Supercharge Your Innovation With Domain-Expert AI Agents!

Method for testing substitution degree of condensed silicon 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, and inability to fully represent the degree of substitution of silicone resin, so as to facilitate quality control, simplify test methods, improve efficiency and accuracy degree of effect

Active Publication Date: 2021-03-26
中蓝晨光化工有限公司 +1
View PDF18 Cites 0 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for testing substitution degree of condensed silicon resin
  • Method for testing substitution degree of condensed silicon resin
  • Method for testing substitution degree of condensed silicon resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0058] S1. After the sample to be tested is pretreated, measure and 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 substance of the active group X to the inactive substituent group R X / R ;

[0059] Among them, the pretreatment and determination of the sample to be tested adopt the existing technology;

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

[0061] Among them, the pretreatment and determination of the sample to be tested adopt the existing technology;

[0062] S3. Bring the parameters obtained through steps S1 and S2 into formula (1) to obtain the degree of substitution P of the condensation type silicone resin of the sample to be tested ...

Embodiment 2

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

[0087] Take one drop of 0.5mL sample to be tested on a clean and dry glass slide, and let it stand and dry for 24h in a ventilated environment at (25±15)°C; then, put it in a vacuum oven, set the temperature at 50°C, The pressure is not higher than 100Pa, and it is dried for 12 hours. Take (20±2)mg dried sample to be tested and dissolve it in 0.5mL deuterated tetrahydrofuran, send the sample for 1 H NMR test (results such as image 3 shown);

[0088] With no addition of tetramethylsilane in the sample solution to be tested as the internal standard, and the solvent peak calibration, the mole fraction of each inactive substituent group R, the mole fraction of the active group X, and the active group The ratio of X to the amount of substance of the non-reactive substituent group R R X / R .

[...

Embodiment 3

[0091] Based on Example 1, the sample 2 to be tested is taken in this example 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 o-dichlorobenzene by solvent replacement, and send the sample for 1 H NMR test;

[0093] With no addition of tetramethylsilane in the sample solution to be tested as the internal standard, and the solvent peak calibration, the mole fraction of each inactive substituent group R, the mole fraction of the active group X, and the active group The ratio of X to the amount of substance of the non-reactive substituent group R R X / R .

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a method for testing the substitution degree of condensed silicon resin, and belongs to the technical field of silicon resin. The method comprises the following steps: pretreating a to-be-detected sample, and then adopting a nuclear magnetic resonance method, an inductively coupled plasma (ICP) method or a titration method; measuring the molar fraction of each non-active substituent group R, the molar fraction of the active group X, the ratio of the amount of substance of the active group X to the amount of substance of the non-active substituent groups R and the mass fraction of the silicon element accounting for the total mass of the silicon resin in the condensed silicon resin, calculating the substitution degree (R / Si ratio) of the condensed silicon resin, and providing a theoretical basis for a silicon resin structure, thereby facilitating the silicon resin product quality control, structural analysis of silicon resin with unknown components and the like.

Description

technical field [0001] The invention relates to a test method for the degree of substitution (R / Si ratio) of condensation-type silicone resin, in particular to a method for calculating the degree of substitution (R / Si ratio) of 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 the cured silicone resin is as follows: figure 1 Shown, wherein, R is an organic group, such as: methyl, phenyl, etc. [0004] figure 2 Among them, it contains four k...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(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
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com