Catalyst for preparing pyromellitic dianhydride by oxidizing durene and preparation method thereof

A technology of durene and catalysts, which is applied in the field of catalysts for the production of pyromellitic dianhydride, can solve the problems of limited catalyst performance improvement and difficulty in exerting synergistic effects of elements, and achieve the goal of improving reaction activity, improving reaction performance, and improving effect of ability

Active Publication Date: 2020-04-28
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, pure mechanical mixing can only reflect the carrier effect from a macroscopic point of view, and it is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 241g of titanyl sulfate into 1.5L of deionized water and stir to dissolve it, then add 65.1g of cerium nitrate into the solution to form a mixed solution, then heat the mixed solution to 50°C and keep it warm. 25% concentrated ammonia water was added dropwise into the above mixed solution until the pH was 9. The above precipitate was filtered and washed until the pH of the filtrate was neutral. The filter cake was dried at 120°C for 5h, and then placed in a muffle furnace for sintering at 600°C for 4h to obtain the Ti-Ce-Ox composite oxide.

[0024] Heat 500mL of deionized water to 80°C, add 128g of oxalic acid and stir to dissolve it, then slowly add 46.8g of ammonium metavanadate, stir and react for 30min, then add 1.15g of ammonium dihydrogen phosphate, 7.04g of ammonium heptamolybdate, 0.58g of antimony trioxide and 4.3g of niobium oxalate were stirred to dissolve. Add 120 g of the prepared Ti-Ce-Ox composite oxide carrier into the solution, put it into a ball...

Embodiment 2

[0028] Add 224g of titanyl sulfate into 1.5L of deionized water and stir to dissolve it, then add 86.8g of cerium nitrate and 34.9g of zirconyl nitrate into the solution to form a mixed solution, then heat the mixed solution to 50°C and keep it warm. 25% concentrated ammonia water was added dropwise into the above mixed solution until the pH was 9. The above precipitate was filtered and washed until the pH of the filtrate was neutral. The filter cake was dried at 120°C for 5h and then placed in a muffle furnace for sintering at 600°C for 4h to obtain the Ti-Ce-Zr-Ox composite oxide.

[0029] Heat 500mL of deionized water to 80°C, add 120g of oxalic acid and stir to dissolve it, then slowly add 49.1g of ammonium metavanadate, stir and react for 30min, then add 3.45g of ammonium dihydrogen phosphate, 8.51g of ammonium heptamolybdate, 0.88g of antimony trioxide and 5.38g of niobium oxalate were stirred to dissolve. Add 125 g of the prepared Ti-Ce-Zr-Ox composite oxide support i...

Embodiment 3

[0033] Add 224g of titanyl sulfate into 1.5L of deionized water and stir to dissolve it, then add 112.5g of stannous chloride into the solution to form a mixed solution, then heat the mixed solution to 40°C and keep it warm. Add 1 mol / L sodium hydroxide aqueous solution dropwise to the above mixed solution until the pH is 10. The above precipitate was filtered and washed until no chloride ions were detected in the filtrate. The filter cake was dried at 120°C for 5h, and then placed in a muffle furnace for sintering at 650°C for 4h to obtain the Ti-Sn-Ox composite oxide.

[0034] Heat 500mL of deionized water to 80°C, add 128g of oxalic acid and stir to dissolve it, then slowly add 58.5g of ammonium metavanadate, stir and react for 30min, then add 8.05g of ammonium dihydrogen phosphate, 5.28g of ammonium heptamolybdate, 4.96g of ammonium metatungstate and 5.38g of niobium oxalate were stirred to dissolve. Add 140 g of the prepared Ti-Sn-Ox composite oxide carrier into the sol...

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Abstract

The invention provides a catalyst for preparing pyromellitic dianhydride by oxidizing durene and a preparation method thereof. The active component of the catalyst is composed of an active component,an auxiliary agent and a composite oxide carrier, and the composition is V-Ma-Ox/Ti-Mb-Ox, wherein V is the active component, the content of V in the active component is 10-30 wt%, Ma is the auxiliaryagent and is selected from one or more of Mo, W, P, Sb and Nb, and the molar ratio of the auxiliary agent Ma to the active component V is 0.01-0.5, the composite oxide carrier is Ti-Mb-Ox, Mb is oneor more of Ce, Zr and Sn, and the molar ratio of Mb to Ti is 0.1-0.8. A solid solution composite oxide with relatively high activation and oxygen species transmission capabilities is prepared througha coprecipitation or sol-gel method and then mixed with an active component solution to obtain active component slurry and then sprayed onto a spherical or annular catalyst carrier, dried and roastedto obtain the catalyst.

Description

technical field [0001] The invention relates to the technical field of catalysts, and relates to a catalyst for producing pyromellitic dianhydride (abbreviated as homoanhydride) by using durene as a raw material and a method for using the same. Background technique [0002] Homoanhydride is the main monomer material for polyimide synthesis. Polyimide has a high dielectric constant, excellent high temperature and low temperature resistance, and its service temperature ranges from -269 to 500 °C. Polyimide has good processability, and its products are indispensable in important fields such as aviation, aerospace, microelectronics, nanometers, liquid crystals, separation films, lasers, and flexible displays. With the continuous development of the national economy, the demand and production capacity of average anhydride are also increasing. [0003] Homoanhydride is mainly produced by durene oxidation method. According to the different phases of raw materials during the reacti...

Claims

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Application Information

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IPC IPC(8): B01J23/10B01J23/28B01J23/30B01J23/14B01J37/08B01J37/02C07D493/04
CPCC07D493/04B01J23/10B01J23/28B01J23/30B01J23/14B01J37/082B01J37/0215B01J23/002B01J2523/00B01J2523/3712B01J2523/47B01J2523/48
Inventor 张利杰冯晴曾贤君李贺孙彦民于海斌李晓云
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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