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Continuous production process of tetraaryl porphin

A production process, porphin technology, applied in the field of continuous production process of tetraaryl porphine, can solve the problems of increasing a large amount of solvent separation, not suitable for industrial production, high production cost, etc., achieve high-selectivity continuous production, and avoid recycling The effect of high processing and production costs

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

Because the solubility of tetraaryl porphine and tetraaryl chlorphine in inorganic and organic solvents is very small, no matter it is the separation method of chromatographic column or the method of adding chemical oxidant, it is necessary to increase the separation of a large amount of solvents, and there are many procedures and solvents. Large loss, high production cost, not suitable for industrial production

Method used

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  • Continuous production process of tetraaryl porphin
  • Continuous production process of tetraaryl porphin
  • Continuous production process of tetraaryl porphin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] use figure 1 The gas-liquid-solid multiphase reaction separation synchronous reactor shown in the figure uses p-propylbenzaldehyde and pyrrole as raw materials for air oxidation to prepare tetra-p-propylphenylporphin products; wherein, the diameter-to-height ratio of the stirred reaction tower is 1:20 ; There are two constant temperature settling towers with the same structure and size, 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.

[0038]Control the tee under the stirring reaction tower to connect the stirring reaction tower with the constant temperature settling tower I, and add acetic acid 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 ...

Embodiment 2

[0042] use figure 1 The gas-liquid-solid heterogeneous reaction separation synchronous reactor shown in the figure uses p-chlorobenzaldehyde and pyrrole as raw materials to carry out air oxidation to prepare tetra-p-chlorophenylporphin products; wherein, the diameter-to-height ratio of the stirring reaction tower is 1:25; There are constant temperature settling tower I and constant temperature settling tower II, two constant temperature settling towers with the same structure and size; the outlet of the reaction liquid is 1 / 3 of the height of the tower body from the top of the reaction tower.

[0043] 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...

Embodiment 3

[0047] use figure 1 The gas-liquid-solid multiphase reaction separation synchronous reactor shown in the figure uses m-nitrobenzaldehyde and pyrrole as raw materials for air oxidation to prepare tetra-m-nitrophenylporphine products; wherein, the diameter-to-height ratio of the stirred reaction tower is 1:35 ; There are two constant temperature settling towers with the same structure and size, 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.

[0048] 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 temperature s...

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Abstract

The invention discloses a continuous production process of tetraaryl porphin. The process is as follows: firstly, adding a solvent into a multi-phase reaction separating 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 internally 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 reaction materials pyrrole and aromatic aldehyde into the stirring reaction tower to contact and react with inlet air when the temperature is increased to the reflux temperature of the solvent, directly settling the tetraaryl porphin generated by the reaction into the constant-temperature settling towers from the reaction region under gravity action until the constant-temperature settling tower are filled up with the tetraaryl porphin, and switching the stirring reaction tower to be communicated with the other constant-temperature settling tower filled up with the solvent, and carrying out the process alternatively to realize continuous production. The continuous production process disclosed by the invention can be used for continuously producing high-purity tetraaryl porphin with high yield and low cost.

Description

technical field [0001] The invention relates to a continuous production process of tetraaryl porphine, which belongs to the field of organic synthesis. Background technique [0002] Tetraarylporphines are important luminescent materials and color developers, and are also raw materials for the synthesis of metalloporphyrin catalysts. Chemically, tetraarylporphines are formed from pyrrole and aromatic aldehydes via the following process: [0003] [0004] First, pyrrole and aromatic aldehydes are acid-catalyzed to form linear polymers (1), followed by intramolecular dehydration and ring-forming of linear polymers (1) with n = 4 to form tetraaryl chlorin (2), and then tetraaryl chlorin The target molecule tetraaryl porphine (3) was generated by reducing two hydrogen atoms through oxidative dehydrogenation of the base chlorin (2). In the above reaction process, the formation process of compounds (1) and (2) is a reversible process, while the formation process of compound (3...

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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