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A kind of phenolic resin composition test and quantitative analysis method and application

A technology of phenolic resin and analytical method, which is applied in the field of quantitative measurement, can solve the problems of little difference in molecular volume, the test efficiency needs to be improved, and the separation efficiency of chromatographic columns is difficult, so as to achieve the effect of easy analysis, fast detection speed and intuitive spectrum

Active Publication Date: 2021-09-28
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, although GPC can be used to distinguish free phenol, monomethylol phenol or dimers in the resin, as the degree of polymerization of the components increases, the difference in molecular volume is not large, and the elution time between components overlaps. The separation efficiency of the chromatographic column is difficult to distinguish them. For example, the trimer, tetramer, pentamer and other components in the thermoplastic phenolic resin have a broad peak in the GPC curve, which cannot be distinguished, and it is even more difficult to quantify different polymerization degrees. The relative content of points
In addition, in order to ensure the separation efficiency, the GPC test time is generally about 40 minutes, and the test efficiency needs to be improved
[0006] In summary, the current technical means for testing the composition of phenolic resins, especially GPC, still has obvious deficiencies.

Method used

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  • A kind of phenolic resin composition test and quantitative analysis method and application
  • A kind of phenolic resin composition test and quantitative analysis method and application
  • A kind of phenolic resin composition test and quantitative analysis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Thermoplastic phenolic resin (purchased from Jinan Shengquan Group Co., Ltd., brand PF-8020, softening point is 105-109 ° C) sample FD-MS spectrum determination and component characteristics, relative content of each component and average molecular weight calculate.

[0063] (1) Preparation of test samples

[0064] Take a PF-8020 resin sample and place it in a sample bottle, dry it in an oven at 105°C for 30 minutes to remove the absorbed moisture, and grind it into a fine powder after cooling in the dryer. Take chromatographically pure tetrahydrofuran (THF), measure 10mL, add to the sample dissolving bottle; weigh 200mg of PF-8020 powder sample, dissolve it in the above 10mL THF, sonicate the sample to completely dissolve, and prepare a solution with a concentration of 20mg / mL ,stand-by.

[0065] (2) FD-MS spectrum test

[0066] The German Thermo Fisher DFS high-resolution double-focusing magnetic mass spectrometer was used to test the PF-8020 resin FD-MS spectrum. ...

Embodiment 2

[0076] Determination of FD-MS spectrum of a sample of thermoplastic phenolic resin (purchased from Jinan Shengquan Group Co., Ltd., brand PF-8013, softening point 89-94°C) and its component characteristics, relative content of each component and calculation of average molecular weight .

[0077] (1) Preparation of test samples

[0078] Take the PF-8013 resin sample and place it in a sample bottle, dry it in an oven at 105°C for 30 minutes to remove the absorbed moisture, and grind it into a fine powder after cooling in the dryer. Take chromatographically pure N,N-dimethylformamide (DMF), measure 10mL, and add it to the sample dissolution bottle; weigh 250mg of PF-8013 powder sample, dissolve it in the above 10mL THF, sonicate the sample to completely dissolve, and prepare into a solution with a concentration of 25 mg / mL for use.

[0079] (2) FD-MS spectrum test

[0080] The PF-8013 resin FD-MS spectrum was tested by a German Thermo Fisher DFS high-resolution double-focusing...

Embodiment 3

[0090] Determination of the FD-MS spectrum of the high-purity phenolic resin sample (softening point 80-85°C) made by the Institute of Chemistry, Chinese Academy of Sciences, and the calculation of its component characteristics, relative content of each component and average molecular weight.

[0091] (1) Preparation of homemade thermoplastic high-purity phenolic resin

[0092] Take 94.11 grams of phenol, 64.04 grams of formaldehyde and 1.58 grams of oxalic acid, put them into a 250mL three-necked flask equipped with a mechanical stirrer, a thermometer and a condenser, and stir for 10 minutes to mix the materials evenly; use an oil bath to heat the above reaction materials, and after 30 minutes The temperature was raised to 70°C, and the temperature was kept for 1.5 hours, and the temperature was further raised to 85°C, and the temperature was continued for 2 hours. After the reaction was completed, deionized water was added, washed with water until neutral, and the water laye...

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Abstract

The invention provides a method for testing and quantitatively analyzing the composition of phenolic resin, which adopts the characteristic ion source of soft ionization, suitable scan rate, scan interval, filament heating rate, ionization voltage and other test parameters to ensure the spectrum information obtained by the test. High noise ratio and good stability; the data calculation method proposed by the invention has the characteristics of accurate data, simple algorithm, good reproducibility, stability and reliability, and is suitable for quantitative analysis of composition and molecular weight characteristic analysis of phenolic resin.

Description

technical field [0001] The invention relates to a phenolic resin composition test and quantitative analysis method and application thereof, which can be used for determining the composition characteristics and molecular weight of the phenolic resin, and belongs to the field of quantitative measurement. Background technique [0002] Phenolic resin is a kind of polymer material prepared by the addition and condensation reaction between phenols and aldehydes. Since the German scientist Bayer first synthesized the resin in the laboratory in 1872, it has been developed for nearly 150 years. , which is one of the earliest known and most widely used synthetic polymer materials. Phenolic resin has a series of excellent properties, such as high temperature resistance, high carbon residue, excellent dimensional stability, flame retardancy, low smoke toxicity and so on. Therefore, phenolic resins are widely used in construction (such as thermal insulation materials), transportation (s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/62
CPCG01N27/62
Inventor 赵彤罗振华王娟李昊陈凤华
Owner INST OF CHEM CHINESE ACAD OF SCI
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