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High-purity iron p-toluenesulfonate solution synthesis method

A technology of iron toluene sulfonate and p-toluene sulfonic acid is applied in the field of synthesis of high-purity ferric p-toluene sulfonate solution, and can solve the problem that the leakage current of solid electrolytic capacitors has great influence, equipment corrosion and environmental pollution. Large impact, shortened high temperature service life and other problems, to achieve the effect of less impurity ions, low cost and moderate reaction speed

Inactive Publication Date: 2015-11-04
武汉海斯普林科技发展有限公司
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Problems solved by technology

Chinese patent (application number: CN200610156892.X) introduces the synthesis method of ferric alkylbenzene sulfonate with iron trichloride as raw material, because chloride ions can strongly corrode the electrolytic aluminum oxide film, it has a great influence on the leakage current of solid electrolytic capacitors Large, the production method is very cumbersome to remove a large amount of chloride ions
In particular, expensive silver nitrate is needed to remove trace chloride ions, which is not only expensive, but also leaves nitrate residues
The residual nitrate is easy to migrate in the polymerized PEDOT conductive material, which has a great influence on the corrosion of the dielectric film of the solid capacitor, which will greatly increase the leakage current and shorten the service life at high temperature
At the same time, the hydrogen chloride azeotroped with ethanol is easy to volatilize, and the post-treatment is difficult, which has a great impact on equipment corrosion and environmental pollution.

Method used

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preparation example Construction

[0029] The synthetic method of the high-purity ferric p-toluenesulfonate solution provided by the present invention comprises the following steps:

[0030] 1. The configuration concentration is 5%~15% ferric sulfate solution, and the sodium hydroxide solution is 10%~20%.

[0031] Ferric sulfate and sodium hydroxide solution are used for the reaction, because the ferric hydroxide generated by ferric sulfate has good activity, and the reaction with p-toluenesulfonic acid is complete, fast and thorough.

[0032] The preparation process of the 5%-15% ferric sulfate solution is as follows: ferrous sulfate, sulfuric acid and hydrogen peroxide are prepared by redox reaction;

[0033] The method provided by the present invention is carried out through the following steps:

[0034] 2FeSO 4 +H 2 SO 4 +H 2 O 2 →Fe 2 (SO 4 ) 3 +2H 2 O

[0035] Fe 2 (SO 4 ) 3 +6NaOH→2Fe(OH) 3 +3Na 2 SO 4

[0036] Fe(OH) 3 +3TsOH·H 2 O→Fe(TSOH) 3 +6H 2 O

[0037] 2. The sodium hydroxi...

Embodiment 1

[0043] Synthesis of high-purity ferric p-toluenesulfonate solution:

[0044] In a 5000mL beaker, add 2000g of high-purity water, then add ferrous sulfate, concentrated sulfuric acid and hydrogen peroxide to prepare a ferric sulfate solution with a concentration of about 5%; in another 1000mL beaker, prepare a sodium hydroxide solution with a concentration of about 10% . The sodium hydroxide solution was slowly added to the ferric sulfate solution, while stirring continuously, until the pH value was 7.5 (the pH value was measured with a pH meter), and a large amount of ferric hydroxide floccules were formed at this time.

[0045] Add high-purity water to the 5000mL beaker to the 5000mL mark of the beaker, stir and wash the ferric hydroxide for 2 minutes, stand for stratification, the upper layer is aqueous liquid, and the lower layer is ferric hydroxide precipitation, and the upper aqueous liquid is excluded. Repeatedly adding deionized water for 6 times, until the pH of the s...

Embodiment 2

[0049] Synthesis of high-purity iron p-toluenesulfonate solution:

[0050] In a 5000mL beaker, add 2000g of high-purity water, then add ferrous sulfate, concentrated sulfuric acid and hydrogen peroxide to prepare a ferric sulfate solution with a concentration of about 10%; in another 1000mL beaker, prepare a sodium hydroxide solution with a concentration of about 20% . The sodium hydroxide solution was slowly added to the ferric sulfate solution, while stirring continuously, until the pH value was 8.5 (the pH value was measured with a pH meter), and a large amount of ferric hydroxide floccules were formed at this time.

[0051] Add high-purity water to the 5000mL beaker to the 5000mL mark of the beaker, stir and wash the ferric hydroxide for 2 minutes, stand for stratification, the upper layer is aqueous liquid, and the lower layer is ferric hydroxide precipitation, and the upper aqueous liquid is excluded. Repeatedly adding deionized water to wash for 8 times until the pH of...

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Abstract

The present invention belongs to the technical field of electronic chemical production, and particularly relates to a high-purity iron p-toluenesulfonate solution synthesis method, which comprises: 1) preparing a ferric sulfate solution and a sodium hydroxide solution; 2) preparing ferric hydroxide floc; 3) preparing ferric hydroxide filter cake having sulfate ions achieving the standard; 4) preparing a p-toluenesulfonic acid solution having qualified sulfate ions; and 5) preparing the high-purity iron p-toluenesulfonate solution. According to the present invention, the prepared reaction intermediate ferric hydroxide has good activity and completely reacts with p-toluenesulfonic acid, the product has high purity, and the impurity ions are less.

Description

technical field [0001] The invention belongs to the technical field of production of electronic chemicals, in particular to a method for synthesizing a high-purity ferric p-toluenesulfonate solution. Background technique [0002] Ferric p-toluenesulfonate is an orange-yellow solid, easily soluble in water and alcohol, and is a necessary polymerization oxidant for the preparation of high-conductivity organic conductive materials. Since the invention of 3,4-ethylenedioxythiophene (EDOT) conductive compound by Bayer in Germany in 1990, EDOT (3,4-ethylenedioxythiophene) and oxidant (iron p-toluenesulfonate) Polyethylenedioxythiophene (PEDOT for short) polymer has been widely used. Mainly used in the manufacture of solid electrolytic capacitors. The solid electrolyte made of this material is the core of the solid polymer capacitor, which makes the solid polymer capacitor overcome the performance defects such as low conductivity and liquid leakage. Excellent frequency character...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/30C07C303/32
Inventor 陈丹周宜海杨光黄迅王文潘君郭春花周阳
Owner 武汉海斯普林科技发展有限公司
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