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Method for preparing alkyl aromatic ferric sulfonate

A technology of aromatic sulfonic acid and ferric sulfonate, applied in the preparation of sulfonate, organic chemistry, etc., can solve the problems of oxide film damage, affecting the life of electrical properties, etc., and achieve the effect of simple preparation method

Inactive Publication Date: 2011-03-30
胡思棉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent application 200610156892.X has disclosed a kind of preparation method of alkylaromatic ferric sulfonate, because its raw material adopts iron trichloride, has caused chloride ion to be introduced in alkylaromatic ferric sulfonate, although by reaction reagent will Chloride ions are partially removed, but there will still be some chloride ions, which will cause damage to the oxide film layer of the electrolytic capacitor, thus affecting its electrical performance and life

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Ferric hydroxide and p-toluenesulfonic acid are placed in a reaction kettle with a reflux condenser according to a molar ratio of 1:2, and 3 times the pure water of the total amount of ferric hydroxide and p-toluenesulfonic acid is added therein, heated After reflux for 3 hours, cool to room temperature, take the upper liquid and filter to obtain the filtrate; spray-dry the obtained filtrate at a temperature of 300°C to obtain a reddish-brown iron p-toluenesulfonate crude product; wash the obtained crude product with an appropriate amount of ether 3 times, and the washing time 1 hour each to remove excess p-toluenesulfonic acid, then vacuum rotary steam the washed product to remove ether and moisture in the product to obtain the final product, reddish-brown iron p-toluenesulfonate powder; dissolve this reddish-brown powder in 1.5 Double n-butanol solution, under the condition of 60°C, carry out vacuum rotary evaporation to 55% concentration, and the obtained reddish-brow...

Embodiment 2

[0017] Place ferric hydroxide and p-toluenesulfonic acid in a reaction kettle with a reflux condenser in a molar ratio of 1:3, and add pure water 3 times the total amount of ferric hydroxide and alkylaromatic sulfonic acid , heated to reflux for 3 hours and then cooled to room temperature, the upper layer liquid was taken and filtered to obtain a filtrate; the obtained filtrate was spray-dried at a temperature of 200°C to obtain a reddish-brown iron p-toluenesulfonate crude product; the obtained crude product was washed with an appropriate amount of ether for 3 times, The washing time is 1 hour each to remove excess p-toluenesulfonic acid, and then the washed product is subjected to vacuum rotary evaporation to remove ether and water in the product to obtain the final product, reddish-brown iron p-toluenesulfonate powder; dissolve the reddish-brown powder In a 2.5-fold n-butanol solution, vacuum rotary steaming at 80°C to a concentration of 55%, the obtained reddish-brown trans...

Embodiment 3

[0019] Place ferric hydroxide and p-toluenesulfonic acid in a reaction kettle with a reflux condenser in a molar ratio of 1:4, and add pure water 3 times the total amount of ferric hydroxide and alkylaromatic sulfonic acid , heated to reflux for 3 hours and then cooled to room temperature, the upper layer liquid was taken and filtered to obtain a filtrate; the obtained filtrate was spray-dried at a temperature of 120° C. to obtain a reddish-brown iron p-toluenesulfonate crude product; the obtained crude product was washed with an appropriate amount of ether for 3 times, The washing time is 1 hour each to remove excess p-toluenesulfonic acid, and then the washed product is subjected to vacuum rotary evaporation to remove ether and water in the product to obtain the final product, reddish-brown iron p-toluenesulfonate powder; dissolve the reddish-brown powder In a 2-fold n-butanol solution, vacuum rotary steaming at 80°C to a concentration of 55%, the obtained reddish-brown trans...

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Abstract

The invention relates to a method for preparing alkyl aromatic ferric sulfonate, which comprises the following steps of: carrying out back flowing reaction of ferric hydroxide and alkyl aromatic sulfonic acid in water solution with the mol ratio of ferric hydroxide to alkyl aromatic sulfonic acid being 1 / 2 to 1 / 4; carrying out spray drying at the temperature between 120 DEG C and 300 DEG C to obtain crude products of the alkyl aromatic ferric sulfonate; washing the generated crude products with diethyl ether; removing the excessive alkyl aromatic sulfonic acid; and then, removing the diethyl ether and the water through vacuum distillation to obtain finished products. The method avoids the introduction of chloridion in the preparation process, is quite suitable for mass production, and is more applicable to solid-state electrolytic capacitor industry in the electronic industry.

Description

technical field [0001] The invention relates to a preparation method of alkyl aromatic iron sulfonate powder and its solution. Background technique [0002] Alkylaromatic iron sulfonate is an organic iron salt, which has good solubility in most organic solvents, and because it has a suitable oxidation potential, it can be used as an oxidant and oxidatively polymerized with a monomer to form a conductive polymer. Polymer, the conductive polymer is widely used in organic semiconductors, electrolytic capacitors, antistatic coatings and other fields due to its excellent conductivity and stability. It is also based on the emergence of the conductive polymer that the electrolytic capacitor has entered a new era of solid electrolytic capacitors. The traditional liquid electrolyte is replaced by a solid conductive polymer, which makes the electrical performance of the electrolytic capacitor more optimized and the working state more stable. [0003] Chinese patent application 200610...

Claims

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Application Information

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IPC IPC(8): C07C309/30C07C303/32
Inventor 胡思棉
Owner 胡思棉
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