Method for measuring content of phenolic hydroxyl groups in polyphenyl ether by titrimetry

A polyphenylene ether and phenolic hydroxyl technology, which is applied in the detection field of titration to determine the content of phenolic hydroxyl in polyphenylene ether, can solve the problems of difficult titration and cumbersome operation of the titration process, and achieve simple operation, simple experimental equipment, and measurement high precision effect

Inactive Publication Date: 2010-11-03
CHINA NAT BLUESTAR GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Since polyphenylene ether is insoluble in water and alcohols, it is difficult to tit

Method used

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  • Method for measuring content of phenolic hydroxyl groups in polyphenyl ether by titrimetry
  • Method for measuring content of phenolic hydroxyl groups in polyphenyl ether by titrimetry
  • Method for measuring content of phenolic hydroxyl groups in polyphenyl ether by titrimetry

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0041] Example 1

[0042] For a polyphenylene ether sample with a number average molecular weight of about 12,400, the steps for measuring its phenolic hydroxyl content by titration are as follows:

[0043] 1) Use an electronic analytical balance to accurately weigh out 5.000 g of a polyphenylene ether sample into a 250 mL Erlenmeyer flask, add 50 mL of chloroform, and stir to dissolve.

[0044] 2) Add 0.05 g of 4-methoxybenzoyl chloride, heat to reflux for 30 min (temperature 55°C), and then cool to room temperature.

[0045] 3) Add 10ml of deionized water to the Erlenmeyer flask, stir for 10min, add 10ml of deionized water from the top of the condenser to rinse the inner wall of the condenser, and then remove the condenser.

[0046] 4) Add 4 drops of phenolphthalein indicator solution to the Erlenmeyer flask and titrate with a standard KOH aqueous solution under stirring until the system is pink and does not fade for 30 seconds.

[0047] 5) Repeat the previous four steps twice.

[0048]...

Example Embodiment

[0050] Example 2

[0051] For a polyphenylene ether sample with a number average molecular weight of about 5200, the steps to measure its phenolic hydroxyl content by titration are as follows:

[0052] 1) Use an electronic analytical balance to accurately weigh out 5.000 g of a polyphenylene ether sample into a 250 mL Erlenmeyer flask, add 50 mL of chloroform, and stir to dissolve.

[0053] 2) Add 0.05 g of 4-methoxybenzoyl chloride, heat to reflux for 30 min (temperature 50° C.), and then cool to room temperature.

[0054] 3) Add 10ml of deionized water to the Erlenmeyer flask, stir for 10min, add 10ml of deionized water from the top of the condenser to rinse the inner wall of the condenser, and then remove the condenser.

[0055] 4) Add 4 drops of phenolphthalein indicator solution to the Erlenmeyer flask and titrate with a standard KOH aqueous solution under stirring until the system is pink and does not fade for 30 seconds.

[0056] 5) Repeat the previous four steps twice.

[0057] 6)...

Example Embodiment

[0059] Example 3

[0060] For a polyphenylene ether sample with a number average molecular weight of about 1200, the steps to measure its phenolic hydroxyl content by titration are as follows:

[0061] 1) Use an electronic analytical balance to accurately weigh out 5.000 g of a polyphenylene ether sample into a 250 mL Erlenmeyer flask, add 50 mL of chloroform, and stir to dissolve.

[0062] 2) Add 0.05 g of 4-methoxybenzoyl chloride, heat to reflux for 30 min (temperature 60°C), and then cool to room temperature.

[0063] 3) Add 10ml of deionized water to the Erlenmeyer flask, stir for 10min, add 10ml of deionized water from the top of the condenser to rinse the inner wall of the condenser, and then remove the condenser.

[0064] 4) Add 4 drops of phenolphthalein indicator solution to the Erlenmeyer flask and titrate with a standard KOH aqueous solution under stirring until the system is pink and does not fade for 30 seconds.

[0065] 5) Repeat the previous four steps twice.

[0066] 6) P...

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Abstract

The invention provides a method for measuring content of phenolic hydroxyl groups in polyphenyl ether by titrimetry. The method comprises the following steps: dissolving polyphenyl ether to be measured in an organic solvent, adding a reagent, and heating at 0-60 DEG C for 10-30 minutes; and cooling to room temperature, adding de-ionized water, dropwisely adding several drops of phenolphthalein indicator solution, titrating by using a standard potassium hydroxide water solution until pink stays fadeless for 30 seconds, and calculating the content of phenolic hydroxyl groups in polyphenyl ether according to the blank experiment. The method has the advantages of simple experimental apparatus and high measuring accuracy.

Description

technical field [0001] The invention relates to a detection method, in particular to a detection method for determining the content of phenolic hydroxyl groups in polyphenylene ether by titration. Background technique [0002] The content of phenolic hydroxyl group in polyphenylene ether is one of the important indicators to characterize its performance. The content of phenolic hydroxyl group varies with the molecular weight and chemical composition of polyphenylene ether. [0003] Since polyphenylene ether is insoluble in water and alcohols, it is difficult to titrate directly by conventional acid-base titration, and the titration process is cumbersome. [0004] It is necessary to study a method that can accurately measure the content of phenolic hydroxyl groups in polyphenylene ether. Contents of the invention [0005] The purpose of the present invention is to provide a titration method for determining the content of phenolic hydroxyl groups in polyphenylene ether, whi...

Claims

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Application Information

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IPC IPC(8): G01N21/79
Inventor 张洪波刘宇辉王海军高岱巍李瑞亢胡衍平
Owner CHINA NAT BLUESTAR GRP CO LTD
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