A method for determining the end point of cyanate resin prepolymerization

A technology of cyanate ester resin and reaction end point, applied in flow characteristics, measuring devices, instruments, etc., can solve problems such as untestable, unsuitable, difficult to uniform films, etc., to achieve industrial production monitoring, high precision, process Simple and Controllable Effects

Active Publication Date: 2017-02-22
AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the period close to the end of prepolymerization, when the melt drops to about 25°C, the viscosity is very high, it is difficult to flow on the observation glass of the refractive index meter to form a uniform film, and normal testing cannot be performed.
Therefore, this method cannot be applied because the viscosity of the prepolymer is large when the prepolymerization is close to the end point.

Method used

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  • A method for determining the end point of cyanate resin prepolymerization
  • A method for determining the end point of cyanate resin prepolymerization
  • A method for determining the end point of cyanate resin prepolymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 0.2g of bisphenol A cyanate resin monomer to the center of the lower plate in the high-temperature plate rotational rheometer, raise the temperature to 100°C, the monomer material melts, and lower the upper plate of the rheometer to touch the molten single Object, under the conditions of torsion frequency (1Hz) and torsion force (1mN·m), the temperature of the plate is raised to the temperature of the polymerization reaction (180°C), and the timing is started. The storage modulus G' of the melt is measured by a rheometer, wherein the storage modulus G' is determined by 10 -4 When Pa rises to 100Pa, it can be judged that the prepolymerization reaction has reached a suitable level, and the time to reach this point is recorded as 195 minutes.

[0037] The parameters of cyanate resin prepolymerization reaction temperature (180°C) and time (195min) determined according to this example can be applied to the preparation of cyanate resin prepolymers, which can be transparen...

Embodiment 2

[0039] Take out 0.2 g of bisphenol A cyanate resin prepolymer that has been prepolymerized for a certain period of time from the reactor, add it to the center of the lower plate in the high-temperature plate rotary rheometer, and raise the temperature to 190 ° C. When the material melts, lower the upper plate of the rheometer to touch the molten material to a specified area, measure the storage modulus G' under the conditions of torsion frequency (0.5Hz) and torsion force (3mN·m), and start timing. The storage modulus G' of the melt is measured by a rheometer, and the storage modulus G' is determined by 10 -3 When Pa rises to 10Pa, it can be judged that the polymerization reaction has reached a suitable level, and the time to reach this point is recorded as 14 minutes.

[0040] The temperature (190°C) and time (14min) parameters of the cyanate ester resin prepolymerization determined according to this example are applied to the preparation of the prepolymerization resin, which c...

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Abstract

The invention provides a method for determining the end point of prepolymerization reaction of cyanate ester resin. The method provided by the invention has the beneficial effects that the change of the energy-storage modulus of melt and the corresponding rule of the polymerization-reaction degree to represent and control the degree of the polymerization reaction, the process is simple, controllable and high in accuracy; the determination can be carried out at relatively high temperature, the change of the melt can be completely represented in the whole process from the state with the very-low viscosity and the extremely-easy flowing to be out of the prepolymerization end point, and the reflected characteristics of the change of the polymerization reaction is relatively close to that in the real state.

Description

technical field [0001] The invention relates to a method for determining the end point of cyanate resin prepolymerization, belonging to the technical field of resin synthesis. Background technique [0002] Cyanate resin is a thermosetting resin with two or more cyanate functional groups (-OCN) in its molecular structure developed in the 1960s. Its molecular structure is: NCO-R-OCN; formed after curing reaction The triazine ring with a symmetrical structure makes the cyanate resin have excellent high-temperature mechanical properties, low molding shrinkage, good dimensional stability, and the dielectric properties show unique stability to changes in temperature and electromagnetic wave frequency. [0003] The most common type of cyanate resin is bisphenol A type cyanate resin, such as figure 1 shown. The synthesis process is simple, the raw materials are cheap, and it can be made into fiber-reinforced prepregs to prepare composite parts. The bisphenol A cyanate resin monom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N11/14
Inventor 李洪深唐培毅杨洁颖郭世峰裴雨辰
Owner AEROSPACE INST OF ADVANCED MATERIALS & PROCESSING TECH
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