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Method for preparing iron p-toluenesulfonate and solution thereof

A technology of p-toluenesulfonic acid and ferric toluenesulfonate, which is applied in the field of chemical engineering, can solve problems such as incomplete reaction, poor product activity, and large environmental pollution, and achieve moderate reaction speed, less impurity ions, and environmental protection. The effect of less pollution

Active Publication Date: 2013-02-06
广州化学试剂厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ferric nitrate is used as the iron source, and hydrazine hydrate is added to reduce the nitrate to generate nitrogen gas discharge. The reaction is incomplete, and the remaining nitrate will remain as impurities. Hydrazine hydrate is poisonous, and there are potential safety hazards in operation, which will cause certain pollution to the environment. Reaction reflux time is long, efficiency is low, product activity is poor
Therefore, the traditional method has shortcomings such as incomplete reaction, cumbersome operation, low reaction efficiency, high toxicity, large environmental pollution, and poor activity of the prepared ferric p-toluenesulfonate.

Method used

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  • Method for preparing iron p-toluenesulfonate and solution thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Preparation of iron p-toluenesulfonate:

[0051] In a 2000mL beaker, prepare a sodium hydroxide solution with a concentration of about 20% (be careful to let it cool). In another 2000mL beaker, add 400g CP ferric ammonium sulfate, add 1200g deionized water, and stir until it is completely dissolved. The sodium hydroxide solution is slowly added in the ammonium ferric sulfate solution, while constantly stirring, until the pH value is 7.5 (the pH value is measured with a pH meter), and a total of about 93g of CP solid sodium hydroxide is consumed, and a large amount of ferric hydroxide precipitation occurs at this time Move the ferric hydroxide precipitation into a 50L plastic bucket, add 3 times the volume of the precipitation to the deionized water, stir and wash for 2 minutes, let it stand for stratification, and drain the supernatant, and repeat the operation 5 times until the supernatant The electrical conductivity is less than 100us / cm. Put the washed ferric hydrox...

Embodiment 2

[0054] Preparation of iron p-toluenesulfonate:

[0055] In a 2000mL beaker, prepare a sodium hydroxide solution with a concentration of about 15% (be careful to let it cool). In another 2500mL beaker, add 400g of CP ferric ammonium sulfate, add 1600g of deionized water, and stir until it is completely dissolved. The sodium hydroxide solution is slowly added to the ammonium ferric sulfate solution, while stirring continuously, until the pH value is 7.0 (the pH value is measured with a pH meter), and a total of about 92.5 g of CP solid sodium hydroxide is consumed, and a large amount of ferric hydroxide is precipitated at this time appear; move the ferric hydroxide precipitate into a 50L plastic bucket, add 7 times the volume of deionized water of the precipitate, stir and wash for 5 minutes, let it stand for stratification, and drain the supernatant, and repeat the operation 6 times until the above The conductivity of the serum is less than 100us / cm. Put the washed ferric hydr...

Embodiment 3

[0059] Preparation of iron p-toluenesulfonate:

[0060] In a 2000mL beaker, prepare a sodium hydroxide solution with a concentration of about 30% (be careful to let it cool). In another 2000mL beaker, add 400g of CP ferric ammonium sulfate, add 600g of deionized water, and stir until it is completely dissolved. The sodium hydroxide solution is slowly added to the ammonium ferric sulfate solution, while stirring continuously, until the pH value is 9.0 (the pH value is measured with a pH meter), and a total of about 93.3g of CP solid sodium hydroxide is consumed, and a large amount of ferric hydroxide is precipitated at this time appear; move the ferric hydroxide precipitate into a 50L plastic bucket, add 5 times the volume of the precipitated deionized water, stir and wash for 3 minutes, let it stand for stratification, and drain the supernatant, and repeat the operation 10 times until the supernatant The conductivity of the liquid is less than 100us / cm. Put the washed ferric ...

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Abstract

The invention discloses a method for preparing iron p-toluenesulfonate and a solution thereof. The method for preparing the iron p-toluenesulfonate includes the steps that (1) a sodium hydroxide solution and an ammonium ferric sulfate solution are prepared; (2) the sodium hydroxide solution is added in the ammonium ferric sulfate solution, the final potential of hydrogen (pH) value of reaction is 7.0 to 9.0, and iron hydroxide precipitation is obtained; (3) the iron hydroxide precipitation is washed, placed in a filter bag and suspended to be dried at room temperature until the iron hydroxide precipitation which is colloid and contains a small amount of water is formed; (4) iron hydroxide which is suspended to be dried is reacted with a p-toluene sulfonic acid to generate an iron p-toluenesulfonate solution; (5) the iron p-toluenesulfonate solution is filtered and concentrated to be viscous, and discharging-cooling and crystallization are performed; and (6) crystals are crushed and dried to obtain the product. The method for preparing the iron p-toluenesulfonate and the solution thereof has the advantages that the activity of the reaction intermediate iron hydroxide is good, the reaction with the p-toluene sulfonic acid is complete, the process is simple, the energy consumption and the cost are low, and the environmental pollution is small.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and relates to a preparation method and application of ferric p-toluenesulfonate and its solution. Background technique [0002] PEDT conductive polymer made of EDOT (ethylenedioxythiophene) and oxidant (iron p-toluenesulfonate), the main purpose is to produce solid polymer capacitors, the solid electrolyte made of this material is the core of solid polymer capacitors , so that the solid polymer capacitor overcomes performance defects such as low conductivity and liquid leakage, and has high frequency and low impedance, high ripple current resistance, good instantaneous response characteristics, excellent temperature and frequency characteristics, good moisture resistance, small size, and long life. Safe and reliable and suitable for surface mount and other advantages. Polyethylenedioxythiophene (PEDOT) has become one of the most promising conductive polymers because of its high con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/30C07C303/32C08G61/12
Inventor 王保金李帅
Owner 广州化学试剂厂
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