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Analysis method of perfluoropolyether relative molecular mass and distribution

A technology of relative molecular weight and perfluoropolyether, which is applied to the analysis of materials, analysis by nuclear magnetic resonance, and measurement devices. It can solve problems such as ambiguity in molecular structure, and achieve strong versatility, simple operation, and good repeatability. Effect

Inactive Publication Date: 2016-12-07
JUHUA GROUP TECH CENT
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Problems solved by technology

When using the end group analysis method to determine the number average molecular weight of perfluoropolyether, it is not only necessary to determine the chemical structure of perfluoropolyether by means of other analytical methods, but also requires the end of the perfluoropolyether molecular chain to have a group that can be used for chemical analysis (such as Carboxyl, ester), for high molecular weight perfluoropolyether with unclear molecular structure, this method has a large analysis error

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  • Analysis method of perfluoropolyether relative molecular mass and distribution
  • Analysis method of perfluoropolyether relative molecular mass and distribution
  • Analysis method of perfluoropolyether relative molecular mass and distribution

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Embodiment

[0031] 1: Identification of perfluoropolyether standard samples

[0032] 1.1 Perfluoropolyether 19 Determination of F-NMR spectrum

[0033] Take a small amount of perfluoropolyether sample prepared by anionic polymerization in a 5mm nuclear magnetic tube, dissolve it with hexafluorobenzene, place it in a nuclear magnetic resonance instrument, and use the pulse program zgflqn to measure the concentration of the sample solution. 19 F-NMR spectrum. The observation frequency is 500MHz, the measured temperature is 298K, the spectral width is 113636.367Hz, the sampling data points are 131072, the delay time is 6.50μs, the receiving gain is 9, the number of empty scans is 4 times, and the number of scans is 256 times.

[0034] 1.2 Perfluoropolyether 19 Identification of F atom signal peak in F-NMR spectrum

[0035] 19 After the phase correction, baseline correction and chemical shift correction of the F-NMR spectrum, according to the chemical shift value of the F atom signal pea...

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Abstract

The invention discloses an analysis method of perfluoropolyether relative molecular mass and distribution. According to the method, perfluoropolyether, which is identified by nuclear magnetic resonance spectrum and is synthesized by an anionic polymerization method, is taken as the standard substance; then perfluoropolyether is dissolved by dichloro-perfluoropropane to obtain a solution with a concentration of 10 to 20 mg / mL; gel permeation chromatograph, a differential refraction detector, and a gel chromatographic column are adopted, the mobile phase is dichloro-perfluoropropane, the flow speed is 0.6 mL / min, the column temperature is 35 DEG C, standard samples are analyzed one by one according to the chromatographic conditions mentioned above, then a standard curve is manufactured, a standard curve equation is determined, the linearly dependent coefficient is measured, and an effective detection method is provided for analyzing the molecular mass of perfluoropolyether prepared by an optical oxidation polymerization method, a photocatalytic polymerization method, or an anionic polymerization method. The provided analysis method has the advantages of strong universality, high accuracy, good repeatability, and simple operation, can be used to establish quality detection standards of perfluoropolyether products for enterprises, and has a very important practical value.

Description

technical field [0001] The invention belongs to the technical field of polymer material analysis, and relates to a method for analyzing the relative molecular mass and distribution of perfluoropolyether by gel permeation chromatography. It can be used to analyze perfluoropolyether with a molecular weight of 1000-8000, and can also be used as an enterprise quality inspection standard for related products. Background technique [0002] Perfluoropolyether (Perfluoropolyether) is a colorless and transparent perfluoropolymer material with only three elements, C, F and O, in the molecule. Compared with the molecular structure of hydrocarbon polyether, perfluoropolyether uses C-F bond instead of C-H bond, and the strong electronegative fluorine atom makes the intermolecular attraction smaller and has smaller surface tension; The shielding effect of the chain makes it have very high anti-oxidation, anti-corrosion, anti-radiation, heat-resistant and non-combustible properties. Perf...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N24/08
CPCG01N30/02G01N24/08G01N30/06
Inventor 谭慧钟军张庆华
Owner JUHUA GROUP TECH CENT
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