Method for measuring content of cyanate ester monomers

A technology of monomer content and determination method, which is applied in measurement devices, instruments, scientific instruments, etc., to achieve the effects of high precision, avoidance of interference, and easy operation.

Inactive Publication Date: 2018-03-30
GUANGDONG SHENGYI SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the cyanate ester prepolymer cannot be separated and determined by conventional high performance liquid chromatography

Method used

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  • Method for measuring content of cyanate ester monomers
  • Method for measuring content of cyanate ester monomers

Examples

Experimental program
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Embodiment 1

[0027] Embodiment 1 (taking the content measurement of cyanate ester monomer in the bisphenol A type cyanate ester prepolymer as an example)

[0028] 1. Desolventization of bisphenol A cyanate prepolymer

[0029] Spread the bisphenol A cyanate prepolymer thinly on a clean tinfoil paper, and then place it in a vacuum drying oven for drying. The drying temperature can be 20-40°C, and the drying time can be 30-120 minutes. In this embodiment, the drying temperature is set at 30° C., and the drying time is 90 minutes.

[0030] 2. Solvent handling

[0031] The solvent is ultrasonically treated, the temperature of the treatment can be 10-30°C, and the time can be 10-20 minutes. The solvent can be selected from one of toluene and tetrahydrofuran. In this embodiment, the ultrasonic treatment temperature is set at 25°C. The time was 15 minutes and the solvent was tetrahydrofuran (chromatographically pure grade).

[0032] 3. Make the standard curve of cyanate monomer standard solutio...

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Abstract

The application provides a method for measuring the content of cyanate ester monomers. The method comprises the following steps: (1) making standard curves of the concentration X and the peak area Y of a cyanate ester monomer standard liquid: preparing a cyanate ester monomer standard liquid, and obtaining a linear equation of the concentration and the peak area of the cyanate ester monomer standard liquid according to gel permeation chromatographic analysis; (2) preparing a cyanate ester polymer liquid: performing desolvation treatment on a cyanate ester polymer, and then preparing the cyanate ester polymer subjected to desolvation treatment into the cyanate ester polymer liquid which has the same solvent as the cyanate ester monomer standard liquid; and (3) acquiring the content of the cyanate ester monomers: performing gel permeation chromatographic analysis on the cyanate ester polymer liquid to obtain the peak area Y, and acquiring the content of the cyanate ester monomers throughthe standard curves in (1). As desolvation treatment is performed on the cyanate ester polymer, and the monomer liquid and the polymer liquid adopt the same solvent, the measurement result cannot beinterfered by bubbles produced by mixing of different solvents, and accordingly, the measurement result is high in precision and accurate and stable in data.

Description

technical field [0001] The present application relates to the determination of monomer content, in particular to the determination method of cyanate monomer content. Background technique [0002] Cyanate Ester Resin is a kind of thermosetting resin with -OCN functional group at the end group, which has low dielectric constant, low dielectric loss, low moisture absorption, low volume shrinkage, excellent heat resistance and good resistance Flammability and other characteristics, has been widely used in electronic packaging, printed circuit boards, satellite equipment and aerospace and other fields. [0003] Cyanate ester monomer is a powdery crystal at room temperature, with a symmetrical structure and easy to precipitate out when mixed with other resins. In order to improve the manufacturability of crystalline cyanate resin, the cyanate resin is prepared into a prepolymer with a polymerization degree of 30%-50%, and solvents such as acetone, methyl ethyl ketone or toluene a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/86G01N30/14
CPCG01N30/02G01N30/14G01N30/8634
Inventor 盘文辉王小兵张艳华
Owner GUANGDONG SHENGYI SCI TECH
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