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A kind of zeolite-like porous material and its preparation method and application

A porous material and zeolite-like technology, applied in the field of synthetic ammonia, can solve problems such as increasing catalyst cost, and achieve the effects of low cost, easy industrial production and mild reaction conditions

Inactive Publication Date: 2011-12-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patents CN1293593, CN1099353, US3839229, etc. mainly focus on the improvement of the original molten iron catalyst, while the catalysts reported in patents CN1401426, CN1270081A, DE2748972, GB2034194, WO84-3642, US4142993, US3830753 and US4600571 all use ruthenium as the active component Although the new ruthenium-based ammonia synthesis catalyst can operate at low temperature and low pressure, and has a long life, it can save a lot of energy consumption. However, due to the rarity and high cost of ruthenium, it will inevitably cause problems such as a substantial increase in the cost of the catalyst.

Method used

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preparation example Construction

[0020] The preparation method of zeolite-like porous catalyst of the present invention comprises the following steps:

[0021] (1) Prepare porphyrin or porphyrin derivatives by reacting pyrrole with corresponding aldehyde.

[0022] The aldehydes are p-carboxybenzaldehyde, m-carboxybenzaldehyde, p-phosphonate benzaldehyde, m-phosphonate benzaldehyde, p-sulfonate benzaldehyde, m-sulfonate benzaldehyde and the like.

[0023] (2) Using the corresponding metal salt and porphyrin or porphyrin derivative to obtain the corresponding metalloporphyrin or metalloporphyrin derivative by reflux reaction in DMF solvent.

[0024] The metal salts are nitrates, acetates, perchlorates, halides, sulfates and the like of Fe, Ni, Co, Ru, Pd, Pt, Rh, Ta, Re, Mo, W and other metals.

[0025] (3) In a mixed solvent, the metal porphyrin or porphyrin derivative carrier is reacted with a metal salt to obtain a dark brown-red solution. After a period of time, dark brown crystals are obtained, and then f...

Embodiment 1

[0033] In a mixed solvent, such as: DMF, chlorobenzene, methanol and acetic acid, react the benzoic acid derivative of palladium porphyrin with the metal salt nitric acid at 80°C to obtain a dark brownish red solution. After ten days, dark brown crystals were obtained, which were then filtered, washed with solvents such as DMF, ethanol and ether, and finally dried in air. The compound is a porous zeolite compound through single crystal X-ray diffraction, PLATON calculation and BET specific surface area calculation. The crystallization solvent of the compound in the channel can be removed by heating and vacuuming. Thermal weight loss and powder X-ray diffraction showed that the overall skeleton of the compound remained unchanged after losing solvent molecules.

Embodiment 2

[0035] Catalyst activity evaluation was carried out in MRCS8004 device. The inner diameter of the reactor is a fixed bed of 2 mm, the bulk volume is 0.03 mL, the reaction gas is a 1:3 mixture of nitrogen and hydrogen, the gas flow rate is 12 mL / min, and the catalyst is activated at 200 ° C for 30 minutes. The results show that ammonia gas begins to be generated at room temperature, and the conversion rate reaches 7% at 310°C, and is not limited by traditional thermodynamic conditions.

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Abstract

The invention discloses a zeolite-like porous material, a preparation method and application thereof. The zeolite-like porous material consists of a porphyrin or porphyrin derivative basic carrier, transitional metal ion active components and metal ion nodes. When the zeolite-like porous material is used for a catalyst of synthetic ammonia, reaction conditions are mild, and catalytic reaction can be carried out under the normal pressure with low cost, high conversion rate and no limit of thermodynamic conditions. If the zeolite-like porous material replaces the prior industrial synthetic ammonia catalyst, cost can be greatly reduced, and industrial mass production is easy to realize. The zeolite-like porous material can be widely applied to the synthetic ammonia industry.

Description

technical field [0001] The invention relates to the technical field of ammonia synthesis, in particular to a zeolite-like porous material, a preparation method and application. Background technique [0002] Although ammonia synthesis catalysts have been researched for nearly a century, the traditional molten iron catalysts are still widely used at present, with alumina, potassium oxide, etc. ), low activity (conversion rate 15-25%), which must become the restrictive factor of energy saving and consumption reduction, and has strict requirements on equipment materials. Therefore, it is imperative to develop a new generation of high-efficiency and energy-saving catalysts for ammonia synthesis. Patents CN1293593, CN1099353, US3839229, etc. mainly focus on the improvement of the original molten iron catalyst, while the catalysts reported in patents CN1401426, CN1270081A, DE2748972, GB2034194, WO84-3642, US4142993, US3830753 and US4600571 all use ruthenium as the active component...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/04C01C1/04
CPCY02P20/52
Inventor 吴传德解明华郑小明楼辉
Owner ZHEJIANG UNIV
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