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High-purity iron p-toluenesulfonate preparation method

A technology of ferric p-toluenesulfonate and p-toluenesulfonic acid, which is applied in the field of electronic chemicals, can solve the problems of shortening the service life of electrolytic capacitors, corrosion of oxide films by chloride ions, and difficulty in removing anions, and achieves high solubility and clean process. , the effect of low moisture

Inactive Publication Date: 2014-12-31
张 雪琴
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Currently reported reactions using ferric chloride, ferric sulfate, ferric nitrate or ferric formate as an iron source generally have the following problems: various anions are difficult to remove, and trace solvent residues cause ferric p-toluenesulfonate to be used as an electronic material. When the oxidant is used as a dopant, the residual chloride ions, sulfate ions or nitrate ions will seriously corrode the oxide film, resulting in shortened service life and poor performance of electrolytic capacitors, which cannot meet the requirements of electronic chemicals well.

Method used

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  • High-purity iron p-toluenesulfonate preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 1000g of deionized water, 500g of p-toluenesulfonic acid and 100g of ferric hydroxide into a 2000ml flask, heat the reaction temperature at 100-104°C, react for 5h, cool and filter. The filtrate was spray-dried to obtain 450 g of solids. Karl Fischer detected moisture<0.2%, particle size<25um, no chloride ions were detected, no nitrate ions were detected, and sulfate ions were 2ppm.

Embodiment 2

[0027] Add 500g of deionized water, 500g of p-toluenesulfonic acid and 100g of ferric hydroxide into a 2000ml flask, heat the reaction temperature at 105-110°C, react for 3h, cool and replenish water and filter. The filtrate was spray-dried to obtain 430 g of solids. Karl Fischer detected moisture<0.2%, particle size<25um, no chloride ions were detected, no nitrate ions were detected, and sulfate ions were 2ppm.

Embodiment 3

[0029] Add 100g of deionized water, 500g of p-toluenesulfonic acid and 100g of ferric hydroxide into a 2000ml flask, heat the reaction temperature at 115-120°C, react for 2h, cool and replenish water and filter. The filtrate was spray-dried to obtain 380 g of solids. Karl Fischer detected moisture <0.2%, particle size <25um, no chloride ions, no nitrate ions, and 3 ppm sulfate ions.

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Abstract

The invention provides a high-purity iron p-toluenesulfonate preparation method, and is characterized in that the preparation method comprises the steps: taking ferric hydroxide as an iron source, carrying out a reaction with p-toluenesulfonic acid, and after the product is filtered, carrying out spray drying to obtain qualified iron p-toluenesulfonate, wherein the molar ratio of ferric hydroxide to p-toluenesulfonic acid is 1:1-3.5. The method can prepare the high-purity iron p-toluenesulfonate having the advantages of low moisture, low contents of various anions, fine particles and high solubility and meeting requirements of electronic products, and is more suitable for industrialized production.

Description

technical field [0001] The invention relates to the field of electronic chemicals, in particular to a high-purity method for electronic-grade iron p-toluenesulfonate. Background technique [0002] Ferric p-toluenesulfonate is widely used in organic conductive materials, and mixed with heterocyclic monomers, such as 3,4-ethylenedioxythiophene, to improve the mixing efficiency by organic solvents such as isopropanol, methanol or acetone, and then carry out Heterocyclic polymerization, this polymer is mainly used for conductive polymer coatings. In addition, iron p-toluenesulfonate is added to organic adhesives and adhesives, such as polyvinyl acetate (PVA) or epoxy silane, to improve its adhesion. [0003] Regarding the preparation of ferric p-toluenesulfonate, Stephen M. Holmes proposed in the literature that ferric trichloride or ferric chloride hydrate and p-toluenesulfonic acid reacted at 160 degrees, and the solid obtained was washed with ether and methanol was refluxed ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/30C07C303/32
Inventor 张雪琴
Owner 张 雪琴
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