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Aryl sulfonic acid compound purifying method

A technology of aryl sulfonic acid and purification method, which is applied in the field of purification of aryl sulfonic acid compounds, can solve problems such as side reactions and limit the types of aryl sulfonic acid salts, and achieve the effect of reducing purification costs

Active Publication Date: 2015-07-29
TORAY ADVANCED MATERIALS RES LAB CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is prone to side reactions in the process of converting calcium salts into sodium salts for compounds whose substrates are aryl polysulfonic acids
In addition, since the reaction of converting calcium salts with carbonates is carried out in the water phase, the carbonates used must be soluble, which further limits the types of cations of arylsulfonates.

Method used

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  • Aryl sulfonic acid compound purifying method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Take 2.0L of the diluted solution after the sulfonation reaction (4,4'-difluoro-3,3'5,5'-tetrasulfonic acid benzophenone compound has a mass of about 186g and sulfuric acid is about 148g in aqueous solution), Gradually add Ca(OH) under the condition of full stirring 2 Suspension (a mixture of 180.0g calcium hydroxide and 150mL deionized water), control the temperature below 45°C. After the addition was completed, the filtrate was filtered, washed and combined to obtain a pink clear liquid. Under the conditions indicated by the pH meter, add an aqueous solution containing 10.0 g of calcium hydroxide to pH = 6.50, filter with suction, wash, and combine to obtain about 2.5 L of light yellow liquid. Add 90.0 g of oxalic acid dihydrate to the solution, control the temperature at 50° C., react for 3 h, filter with suction, wash and combine. Take a small amount of clear liquid and titrate it with the above-mentioned saturated sodium carbonate solution to confirm that the aci...

Embodiment 2

[0028] Take 2.0L of the diluted solution after the sulfonation reaction (4,4'-difluoro-3,3'5,5'-tetrasulfonic acid benzophenone compound has a mass of about 186g and sulfuric acid is about 148g in aqueous solution), Gradually add CaCO under full stirring 3 Suspension (a mixture of 233.2g calcium carbonate and 250mL deionized water), control the temperature below 45°C. After the addition was completed, the filtrate was filtered, washed and combined to obtain a pink clear liquid. Under the conditions indicated by the pH meter, add an aqueous solution containing 15.0 g of calcium carbonate to pH = 7.50, filter with suction, wash, and combine to obtain about 2.5 L of light yellow liquid. Add 65.0 g of anhydrous oxalic acid to the solution, control the temperature at 50°C, react for 3 hours, filter with suction, wash and combine. Take a small amount of clear liquid and titrate it with the above-mentioned saturated sodium carbonate solution to confirm that the acidification has be...

Embodiment 3

[0030] Take 2.0L of the diluted solution after the sulfonation reaction (4,4'-difluoro-3,3'5,5'-tetrasulfonic acid benzophenone compound has a mass of about 186g and sulfuric acid is about 148g in aqueous solution), Gradually add Ca(OH) under the condition of full stirring 2 Suspension (a mixture of 180.0g calcium hydroxide and 150mL deionized water), control the temperature below 45°C. After the addition was completed, the filtrate was filtered, washed and combined to obtain a pink clear liquid. Under the conditions indicated by the pH meter, add an aqueous solution containing 15.0 g of calcium hydroxide to pH = 9.50, filter with suction, wash, and combine to obtain about 2.5 L of light yellow liquid. Add 90.0 g of oxalic acid dihydrate to the solution, control the temperature at 50° C., react for 3 h, filter with suction, wash and combine. Take a small amount of clear liquid and titrate it with the above-mentioned saturated sodium carbonate solution to confirm that the aci...

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Abstract

The invention relates to an aryl sulfonic acid compound purifying method. An aryl sulfonic acid compound mixture prepared through a sulfuric acid or fuming sulfuric acid sulfonation reaction is neutralized, acidified and re-neutralized to remove inorganic acids and inorganic salts except an aryl sulfonic acid compound in the aryl sulfonic acid compound mixture. The method can effectively control and substantially reduce the residual quantity of the inorganic salts in an aryl sulfonate compound, and improves the purity of a sulfonated monomer. A sulfonated polyetheretherketone polymer with high molecular weight is successfully obtained through polymerization of the highly pure aryl sulfonic acid compound and a diphenolic compound. The polymer with high molecular weight can be widely applied in fuel cell electrolyte membrane researches.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to a method for purifying arylsulfonic acid compounds. Background technique [0002] Arylsulfonic acid compounds have a wide range of applications in the fields of medicine, pesticides, materials and the environment. In the field of environment, proton exchange membrane fuel cells have been paid attention to by many researchers because of their advantages such as high power density, low temperature start-up, and environmental friendliness. At present, the commonly used proton exchange membrane is perfluorosulfonic acid membrane (such as Nafion membrane). Due to its high price, low proton conductivity at high temperature and high methanol permeability coefficient, its further development is limited. Therefore, the study of proton exchange membrane materials with good battery performance, low cost and high temperature operation has become a current hot spot. The currentl...

Claims

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Application Information

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IPC IPC(8): C07C309/44C07C303/44C08G65/40C08J5/22H01M8/10H01M8/02
CPCY02E60/50
Inventor 陈广明范少夫陈桥
Owner TORAY ADVANCED MATERIALS RES LAB CHINA
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