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Synthetic process and special equipment for substituted bis [tetraphenylporphinatoiron]

A technology based on double iron porphyrin and synthesis process, applied in the direction of organic compound/hydride/coordination complex catalyst, organic chemistry, physical/chemical process catalyst, etc. Synthesize problems such as tetraphenyl diferric porphyrin to achieve the effects of improving product purity, saving organic solvents and reducing production costs

Active Publication Date: 2013-11-06
YUANJIANG HUALONG CATALYST TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Tetraphenyldiferric porphyrin is an important catalyst for the air oxidation of hydrocarbons; there is no industrial synthesis of tetraphenyldiferric porphyrin
But this method also generates substituted tetraphenyl monoiron porphyrin while generating substituted tetraphenyl bis-iron porphyrin, and column chromatography separation is required to obtain pure substituted tetraphenyl bis-iron porphyrin compound, and the procedure is complicated
This method is also not suitable for the industrial production of substituted tetraphenyl bisiron porphyrin

Method used

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  • Synthetic process and special equipment for substituted bis [tetraphenylporphinatoiron]
  • Synthetic process and special equipment for substituted bis [tetraphenylporphinatoiron]
  • Synthetic process and special equipment for substituted bis [tetraphenylporphinatoiron]

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Refer to attached picture : The metallization reactor is composed of a reaction tank 1; a reflux device 1-3 and a water separator 1-2 are jointly formed, and a stirring device 1-1 is provided in the reaction tank 1; a raw material inlet 1-4, an air inlet 1-5, air outlet 1-6. There is another crystallizer 2, and the outlet pipe at the bottom of the crystallizer communicates with the filtrate storage 3; the reaction mixture overflows or is pumped into the crystallizer 2 for crystallization; the filtrate enters the filtrate storage 3. The filtrate in the filtrate storage 3 is pumped into the organic solvent recovery tower 5 through the pump 4, and enters the organic solvent storage 6 after being dehydrated by the ion exchange resin 5-1, and the organic solvent storage is connected with the reaction tank 1 through the pipeline and the circulation pump 7 to realize organic solvent circulation Use; the waste at the bottom of the recovery tower 5 is pumped into the waste pool...

Embodiment 2

[0023] 2000 L of reaction solvent DMF, 400 moles of tetraphenylporphine and 400 moles of ferrous chloride were pumped into a 3000 L metallization reactor, and stirring was started. Then air was introduced and heated to DMF reflux. After 0.2 hours of reaction, 250 moles of NaOH solid was added, and the reaction was continued for 1 hour before heating was stopped. The above reaction mixture was overflowed into a crystal separator for cooling and crystallization, and suction filtered to obtain solid tetraphenyldiferric porphyrin. The filtrate is pumped into the solvent rectification tower to recover 1900 L DMF, which is dehydrated by ion exchange resin and recycled. The residue of thick matter in the solvent rectification tower is pumped out while it is hot. The solid tetraphenyldiferric porphyrin obtained by suction filtration was washed with hot water and then industrial ethanol to obtain pure tetraphenyldiferric porphyrin with a yield of 98%.

Embodiment 3

[0025] Reaction equipment is identical with embodiment 1. The production process is as follows: 1000 L of propionic acid and 1000 L of DMF, 1000 moles of tetra-p-chlorophenylporphin and 2000 moles of ferrous acetate are pumped into a 3000 L metallization reactor, and stirring is started. Air was then introduced and heated to reflux. After 0.3 hours of reaction, 375 moles of NaOH solids were added, and the reaction was continued for 0.5 hours before heating was stopped. The above reaction mixture was overflowed into a crystal separator for cooling and crystallization, and suction filtered to obtain solid tetra-p-chlorophenyl bis-iron porphyrin. The filtrate is pumped into the solvent rectification tower to recover 920 L propionic acid and 980 L DMF, which are dehydrated by ionexchange resin and recycled. The residue of thick matter in the solvent rectification tower is pumped out while it is hot. The tetra-p-chlorophenyl bis-porphyrin solid obtained by suction filtration was ...

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Abstract

The invention discloses a synthetic process and special equipment for substituted bis [tetraphenylporphinatoiron]. An organic solvent as well as materials comprising substituted tetraphenylporphine and ferric are added in a metallic reactor for heating and refluxing for 0.2-0.5h under the condition of inputting 1 atm of air to synthesize substituted tetraphenylporphyrins; then solid NaOH is added into the same reactor for continuously reacting for 0.5-2h to implement dimerization on the substituted tetraphenylporphyrins, and pure substituted bis [tetraphenylporphinatoiron] is obtained through crystallization and purification. The synthetic yield of the substituted bis [tetraphenylporphinatoiron] is more than 95 percent and the recovery rate of the organic solvent is more than 95 percent.

Description

technical field [0001] The invention relates to the synthesis field of chemical product catalysts; in particular, it relates to a synthesis process and equipment for substituted tetraphenyldiiron porphyrin. Background technique [0002] Tetraphenyldiferric porphyrin is an important catalyst for the air oxidation of hydrocarbons; there is no industrial synthesis of tetraphenyldiferric porphyrin at present. Laboratory synthesis is usually to react substituted tetraphenyl porphyrin and iron salt in DMF solvent back flow, and obtain tetraphenyl monoiron porphyrin through column chromatography separation, then, by tetraphenyl mono iron porphyrin and base in benzene or Reaction in chloroform solvent, solvent distillation and column chromatographic separation to obtain tetraphenyl bis-iron porphyrin. Since the substituted tetraphenyl monoiron porphyrin and the substituted tetraphenyl bis iron porphyrin have very little solubility in benzene or chloroform solvent, a large amount of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22B01J31/22
Inventor 郭灿城罗伟平
Owner YUANJIANG HUALONG CATALYST TECH