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Method for measuring full fluorine sulphonyl resin and sulphonyl monomer content

A technology of fluorosulfonyl resin and sulfonyl monomer is applied in the polymer field, which can solve the problems of many intermediate links, difficulty in meeting requirements, and long test time for chemical testing methods.

Inactive Publication Date: 2007-10-10
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process takes several days, there are many intermediate links, and very skilled operation skills are required to ensure the reliability of the data. It is difficult to measure the sulfonyl monomer content of perfluorosulfonyl resin in a timely and accurate manner.
Long test times of chemical test methods are often difficult to meet when the production process needs to be adjusted according to the calculated sulfonyl monomer value

Method used

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  • Method for measuring full fluorine sulphonyl resin and sulphonyl monomer content
  • Method for measuring full fluorine sulphonyl resin and sulphonyl monomer content
  • Method for measuring full fluorine sulphonyl resin and sulphonyl monomer content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] A perfluorosulfonyl resin produced by Dongyue Group is selected, which is copolymerized from the following two monomers:

[0047] f 2 C=CF 2

[0048]

[0049] Eight batches of perfluorosulfonyl resin samples of this structure were selected, whose sulfonyl monomer content was determined by a standard chemical analysis method.

[0050] Set the value obtained by the chemical analysis method as the real value, and use it as the calibration standard for the quantitative analysis of infrared spectroscopy.

[0051] The single horizontal attenuated total reflection infrared spectrum of a typical perfluorosulfonyl resin is shown in Figure 1: for the convenience of description, it is assumed that the sulfonyl monomer is located at 1430-1490cm -1 The peak in the area is at 1467cm -1 The nearby absorption band is No. 1 band, located at 940-1020cm -1 The peak in the region is 983cm -1 The absorption band is No. 2 band; located at 1030~1280cm -1 The peak in the area is at 1...

Embodiment 2

[0070] Get the infrared spectrogram that test obtains among the embodiment 1. Analyze the absorbance values ​​of bands 1, 2, 3 and 4 using the software that comes with the instrument. The data are summarized in Table 3:

[0071] batch

No

S*

1 / S

Band 1

Absorbance

Band 2

Absorbance

Band 4

Absorbance

R 41 **

R 42 ***

009

0.103

9.698

0.178

0.165

0.717

4.345

4.028

016

0.120

8.305

0.254

0.236

0.909

3.852

3.579

013

0.131

7.651

0.266

0.248

0.865

3.488

3.252

008

0.139

7.178

0.281

0.262

0.886

3.382

3.153

023

0.151

6.641

0.289

0.274

0.889

3.245

3.076

026

0.162

6.155

0.311

0.298

0.9...

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Abstract

A method for measuring sulphonyl monomer content of total fluosulphoylresin resin includes selecting total fluosulphonyl resin samples with different sulphonyl monomer contents, determining ATR-FTIR spectrum corresponding to each sample, selecting absorption spectrum band caused by sulphonyl monomer and carbon-fluorine bond from infrared spectrum as character absorption spectrum hand, setting up operation curve of absorption light intensity of said spectrum hand to sulphonyl monomer content, testing infrared spectrum of unknown sample to know sulphonyl monomer content based on obtained operation curve.

Description

technical field [0001] The invention belongs to the field of macromolecules, and relates to a method for measuring the content of sulfonyl monomers in perfluorosulfonyl resins, in particular to the rapid measurement of sulfonyl in perfluorosulfonyl resins by using attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR). Acyl monomer content method. Background technique [0002] Perfluorosulfonyl resins are generally copolymerized from tetrafluoroethylene monomers and perfluorovinyl ether monomers with sulfonyl fluoride groups, and sometimes other monomers are added for multi-component copolymerization. Perfluorosulfonyl resin can be hydrolyzed to obtain perfluorosulfonic acid resin. Perfluorosulfonic acid resin is a strong solid acid and can be used as ion exchange resin. It has good heat resistance, good electrochemical performance, chemical stability and mechanical strength. Advanced features; it can also be used as a carrier for various chemical re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/35G01J3/42G06F19/00G01N21/3563
Inventor 秦胜高自宏张春玉崔晓梅张永明张恒
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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