Thermoplastic phenolic resin intrinsic structure test and quantitative analysis method and application thereof

A phenolic resin and testing method technology, applied in the field of quantitative measurement, can solve the problems of large molecular weight difference, large molecular weight deviation, molecular weight judgment deviation, etc., and achieve the effects of fast detection speed, simple sample preparation and convenient operation.

Active Publication Date: 2021-02-02
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, the principle of size exclusion chromatography leads to a large deviation in the molecular weight judgment of a large number of isomer components in phenolic resins; for example, the diphenol ring component 4,4-dihydroxyl in thermoplastic phenolic resins Both diphenylmethane and 2,4-dihydroxydiphenylmethane have an absolute molecular weight of 200.08, but due to their different molecular volumes, the molecular weight difference obtained by the test is also large, especially in the high molecular weight of phenolic resin. region, this effect will lead to greater deviation of the molecular weight obtained by GPC test
Further, testing the molecular weight of phenolic resin by GPC has high requirements for the stability of the instrument, and the drift of the baseline will often have a greater impact on the test results, and in order to ensure the separation efficiency, the test time is generally about 40 minutes, and the efficiency is still to be determined. improve

Method used

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  • Thermoplastic phenolic resin intrinsic structure test and quantitative analysis method and application thereof
  • Thermoplastic phenolic resin intrinsic structure test and quantitative analysis method and application thereof
  • Thermoplastic phenolic resin intrinsic structure test and quantitative analysis method and application thereof

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preparation example Construction

[0042]The preparation method and application of the present invention will be further described in detail in conjunction with specific embodiments below. It should be understood that the following embodiments are only for illustrating and explaining the present invention, and should not be construed as limiting the protection scope of the present invention. All technologies realized based on the above contents of the present invention are covered within the scope of protection intended by the present invention.

[0043] Unless otherwise stated, the raw materials and reagents used in the following embodiments are commercially available or can be prepared by known methods.

[0044] Embodiments of the present invention provide a kind of test method of thermoplastic phenolic resin average polymerization degree and molecular weight, comprise the steps:

[0045] Step 1, the thermoplastic phenolic resin is dissolved in a deuterated reagent containing tetramethylsilane (TMS) as an in...

Embodiment 1

[0068] Commercialized thermoplastic phenolic aldehyde (purchased from Jinan Shengquan Group Co., Ltd., brand PF-8020, softening point 105-109°C) was determined by NMR spectrum and its average degree of polymerization (n), average molecular weight (MW) and methylene Calculation of the molar ratio (M / P) of the base functional group structure and the phenolic ring structure.

[0069] (1) Preparation of test samples

[0070] 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 DMSO-d with a deuterium substitution rate of 99.90% 6 As the deuterated reagent to be tested, measure 10mL and add it to the sample dissolving bottle; weigh 100mg of PF-8020 powder sample, dissolve it in the above 10mL deuterated solvent, ultrasonically dissolve the sample completely, and prepare a concentration of 10mg / mL Add the solution to the NMR tube. The ...

Embodiment 2

[0083] Pure phenolic resin (softening point 80-85°C) samples from the Institute of Chemistry, Chinese Academy of Sciences were determined by H NMR spectrum and intrinsic structure determination.

[0084] (1) Preparation of high-purity phenolic resin samples

[0085] Take 188.25 grams of phenol, 128 formaldehyde and 3.16 grams of oxalic acid, put them into a 500 mL 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 rise to To 70°C, heat-retaining reaction for 1.5 hours, further raise the temperature to 85°C, and continue heat-retaining reaction for 2 hours. After the reaction was completed, deionized water was added, washed with water until neutral, and the water layer was sucked out. Heat to make the material temperature rise to 60°C, start dehydration under reduced pressure for 3 hours, the material temperature rises to 82±1°C, fin...

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Abstract

According to the thermoplastic phenolic resin intrinsic structure test and quantitative analysis method and the application thereof provided by the invention, during a nuclear magnetic hydrogen spectrum test, test parameters such as relatively high resonance frequency (400MHz), a specific pulse sequence and a proper center frequency are adopted, so that a spectrum obtained by the test is high in signal-to-noise ratio and good in stability; the data calculation method provided by the invention has the characteristics of accurate data, simple algorithm, good reproducibility, stability and reliability, and is suitable for evaluating the stability of the intrinsic structure of the thermoplastic phenolic resin. According to the method, the real molecular weight of the thermoplastic phenolic resin is determined, the problem that when the molecular weight of the phenolic resin is tested through a gel permeation chromatography (GPC) method, deviation is too large due to the fact that the molecular weight is determined according to the molecular volume is solved, and the nuclear magnetic hydrogen spectrum is rapid in testing, high in efficiency and good in stability.

Description

technical field [0001] The invention relates to a method for testing and quantitatively analyzing the intrinsic structure of a thermoplastic phenolic resin and an application thereof, which can be used for evaluating the quality stability of the resin and belongs to the field of quantitative measurement. Background technique [0002] Thermoplastic phenolic resin is a kind of polymer material prepared by polycondensation reaction between phenol and formaldehyde under acid-catalyzed conditions. Thermoplastic phenolic resins with different molecular weights can be prepared by changing the reaction conditions, such as raw material ratio, type and amount of acid catalyst, reaction temperature and time, and solvent system. The intrinsic structural feature of the resin is that the phenolic ring is connected to the methylene group as the repeating unit, and the phenolic ring is the end-capping group. The schematic diagram of its molecular structure is as follows: figure 1 shown. H...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 罗振华赵彤李昊王倩
Owner INST OF CHEM CHINESE ACAD OF SCI
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