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Synthetic process and special equipment for substituted bis [tetraphenylporphinatoiron]

A technology of tetraphenylbisiron porphyrin and base biferric porphyrin is applied in the field of synthesis of chemical product catalysts, and can solve the problems of unsuitability for industrial production, complicated procedures, and no industrial synthesis of tetraphenylbisferric porphyrin, and the like, Achieve the effect of improving product purity, saving organic solvents and reducing production costs

Active Publication Date: 2012-04-11
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
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Effect test

Embodiment 1

[0021] Reference attached Figure :The metallization reactor is composed of reaction tank 1; reflux device 1-3 and water separator 1-2 together, with stirring device 1-1 in reaction tank 1; raw material inlet 1-4 and air inlet are provided on the top 1-5, air outlet 1-6. There is another crystallization separator 2, and the outlet pipe at the bottom of the crystallization separator is connected with the filtrate storage 3; the reaction mixture is overflowed or pumped into the crystallization separator 2 for crystallization separation; the filtrate enters the filtrate storage 3. The filtrate in the filtrate storage 3 is pumped into the organic solvent recovery tower 5 by the pump 4, and then is dehydrated by the ion exchange resin 5-1 and then enters the organic solvent storage 6, which is connected to the reaction tank 1 through a pipeline and a circulating pump 7 to realize organic solvent circulation Use; the waste at the bottom of the recovery tower 5 is pumped into the wast...

Embodiment 2

[0023] Pump 2000 L of reaction solvent DMF, 400 moles of tetraphenylporphine and 400 moles of ferrous chloride into the 3000 L metallization reactor, and start stirring. Then air was passed through and heated to DMF reflux, 250 moles of NaOH solid was added after 0.2 hours of reaction, and the heating was stopped after the reaction continued for 1 hour. The above reaction mixture flows into a crystallization separator for cooling and crystallization, and suction filtration to obtain solid tetraphenyl diferroporphyrin. The filtrate is pumped into the solvent distillation tower to recover 1900 L DMF, which is recycled after dehydration by ion exchange resin. The residual thick substance in the solvent distillation tower is pumped out while it is hot. The solid tetraphenyl diferroporphyrin obtained by suction filtration was washed with hot water and then washed with industrial ethanol to obtain pure tetraphenyl diferroporphyrin with a yield of 98%.

Embodiment 3

[0025] The reaction equipment is the same as in Example 1. The production process is as follows: pump 1000 L propionic acid and 1000 L DMF, 1000 moles of tetra-p-chlorophenylporphine and 2000 moles of ferrous acetate into a 3000 L metallization reactor, and start stirring. Then air was passed through and heated to reflux. After 0.3 hours of reaction, 375 moles of NaOH solid was added, and the reaction was continued for 0.5 hours and then the heating was stopped. The above reaction mixture flows into a crystallization separator for cooling and crystallization, and suction filtration to obtain solid tetrap-chlorophenyl diferroporphyrin. The filtrate is pumped into the solvent rectification tower to recover 920 L propionic acid and 980 L DMF, which are recycled after being dehydrated by ionomer resin. The residual thick substance in the solvent distillation tower is pumped out while it is hot. The solid tetrap-chlorophenyl diferroporphyrin obtained by suction filtration was wash...

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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 field of synthesis of chemical product catalysts; specifically, it is a synthesis process and equipment for replacing tetraphenyl diferroporphyrin. Background technique [0002] Tetraphenyl bis-iron porphyrin is an important catalyst for the air oxidation of hydrocarbon compounds; there is no industrial synthesis process for tetraphenyl bis-iron porphyrin. Laboratory synthesis usually involves the reflux reaction of substituted tetraphenylporphine and iron salt in DMF solvent, and separation by column chromatography to obtain tetraphenylmonoiron porphyrin. Then, tetraphenylmonoironporphyrin and base are combined in benzene or Reaction in chloroform solvent, solvent distillation and column chromatography to obtain tetraphenyl diferroporphyrin. Since substituted tetraphenyl monoiron porphyrin and substituted tetraphenyl diferric porphyrin have little solubility in benzene or chloroform solvents, a large amount of solvent needs to...

Claims

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Application Information

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