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A kind of test method of degree of substitution of condensed silicone resin

A testing method and technology of silicone resin, applied in the field of silicone resin, can solve problems such as unfavorable product quality control, silicone resin structure analysis, inability to fully represent the degree of substitution of silicone resin, etc., and achieve the effect of facilitating product quality control

Active Publication Date: 2022-07-19
中蓝晨光化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to feeding errors and side reactions in the synthesis process, the calculated value cannot fully represent the actual degree of substitution (R / Si ratio) in the silicone resin, which is not conducive to product quality control and structural analysis of silicone resins with unknown components

Method used

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  • A kind of test method of degree of substitution of condensed silicone resin
  • A kind of test method of degree of substitution of condensed silicone resin
  • A kind of test method of degree of substitution of condensed silicone resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] A method for testing the degree of substitution of condensed silicone resin, comprising the following steps:

[0058] S1. After pre-processing the sample to be tested, measure to obtain the mole fraction of the inactive substituent group R, the mole fraction of the active group X, and the ratio R of the amount of the active group X to the inactive substituent group R. X / R ;

[0059] Wherein, the pretreatment and determination of the sample to be tested adopts the prior art;

[0060] S2. After pre-processing the sample to be tested, measure it to obtain the mass fraction w of silicon element in the total mass of the silicone resin Si ;

[0061] Wherein, the pretreatment and determination of the sample to be tested adopts the prior art;

[0062] S3. Bring the parameters obtained in steps S1 and S2 into formula (1) to obtain the degree of substitution P of the condensed silicone resin of the sample to be tested R / Si ;

[0063]

[0064] In formula (1), P R / Si is th...

Embodiment 2

[0086] Based on Example 1, in this example, sample 1 to be tested is taken to test the degree of substitution, so as to further illustrate the technical solution of the present invention.

[0087] Take 1 drop of 0.5 mL of the sample to be tested on a clean and dry glass slide, and let it dry for 24 hours in a ventilated environment of (25±15) °C; The pressure is not higher than 100Pa, and it is dried for 12h. Take (20 ± 2) mg of the sample to be tested after drying and dissolve it in 0.5 mL of deuterated tetrahydrofuran, and send the sample for 1 H NMR test (results such as image 3 shown);

[0088] Taking the sample solution to be tested without adding tetramethylsilane as the internal standard, and using the solvent peak as calibration, the mole fraction of each inactive substituted group R, the mole fraction of active group X, the active group calculated by the spectrum The ratio R of the amount of X to the amount of the non-reactive substituent group R X / R .

[0089] ...

Embodiment 3

[0091] Based on Example 1, in this example, the sample 2 to be tested is taken to test the degree of substitution, so as to further illustrate the technical solution of the present invention.

[0092] Take 40 mg of sample 2 to be tested in a dry NMR tube, and gradually dissolve the sample to be tested in 0.5 mL of deuterated ortho-dichlorobenzene by solvent replacement. 1 H NMR test;

[0093] Taking the sample solution to be tested without adding tetramethylsilane as the internal standard, and using the solvent peak as calibration, the mole fraction of each inactive substituted group R, the mole fraction of active group X, the active group calculated by the spectrum The ratio R of the amount of X to the amount of the non-reactive substituent group R X / R .

[0094] Take 20g of sample 2 to be tested in a dry polytetrafluoroethylene beaker with a diameter of 80mm, in a ventilated environment of (25±15) ℃, let it stand for drying for 24h; set the temperature of the electric blas...

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Abstract

The invention provides a method for testing the degree of substitution of condensed silicone resins, belonging to the technical field of silicone resins. After pretreatment of the sample to be tested, nuclear magnetic resonance method, inductively coupled plasma spectroscopy (ICP) method or titration method are used to determine the mole fraction of each inactive substituent group R, the mole fraction of active group X, The ratio of the amount of the active group X to the non-active substituent group R, the mass fraction of the silicon element in the total mass of the silicone resin, and the degree of substitution (R / Si ratio) of the condensed silicone resin is calculated to provide a theory for the structure of the silicone resin. It is convenient for the quality control of silicone resin products and the structural analysis of silicone resins with unknown components.

Description

technical field [0001] The invention relates to a method for testing the degree of substitution (R / Si ratio) of a condensation type silicone resin, in particular to a method for calculating the degree of substitution (R / Si ratio) of the silicone resin by measuring the molar ratio of substituent groups and the mass fraction of silicon in the silicone resin. The test method belongs to the technical field of silicone resin. Background technique [0002] Silicone resin is a network polymer with Si-O bond as the main chain. Due to the stable Si-O bond, silicone resin has good temperature resistance, weather resistance, electrical insulation and hydrophobicity. It is widely used in heat-resistant insulating coatings, LED packaging materials, ablation-resistant coatings and other fields. [0003] The molecular structure of silicone resin after curing is as follows figure 1 shown, wherein, R is an organic group, such as: methyl, phenyl, etc. [0004] figure 2 It contains four k...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N33/44G01N21/73G01N31/16G01N24/08
CPCG01N33/442G01N21/73G01N31/16G01N24/08
Inventor 李川阳唐小斗李霞孙挚朱良波
Owner 中蓝晨光化工有限公司
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