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A kind of phenolic resin fingerprint structure test method and quantitative analysis method

A technology of fingerprint structure and quantitative analysis, applied in the direction of nuclear magnetic resonance analysis, etc., can solve the problems of large error and inaccurate calculation of hydroxymethyl index, and achieve the effect of reliable data, convenient quantitative calculation, and simple sample preparation method

Active Publication Date: 2021-02-09
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the above-mentioned defects of the prior art, provide a kind of phenolic resin fingerprint structure testing method and quantitative analysis method, obtain spectral peak resolution height and spectral peak separation independent proton nuclear magnetic spectrum data, have avoided due to signal peak cannot Problems such as the inaccurate calculation of the methylol index and large errors caused by the separation have realized the high-resolution identification of the abnormal structural state of the phenolic resin, and the precise quantitative analysis of the fingerprint structure of the phenolic resin

Method used

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  • A kind of phenolic resin fingerprint structure test method and quantitative analysis method
  • A kind of phenolic resin fingerprint structure test method and quantitative analysis method
  • A kind of phenolic resin fingerprint structure test method and quantitative analysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Adopt solvent-free barium phenolic resin as detection sample, add a certain amount of barium phenolic resin in the sample tube, add deuterium reagent, obtain concentration and be 20mg / mL proton NMR sample, wherein said deuterium reagent is containing The deuterated rate of tetramethylsilane is 99.9% deuterated dimethyl sulfoxide, and the volume fraction of tetramethylsilane is 0.03%; cover the test tube cover, shake to dissolve the sample completely, and ensure that there are no suspended particles in the solution. Put the test tube containing the sample on the rotor with the outer wall wiped clean, and adjust the position of the NMR tube with a gauge to ensure that the solution in the dotted line frame of the gauge is evenly clarified.

[0069] Carry out nuclear magnetic spectrum test to described proton nuclear magnetic spectrum sample, obtain as follows figure 1 The H NMR spectrum is shown. During the test, the resonant frequency is ≥500MHz, the cumulative number is...

Embodiment 2

[0077] Adopt solvent-free barium phenolic resin as detection sample, add a certain amount of barium phenolic resin in the sample tube, add deuterium reagent, obtain concentration and be the 15mg / mL proton NMR sample, wherein said deuterium reagent is containing The deuterated rate of tetramethylsilane is 99.9% deuterated dimethyl sulfoxide, and the volume fraction of tetramethylsilane is 0.03%; cover the test tube cover, shake to dissolve the sample completely, and ensure that there are no suspended particles in the solution. Put the test tube containing the sample on the rotor with the outer wall wiped clean, and adjust the position of the NMR tube with a gauge to ensure that the solution in the dotted line frame of the gauge is evenly clarified.

[0078] The proton nuclear magnetic spectrum test is carried out on the proton nuclear magnetic spectrum sample to obtain the proton nuclear magnetic spectrum. During the test: the resonance frequency is ≥ 500MHz, the number of accum...

Embodiment 3

[0087] Adopt solvent-free barium phenolic resin as detection sample, add a certain amount of barium phenolic resin in the sample tube, add deuterium reagent, obtain concentration and be the NMR sample of 25mg / mL, wherein said deuterium reagent is containing The deuterated rate of tetramethylsilane is 99.9% deuterated dimethyl sulfoxide, and the volume fraction of tetramethylsilane is 0.03%; cover the test tube cover, shake to dissolve the sample completely, and ensure that there are no suspended particles in the solution. Put the test tube containing the sample on the rotor with the outer wall wiped clean, and adjust the position of the NMR tube with a gauge to ensure that the solution in the dotted line frame of the gauge is evenly clarified.

[0088] The proton nuclear magnetic spectrum test is carried out on the proton nuclear magnetic spectrum sample, and the hydrogen nuclear magnetic spectrum diagram is obtained. During the test, the resonant frequency is ≥500MHz, the cum...

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Abstract

The invention relates to a test method and a quantitative analysis method for phenolic resin dactylotype, which belong to the field of quantitative test. The test method comprises the steps of mixingphenolic resin with a deuterium substituted reagent to obtain an NMR hydrogen spectrum sample; performing an NMR hydrogen spectrum test on the NMR hydrogen spectrum sample to obtain NMR hydrogen spectrum data, wherein the resonance frequency is greater than or equal to 500 MHz, the spectrum width is 14-18 ppm, the center frequency is 6-8 ppm, the relaxation time is 3-7 s, and the acquisition timeis 2.5-3.5 s. According to the invention, the NMR hydrogen spectrum data with a high spectral peak resolution and an independent spectral peak separation is obtained, avoiding the problems such as theinability to accurately calculate a hydroxymethyl index and large error due to separation failure of a signal peak, and realizing a high-resolution identification of an abnormal structure state of phenolic resin and an accurate quantitative analysis of a phenolic resin dactylotype.

Description

technical field [0001] The invention relates to a method for quantitative testing and analysis of phenolic resin fingerprint structure and a sample preparation method thereof, belonging to the field of quantitative testing. Background technique [0002] Thermosetting phenolic resin is a kind of low molecular weight mixture formed by the addition and polycondensation reaction of phenol (or mixed phenol) and formaldehyde under alkaline conditions, that is, stage I resin. The qualitative and quantitative description of the chemical structure of this low molecular weight mixture is extremely difficult. of. So far, most of the structural formulas of phenolic first-order resins are possible schematic diagrams, and it is impossible to accurately describe their chemical structures with high resolution. As we all know, the thermal properties, thermal cracking products, mechanical properties, ablation properties of composite materials, and process properties of cured phenolic resin a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 胡宏林张晨余瑞莲纪高宁
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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