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Continuous Production Process of Tetraaryl Metalloporphyrins

A kind of aryl metal porphyrin production process technology, which is applied in the continuous production process field of tetraaryl metal porphyrin, can solve the problems such as poor solubility of tetraaryl metal porphyrin TRPPM, increase of production cost, difficulty in product purification, etc., and achieve Continuous production with high selectivity, increased yield, and the effect of avoiding the use of a large amount of solvents

Active Publication Date: 2016-03-02
YUANJIANG HUALONG CATALYST TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Tetraaryl porphine TRPPH 2 The metallation process of tetraaryl porphyrin TRPPH is a reversible process, and metal salt needs to be greatly excessive when preparing tetraaryl porphyrin TRPPM; In addition, tetraaryl porphyrin TRPPH 2 and the solubility properties of tetraaryl metalloporphyrin TRPPM ​​are not good, and the solubility of product tetraaryl metalloporphyrin TRPPM ​​is better than that of reactant tetraaryl porphyrin TRPPH 2 worse
The above-mentioned characteristics in the synthesis of tetraaryl metalloporphyrins lead to the difficulty of product purification and the treatment of a large amount of solvents in the production of industrial large-scale metalloporphyrins, which increases production costs.

Method used

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  • Continuous Production Process of Tetraaryl Metalloporphyrins
  • Continuous Production Process of Tetraaryl Metalloporphyrins
  • Continuous Production Process of Tetraaryl Metalloporphyrins

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] use figure 1 The liquid-solid heterogeneous reaction separation synchronous reactor is shown, and tetra-p-propylphenylporphyrin and cobalt acetate are used as raw materials for air oxidation to prepare tetra-p-propylphenylporphyrin cobalt products; wherein, the diameter-to-height ratio of the stirred reaction tower The ratio is 1:20; there are two constant temperature settling towers of the same size and structure, 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.

[0047] 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...

Embodiment 2

[0051] use figure 1 The liquid-solid heterogeneous reaction separation synchronous reactor shown, uses tetra-p-methoxyphenyl porphyrin and zinc acetate as raw materials to carry out air oxidation to prepare tetra-p-methoxyphenyl porphyrin zinc product; wherein, the stirring reaction tower diameter The height ratio is 1:20; there are two constant temperature settling towers of the same size and structure, 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.

[0052] 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 t...

Embodiment 3

[0056] use figure 1 The shown liquid-solid multiphase reaction separation synchronous reactor uses tetra-p-chlorophenylporphine and nickel acetylacetonate as raw materials to carry out air oxidation to prepare tetra-p-chlorophenylporphyrin nickel product; wherein, the ratio of diameter to height of the stirred reaction tower is 1:25; There are two constant temperature settling towers of the same size and structure, the constant temperature settling tower I and the constant temperature settling tower II; the outlet of the reaction liquid is 2 / 5 of the height of the tower body from the top of the reaction tower.

[0057] 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 consta...

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PUM

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Abstract

The invention discloses a continuous production process of tetraaryl metal porphyrin. The process is as follows: firstly, adding a solvent into a multi-phase reaction separation synchronous reactor, wherein the reactor comprises a stirring reaction tower with a reflux device, and at least two constant-temperature settling towers communicated with the bottom of the stirring reaction tower, and the stirring reaction tower comprises a gas-phase region and a reaction region; during reaction, filling the solvent in the reaction region and the constant-temperature settling towers, adding the reaction material tetraaryl porphyrin and a metal salt into the stirring reaction tower for stirring when a temperature is increased to reach a reflux temperature of the solvent or reacting under the condition of ventilating air, directly settling the tetraaryl metal porphyrin generated by the reaction under gravity action to enter the constant-temperature settling towers until the constant-temperature settling tower is filled up with the tetraaryl metal porphyrin, switching the stirring reaction tower to communicate with the other constant-temperature settling tower filled with the solvent and carrying out the process alternatively to realize continuous production. The continuous production process disclosed by the invention can continuously produce high-purity tetraaryl metal porphin with high yield and low cost.

Description

technical field [0001] The invention relates to a continuous production process of tetraaryl metal porphyrin, which belongs to the field of catalyst synthesis. Background technique [0002] Metalloporphyrins are widely used as catalysts for the air oxidation of hydrocarbons and can also be used as luminescent materials. In the laboratory, tetraaryl divalent metalloporphyrin TRPPM ​​(2) is commonly used tetraaryl porphine TRPPH 2 (1) in DMF with metal salt M 2+ The metallization preparation: [0003] [0004] The tetraaryl trivalent metalloporphyrin TRPPMX (3) is commonly used in the presence of an oxidizing agent from the tetraaryl porphyrin TRPPH 2 (1) in DMF with metal salt M 2+ The metallization preparation: [0005] [0006] Tetraaryl porphine TRPPH 2 The metallation process of tetraaryl porphyrin TRPPH is a reversible process, and metal salt needs to be greatly excessive when preparing tetraaryl porphyrin TRPPM; In addition, tetraaryl porphyrin TRPPH 2 and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 郭灿城郭欣
Owner YUANJIANG HUALONG CATALYST TECH
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