Continuous production technology for tetra-aryl-bi-metal porphyrin

A technology of bimetalloporphyrin and production process, applied in directions such as organic chemistry, to achieve the effects of improving product purity, reducing production cost, and improving yield

Active Publication Date: 2014-05-28
YUANJIANG HUALONG CATALYST TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this process can only be used for batch production, and there is still a large amount of DMF processing

Method used

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  • Continuous production technology for tetra-aryl-bi-metal porphyrin
  • Continuous production technology for tetra-aryl-bi-metal porphyrin
  • Continuous production technology for tetra-aryl-bi-metal porphyrin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] use figure 1The gas-liquid-solid heterogeneous reaction separation synchronous reactor shown, using tetra-p-propylphenylporphine, ferric chloride and pyridine as raw materials for air oxidation to prepare tetra-p-propylphenylporphyrin iron μ-dimer Products; among them, the diameter-to-height ratio of the stirring reaction tower is 1:20; there are two constant-temperature settling towers, the constant-temperature settling tower I and the constant-temperature settling tower II; the outlet of the reaction liquid is 4 / 9 of the height of the tower body from the top of the reaction tower.

[0041] Control the tee under the stirring reaction tower to connect the stirring reaction tower with the constant temperature settling tower I, and add toluene from the solvent inlet at the top of the constant temperature settling tower to the multiphase reaction separation synchronous reactor until the reaction zone of the stirring reaction tower is full and In the constant temperature se...

Embodiment 2

[0045] use figure 1 The gas-liquid-solid heterogeneous reaction separation synchronous reactor shown, using tetra-p-chlorophenylporphine, ferric chloride and triethylamine as raw materials for air oxidation to prepare tetra-p-chlorophenylporphyrin iron μ-dimer Products; among them, the diameter-to-height ratio of the stirring reaction tower is 1:30; there are two constant-temperature settling towers, the constant-temperature settling tower I and the constant-temperature settling tower II; the outlet of the reaction liquid is 4 / 9 of the height of the tower body from the top of the reaction tower.

[0046] Control the tee under the stirring reaction tower to connect the stirring reaction tower with the constant temperature settling tower I, and add xylene from the solvent inlet at the top of the constant temperature settling tower to the heterogeneous reaction separation synchronous reactor until it fills the reaction zone of the stirring reaction tower And in the constant tempe...

Embodiment 3

[0051] use figure 1 The gas-liquid-solid multiphase reaction separation synchronous reactor shown, using tetra-m-nitrophenylporphine, manganese acetate and sodium hydroxide as raw materials for air oxidation to prepare tetra-m-nitrophenylporphyrin manganese μ-dimer Products; among them, the diameter-to-height ratio of the stirring reaction tower is 1:35; there are two constant-temperature settling towers, the constant-temperature settling tower I and the constant-temperature settling tower II; the outlet of the reaction liquid is 1 / 3 of the height of the tower body from the top of the reaction tower.

[0052] Control the tee under the stirring reaction tower to connect the stirring reaction tower with the constant temperature settling tower I, and add DMF from the solvent inlet at the top of the constant temperature settling tower to the multiphase reaction separation synchronous reactor until the reaction zone of the stirring reaction tower is full and In the constant tempera...

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PUM

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Abstract

The invention discloses a continuous production technology for tetra-aryl-bi-metal porphyrin. The continuous production technology is that a resolvent is fed into a heterogeneous reaction and separation synchronous reactor, wherein the reactor comprises a stirring reaction tower and at least two constant-temperature settling towers, the stirring reaction tower comprises a reflow device, the constant-temperature settling towers are communicated with the bottom of the stirring reaction tower, and the interior of the stirring reaction tower comprises a gas-phase area and a reaction area; during reaction, the reaction area and the constant-temperature settling towers are full of the resolvent, and reaction raw materials such as tetra-aryl-porphin and divalent metal salt are fed into the stirring reaction tower and react with air led into the stirring reaction tower when the reaction area and the constant-temperature settling towers are heated to the backflow temperature of the resolvent; the tetra-aryl-bi-metal porphyrin generated during the reaction settles directly under the actino of gravity and enters into a constant-temperature settling tower from the reaction area; when the constant-temperature settling tower is fully filled with the tetra-aryl-bi-metal porphyrin, the stirring reaction tower is switched to be communicated with the other constant-temperature settle tower fully filled with the resolvent; the steps are carried out alternately to ensure continuous production. The technology can be used for producing high-purity tetra-aryl-bi-metal porphyrin continuously with high yield and low cost.

Description

technical field [0001] The invention relates to a continuous production process of tetraaryl double metal porphyrin, which belongs to the field of catalyst synthesis. Background technique [0002] Tetraaryl dimetalloporphyrins are important catalysts for the air oxidation of hydrocarbons. Chemically, tetraaryl bismetalloporphyrins [TRPPM] 2 O(3) using tetraaryl porphine TRPPH 2 (1) as the raw material is synthesized through the following process: [0003] [0004] First, the tetraaryl porphine TRPPH 2 (1) metallization in the presence of oxygen into the monometalloporphyrin TRPPMX (2), and then, bimetallation of the monometalloporphyrin TRPPMX (2) in an alkaline environment into the product tetraaryl bismetalloporphyrin [TRPPM ] 2 O(3). [0005] The above reaction is characterized by the transformation of monometalloporphyrin TRPPMX(2) into tetraaryl bismetalloporphyrin [TRPPM] 2 The double metallation process of O(3) is a reversible process, and the product tetraa...

Claims

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Application Information

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IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 郭灿城郭欣
Owner YUANJIANG HUALONG CATALYST TECH
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