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Continuous production process of tetraaryl metal porphyrin

An aryl metal and production process technology, applied in the field of continuous production technology of tetraaryl metalloporphyrin, can solve the problems of poor solubility of tetraaryl metalloporphyrin TRPPM, difficulty in product purification, increase in production cost, etc. Continuous production with high selectivity, avoiding the use of a large amount of solvent, and improving the yield

Active Publication Date: 2014-06-25
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 metal porphyrin
  • Continuous production process of tetraaryl metal porphyrin
  • Continuous production process of tetraaryl metal porphyrin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] use figure 1 The shown liquid-solid heterogeneous reaction separation synchronous reactor uses tetra-p-propyl phenyl porphine and cobalt acetate as raw materials for air oxidation to prepare tetra-p-propyl phenyl porphyrin cobalt product; wherein, the diameter-to-height ratio of the stirring reaction tower is It is 1:20; there are two constant temperature settling towers with the same size and structure as constant temperature settling tower I and constant temperature settling tower II; the reaction liquid outlet 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 and the constant temperature settling tower I, and add toluene from the solvent inlet at the top of the constant temperature settling tower into the multiphase reaction separation synchronous reactor until the reaction zone and In the constant temperature sedimentation tower I, when the temperat...

Embodiment 2

[0051] use figure 1 The shown liquid-solid heterogeneous reaction separation synchronous reactor uses tetra-p-methoxyphenylporphine and zinc acetate as raw materials for air oxidation to prepare tetra-p-methoxyphenylporphyrin zinc product; among them, the stirring reaction tower diameter The height ratio is 1:20; there are two constant temperature settling towers with the same size and structure as the constant temperature settling tower I and the constant temperature settling tower II; the reaction liquid outlet 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 and the constant temperature settling tower I, and add xylene from the solvent inlet on 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 filled When the temperature is increased to reac...

Embodiment 3

[0056] use figure 1 The shown liquid-solid heterogeneous reaction separation synchronous reactor uses tetra-p-chlorophenyl porphine and nickel acetylacetonate as raw materials for air oxidation to prepare tetra-p-chlorophenyl porphyrin nickel product; wherein the diameter-to-height ratio of the stirring reaction tower is 1:25; There are two constant temperature settling towers with the same size and structure, the constant temperature settling tower I and the constant temperature settling tower II; the reaction liquid outlet is 2 / 5 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 on the top of the constant temperature settling tower to the multiphase reaction separation synchronous reactor until the reaction zone and In the constant temperature settling tower I, when the temperature is i...

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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 metalloporphyrin, 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) generally uses tetraaryl porphyrin TRPPH 2 (1) In DMF with metal salt M 2+ Preparation of metallization: [0003] [0004] The tetraaryl trivalent metal porphyrin TRPPMX (3) is generally used in the presence of an oxidizing agent from the tetraaryl porphyrin TRPPH 2 (1) In DMF with metal salt M 2+ Preparation of metallization: [0005] [0006] Tetraarylporphine TRPPH 2 The metalization process is a reversible process. When preparing tetraarylmetalloporphyrin TRPPM, a large excess of metal salt is required; in addition, tetraarylporphine TRPPH 2 The solubility of TRPPM ​​and tetraarylmetalloporphyrin...

Claims

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Application Information

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