Catalyst for preparing pyromellitic dianhydride from durene through gaseous catalytic oxidation and preparation method thereof

A technology of pyromellitic dianhydride and gas-phase catalytic oxidation, which is applied in the fields of physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., can solve problems such as low yield, restriction of PMDA, and complex active components, and achieve Improve yield and purity, reduce production cost, and reduce resource consumption

Active Publication Date: 2011-04-06
常熟市知识产权运营中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The system has many catalyst active components, and the preparation process is relatively complicated, requiring a high space velocity of about 6000-10000h-1. Meanwhile, the yield of PMDA is also low, and the weight yield is only 84%-100%.
[0009] Chinese patent CN 1321543A discloses a catalyst for producing PMDA by gas-phase oxidation of durene, which can be produced by V 2 o 5 、TiO 2 , Nb 2 o 5 、Cs 2 O and P 2 o 5 and other active components can also be composed of V 2 o 5 、TiO 2 , Nb 2 o 5 、Na 2 O and B 2 o 3 However, the active components of the two catalytic systems are relatively complex, and the Nb

Method used

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  • Catalyst for preparing pyromellitic dianhydride from durene through gaseous catalytic oxidation and preparation method thereof

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0034] Example 1:

[0035] A) Prepare a vanadyl ammonium oxalate solution, the molar ratio of oxalic acid to distilled water is 1:21, put the weighed oxalic acid into a container filled with distilled water and equipped with a heating device and a stirrer, stir and heat up to 90°C. After the oxalic acid is fully dissolved, slowly add ammonium metavanadate, the molar ratio of ammonium metavanadate to oxalic acid is 0.4:1, continue the stirring reaction to obtain an ammonium vanadyl oxalate solution;

[0036] B) Prepare spraying liquid, follow V 2 O 5 : TiO 2 (Anatase): P 2 O 5 The molar ratio = 1:3.8:0.125 will (NH 4 ) 2 VO 3 , TiO 2 And (NH 4 ) 2 HPO 4 Add to the vanadyl ammonium oxalate solution obtained in step A), the vanadyl ammonium oxalate solution and TiO 2 The weight is 4.6:1 and stir evenly to obtain spray liquid;

[0037] C) Spraying: spray the spraying liquid obtained in step B) uniformly at 260°C on the surface of SiC spheres with a diameter of 4-6 mm as an inert carrier,...

Example Embodiment

[0040] Example 2:

[0041] A) Prepare vanadyl ammonium oxalate solution. The molar ratio of oxalic acid to distilled water is 1:23. Put the weighed oxalic acid into a container filled with distilled water and equipped with a heating device and a stirrer. Stir and heat to 60°C. After the oxalic acid is fully dissolved, slowly add ammonium metavanadate, the molar ratio of ammonium metavanadate to oxalic acid is 0.5:1, and continue the stirring reaction to obtain an ammonium vanadyl oxalate solution;

[0042] B) Prepare spraying liquid, follow V 2 O 5 : TiO 2 (Anatase): P 2 O 5 The molar ratio = 1:15:0.313 will (NH 4 ) 2 VO 3 , TiO 2 And (NH 4 ) 2 HPO 4 Added to the ammonium vanadyl oxalate solution obtained in step A), wherein the vanadyl ammonium oxalate solution and TiO 2 The weight ratio is 4.6:1, and stir evenly to obtain spraying liquid;

[0043] C) Spraying: the spraying liquid obtained in step B) is uniformly sprayed on the surface of the porcelain ring with a diameter of 4-6 mm...

Example Embodiment

[0046] Example 3:

[0047] The catalyst was prepared in the same way as in Example 2 and the catalyst activity was evaluated. The 50ml catalyst was put into a Φ25mm fixed bed reaction tube, the reaction hot spot temperature was controlled at 440-450°C, mesitylene was introduced, and air was used for oxidation. React for 2 hours. Catalyst load 60~80g / L·h, space velocity 4000~4600h -1 , The furnace temperature is 355-375°C, the weight yield of PMDA is 97%-103%, and the purity is above 95.5%.

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Abstract

The invention relates to a catalyst for preparing pyromellitic dianhydride from durene through gaseous catalytic oxidation and a preparation method thereof, belonging to the technical field of catalytic oxidation. The catalyst is characterized by comprising V2O5, TiO2 and P2O5, wherein the molar ratio of V2O5 to TiO2 to P2O5 is 1:3.750-15.000:0.125-0.313. The catalyst provided by the invention has the advantages of low airspeed, low energy consumption, high selectivity and high weight gain percentage during application, is helpful to energy saving and resource consumption reduction and is beneficial to increasing the yield and the purity of pyromellitic dianhydride and reducing the production cost for preparing pyromellitic dianhydride through gaseous catalytic oxidation. The provided preparation method of the catalyst has simple and succinct technological steps and can ensure the overall embodiment of the effect of the catalyst.

Description

technical field [0001] The invention belongs to the technical field of catalytic oxidation, and relates to a catalyst for preparing pyromellitic dianhydride by gas-phase catalytic oxidation of durene, and also relates to a preparation method of the catalyst. Background technique [0002] Pyromellitic dianhydride (PMDA for short) is an important organic chemical product intermediate with high added value, which is mainly used in the production of engineering plastics, coating additives, plastic additives Because of its excellent insulation performance, high and low temperature resistance and mechanical properties, PMDA is widely used in many fields such as electromechanical, aerospace and electronic industries. [0003] There are many industrial production methods of PMDA, such as gas-phase air catalytic oxidation, liquid-phase air oxidation, nitric acid oxidation and chromic acid oxidation, etc., but gas-phase catalytic oxidation is the main method. Since the gas-phase cata...

Claims

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Application Information

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IPC IPC(8): B01J27/198C07D493/04
Inventor 周宇峰张京通陈燕丹李凤娟余文丛丁建林
Owner 常熟市知识产权运营中心有限公司
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