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Vanadium phosphorus oxygen catalyst for preparing acrylic acid and acetic acid by oxidation of propane and preparation method thereof

A technology of acrylic acid and vanadium phosphorus oxide, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of disputes about the exact role and achieve the goal of increasing specific surface area and high propane conversion rate. Effect

Inactive Publication Date: 2004-12-29
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is generally believed that the vanadyl pyrophosphate phase [(VO) 2 P 2 o 7 ] is its main active phase, V 4+ is the main active species; with VOPO 4 in the form of V 5+ It is beneficial to improve the selectivity of acrylic acid, and the excess V 5+ will result in complete oxidation of the product, but for V 5+ The exact role of the

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  • Vanadium phosphorus oxygen catalyst for preparing acrylic acid and acetic acid by oxidation of propane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh V 2 o 5 2.5 grams, placed in isobutanol / benzyl alcohol (40ml / 35ml) mixture, after reflux at 140°C for 6 hours, add 1.4 grams of polyethylene glycol with a molecular weight of 6000, continue to reflux for 1 hour, press P / V=1.2 / 1 atomic ratio, 2.25ml of 85% phosphoric acid was added dropwise. Reflux was continued for 5 hours. Filter and dry to obtain a blue precipitate. The precipitate was dried in an air atmosphere at 120° C. to obtain a catalyst precursor powder. The prepared catalyst precursor powder was pressed into tablets under a pressure of 0.5MP, crushed, and 20-40 mesh sample particles were sieved and activated in a nitrogen atmosphere at 400 ° C for 2 hours, and then switched to the reaction atmosphere (C 3 h 8 / O 2 / He=17 / 30 / 53) continued activation for 6 hours to obtain an activated fresh catalyst with a specific surface area of ​​78m 2 / g, ICP detection results show that the P / V atomic ratio of the sample is 1.10. Weigh 1 gram of activated fre...

Embodiment 2

[0025] Weigh V 2 o 5 3.0 grams, placed in isobutanol / benzyl alcohol (48ml / 48ml) mixture, refluxed at 140°C for 4 hours, then added 2.1 grams of polyethylene glycol with a molecular weight of 10,000, continued to reflux for 2 hours, according to P / V=1.2 / 1 atomic ratio, 2.70ml of 85% phosphoric acid was added dropwise. Reflux was continued for 6 hours. Filter and dry to obtain a blue precipitate. The precipitate was dried in an air atmosphere at 100° C. to obtain a catalyst precursor powder. The prepared catalyst precursor powder was pressed into tablets under a pressure of 0.5MP, crushed, and 20-40 mesh sample particles were sieved and activated in a nitrogen atmosphere at 400 ° C for 2 hours, and then switched to the reaction atmosphere (C 3 h 8 / O 2 / He=17 / 30 / 53) continued activation for 6 hours to obtain an activated fresh catalyst with a specific surface area of ​​72m 2 / g, ICP detection results show that the P / V atomic ratio of the sample is 1.08. Weigh 1 gram of...

Embodiment 3

[0027] Weigh V 2 o 5 3.2 grams, placed in isobutanol / benzyl alcohol (35ml / 35ml) mixed solution, after reflux at 140°C for 6 hours, add 1.5 grams of polyethylene glycol with a molecular weight of 6000, continue to reflux for 1 hour, press P / V=1.2 / 1 atomic ratio, 2.88ml of 85% phosphoric acid was added dropwise. Reflux was continued for 6 hours. Filter and dry to obtain a blue precipitate. The precipitate was dried in an air atmosphere at 120° C. to obtain a catalyst precursor powder. The prepared catalyst precursor powder was pressed into tablets under a pressure of 0.5MP, crushed, and 20-40 mesh sample particles were sieved and activated in a nitrogen atmosphere at 400 ° C for 2 hours, and then switched to the reaction atmosphere (C 3 h 8 / O 2 / He=17 / 30 / 53) continued activation for 6 hours to obtain an activated fresh catalyst with a specific surface area of ​​76m 2 / g, ICP detection results show that the P / V atomic ratio of the sample is 1.12. Weigh 1 gram of activa...

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Abstract

The VPO catalyst is prepared with V2O2 and phosphoric acid in mixed isobutanol-benzyl alcohol solvent, and has polyglycol as dispersant. It has P / V atom rati of 1.1, specific surface area as high as 70-78 sq m / g and main material phase of vanadyl pyrophosphate. It is used the catalyst for oxidizing propane with air to preparing acrylic acid and acetic acid, and has single pass converting rate at the reaction temperature range of 380-400 deg.c of 37-72 % typically, acrylic acid selectivity of 5-35 % and total acrylic acid and acetic acid selectivity of 19-83 %. Under proper reaction condition, it has the propane converting rate of 40.3 %, acrylic acid selectivity of 33.8 %, acetic acid selectivity of 49.4 %, acrylic acid yield of 13.6 %, total acrylic acid and acetic acid yield of 33.5 % and space-time yield obviously higher than that with available similar catalyst. The preparation process of the catalyst is also disclosed.

Description

1. Technical field [0001] This invention relates to vanadium phosphorus oxygen catalysts and the partial oxidation of propylene with air over the catalysts for the preparation of acrylic acid and acetic acid. 2. Technical background [0002] Acrylic acid (AA for short) and its esters are very important organic chemical raw materials. Its unsaturated double bonds are prone to self-polymerization or multi-polymerization with other unsaturated hydrocarbons to form a variety of polymer materials with different properties and uses. Such as polyacrylate, etc. They are widely used in paint, chemical fiber, textile, light industry and other industries, as well as oil exploration, oil additives and so on. New uses are still being developed. In recent years, the production capacity of acrylic acid and its esters in the world has increased steadily. In 1995, the output of acrylic acid and its esters was 2.47 million tons and 1.77-2.04 million tons respectively. 2.65 million tons, th...

Claims

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Application Information

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IPC IPC(8): B01J27/198C07C51/215C07C53/08C07C57/04
Inventor 季伟捷李秀凯赵静张志炳陈懿
Owner NANJING UNIV