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Prepn process of ferric alkyl aryl sulfonate

A technology of aromatic sulfonic acid and ferric sulfonate, applied in sulfonate preparation, organic chemistry, etc., can solve the problems of shortened product life, poor stability, increased impedance and loss, etc., and achieve low raw material cost Effect

Active Publication Date: 2007-11-07
湖北赛尔新能源材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The presence of a small amount of water reduces the conductivity and stability of the polymer produced. When applied to solid capacitors, the impedance and loss increase, and the life of the product is shortened.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put 1 mole of ferric chloride hexahydrate and 3 moles of p-toluenesulfonic acid monohydrate into a 1-liter three-necked flask equipped with a reflux condenser, add 250 milliliters of absolute ethanol, heat to reflux for half an hour, and then Under vacuum and reduced pressure, ethanol and water were completely removed. After the solvent was completely removed, the temperature was raised to 160° C., and the vacuum degree was kept at 2 KPa for 3 hours to obtain a completely dehydrated reddish-brown crude product. Re-dissolve the crude product in absolute ethanol, add an appropriate amount of reactive reagents, remove traces of chloride ions and sulfate ions, filter to remove insoluble matter, remove the solvent, and wash with ether three times to remove free p-toluenesulfonic acid , and recrystallized with a mixed solvent of methanol and acetonitrile at a ratio of 1:5 (v / v) to obtain good orange crystals.

[0037] The obtained orange crystals were kept in a vacuum oven at...

Embodiment 2

[0039] Put 1 mole of anhydrous ferric chloride and 3 moles of p-toluenesulfonic acid monohydrate into a 1-liter three-necked flask equipped with a reflux condenser, add 250 milliliters of absolute ethanol, heat to reflux for half an hour, and then Under vacuum and reduced pressure, ethanol and water were completely removed. After the solvent was completely removed, the temperature was raised to 180° C., and the vacuum degree was kept at 2 KPa for 3 hours to obtain a reddish-brown crude product. Re-dissolve the crude product in absolute ethanol, add an appropriate amount of reactive reagents, remove traces of chloride ions and sulfate ions, filter to remove insoluble matter, remove the solvent, and wash with ether three times to remove excess p-toluenesulfonic acid , and recrystallized from a mixed solvent of methanol and acetonitrile to obtain good orange crystals.

[0040] The obtained orange crystals were placed in a vacuum oven at 70°C for 20 hours. Dissolve it in excess n...

Embodiment 3

[0042] Put 1 mole of anhydrous ferric chloride and 2 moles of p-toluenesulfonic acid monohydrate into a 1-liter three-necked flask equipped with a reflux condenser, add 250 milliliters of absolute ethanol, heat to reflux for half an hour, and then Under vacuum and reduced pressure, ethanol and water were completely removed. After the solvent was completely removed, the temperature was raised to 120° C., and the vacuum degree was kept at 2 KPa for 3 hours to obtain a reddish-brown crude product. Re-dissolve the crude product in absolute ethanol, add an appropriate amount of reactive reagents, remove traces of chloride ions and sulfate ions, filter to remove insoluble matter, remove the solvent, and wash with ether three times to remove excess p-toluenesulfonic acid , and recrystallized from a mixed solvent of methanol and acetonitrile to obtain good orange crystals.

[0043]The obtained orange crystals were placed in a vacuum oven at 70°C for 20 hours. It was dissolved in exce...

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Abstract

The preparation process of ferric alkyl aryl sulfonate includes the following steps: reflux reaction between anhydrous ferric trichloride or ferric trichloride hexahydrate and alkyl aryl sulfonic acid in alcohol solution, eliminating solvent and hydrogen chloride gas at high temperature and low pressure to produce coarse product; washing with ethyl ether to eliminate excessive p-toluene sulfonic acid, and re-crystallizing in mixed solvent of methanol and acetonitrile to obtain purified ferric alkyl aryl sulfonate. The present invention provides also one other process for preparing ferric long chain (benzene) sulfonate. The present invention has low material cost and high product purity, and the product is used in electronic industry.

Description

technical field [0001] The invention relates to the synthesis and purification method of an electronic-grade alkyl aromatic iron sulfonate and its solution. Background technique [0002] Alkylaromatic iron sulfonates are widely used as catalysts and oxidants commonly used in organic synthesis. Compared with inorganic iron salts, due to its relatively large lipophilic anion, it has good solubility in most organic solvents, so it can be widely used in organic reaction processes as catalysts, oxidants or reaction raw materials. Because of its suitable oxidation potential and the good doping function of the anions released after reduction, it is very suitable for the oxidation synthesis of PEDOT, PPY and PAN-type conductive polymers. The conductive polymers generated by oxidation polymerization are not only It has excellent conductivity, and due to the volume steric effect of doping on ions, it has good stability in air and high temperature conditions, so this type of conductiv...

Claims

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Application Information

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IPC IPC(8): C07C309/30C07C303/32
Inventor 徐永进廖振华陈建军刘伟强
Owner 湖北赛尔新能源材料有限公司
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