem...

Embodiment 3

[0027] 4.8g vanadium pentoxide and 72ml benzyl alcohol were refluxed at 140°C for 6 hours, 2.1g PEG6000 was added to the reaction medium, after 1 hour, 6.45g of concentrated phosphoric acid with a mass percentage concentration of 85% was added, and then refluxed for 6 hours. The resulting 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 put into a self-made quartz groove with a volume ratio of 1.5%. In a butane / air atmosphere, the temperature is increased from room temperature to 400°C at a heating rate of 2°C / min, and then kept at this temperature for 15 hours. The activated upper catalyst is compressed into tablets and crushed to 20-40 mesh particles for activity testing .

[0028] Take 5g of the above catalyst and carry out the continuous reaction of acetic acid and formaldehyde to produce acrylic acid in a fixed bed reactor. The reaction temperatur...

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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 prepare acrylic acid (acrylate). Background technique [0002] The production of acrylic acid has experienced the cyanoethanol method, acrylonitrile hydrolysis method, ketene method, Reppe method and two-step oxidation method of propylene. The main methods currently used are acrylonitrile hydrolysis and propylene two-step oxidation. The acrylonitrile hydrolysis method is to first hydrolyze acrylonitrile with sulfuric acid to generate acrylamide, and then generate the corresponding acrylic acid under acidic conditions. The process is relatively simple, the reaction conditions are mild, and acrylamide can be produced at the same time, but the process has serious pollution and by-products. A large number of low-value ammonium sulfate and other shortcomings, so now only a few companies use this production method. The two-step propyle...

Claims

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Application Information

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