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Phenolic resin curing agent and preparation method thereof

A technology of phenolic resin and curing agent, applied in the field of phenolic resin curing agent and its preparation, can solve the problems of difficult to meet the temperature resistance of copper clad laminate reflow soldering, poor processing performance, poor heat resistance, etc., and achieve dimensional stability. , Low thermal expansion coefficient, low water absorption effect

Inactive Publication Date: 2018-05-08
嘉兴市东方万达新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Another patent publication 101108912 is a nanocomposite material composed of a halogen-free flame-retardant epoxy resin, which is to add a flame retardant and a montmorillonite compound to the epoxy resin to achieve a flame-retardant effect. , Patent CN201010260021.9 discloses a highly flame-retardant epoxy resin curing agent, which can achieve self-flame-retardant properties, but the heat resistance is not good, and it is difficult to meet the temperature resistance of reflow soldering required by copper clad laminates, CN200680045043 The patent discloses a biphenyl type epoxy resin. This type of resin is easy to crystallize, easy to precipitate in a state containing a solvent, has poor processing performance, and has low heat resistance when used as an epoxy resin curing agent.
Relying on the special structure of the high benzene ring of the curing agent itself to achieve flame retardancy and endow the product with high heat resistance and high TG, there are not many reports on the epoxy resin curing agent

Method used

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  • Phenolic resin curing agent and preparation method thereof

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Embodiment 1

[0013] Embodiment 1 of the present invention provides a phenolic resin curing agent and its preparation method, characterized in that: under the protection of nitrogen, in a four-necked flask equipped with a stirrer, a reflux condenser, a thermometer port, a nitrogen port, and an HCL recovery device , put in 456g (2mol) of bisphenol A, 44g of water, 102g (1mol) of propylene glycol carbonate, heat up to 80°C, and carry out the reflux reaction while absorbing and removing the HCL gas released from the reaction through a hydrochloric acid absorption device. After 2 hours, slowly raise the reaction temperature, add 122 g of 2-carbonylbenzaldehyde and continue to raise the temperature. When the reaction temperature reaches 130° C., keep the reaction time for 2.5 hours. Then add about 800 grams of pure water for extraction and washing, and repeat this for many times until the pH of the water after washing is directly close to 6-7. Evaporate unreacted phenol, HCL, and a small amount ...

Embodiment 2

[0015] Embodiment 2 of the present invention provides a method for preparing phenolic resin curing agent suction, which is characterized in that: under nitrogen protection, in a four-necked flask equipped with a stirrer, a reflux condenser, a thermometer port, a nitrogen port, and an HCL recovery device , load 385g (3.5mol) of catechol, 89g of water, 204g (2mol) of propylene glycol carbonate, heat up to 80°C, and carry out the reflux reaction, while the methanol gas released from the reaction is condensed and absorbed by the condenser for removal. After 2 hours, add 292 g of 2-carbonylbenzaldehyde and continue to raise the temperature. When the reaction temperature reaches 130° C., slowly increase the reaction temperature. When the reaction temperature reaches 130° C., keep the reaction time for 2.5 hours. Then add about 1000 grams of pure water for washing, and repeat this for many times until the pH of the water after washing is directly close to 6-7. Remove unreacted small ...

Embodiment 3

[0017] Embodiment 3 of the present invention provides a phenolic resin curing agent and a preparation method thereof, which is characterized in that: under nitrogen protection, in a four-necked flask equipped with a stirrer, a reflux condenser, a thermometer port, a nitrogen port, and an HCL recovery device 141g (1.5mol) of phenol, 107g of water, and 208g (2mol) of ethyl methyl carbonate were charged, and the temperature was raised to 80°C. While performing the reflux reaction, the HCL gas released from the reaction was absorbed and removed through the hydrochloric acid absorption device. After about 2 hours of reaction, add 292 g of 2-carbonylbenzaldehyde and continue to raise the temperature. When the reaction temperature reaches 130° C., slowly increase the reaction temperature. When the reaction temperature reaches 130° C., keep the reaction time for 2.5 hours. Then add about 1200 grams of pure water for washing, and repeat this for many times until the pH of the water afte...

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Abstract

The invention relates to a phenolic resin curing agent and a preparation method thereof. The molecular structure of the phenolic resin is as shown in the abstract drawing, wherein n and m are 1-8. Thepreparation method is that carbonates and organic polyphenols are subjected to a condensation polymerization reaction under the presence of a solid organic acid, and then the resulted product reactswith 2-carbonyl benzaldehyde, so as to generate phenolic resin, namely the phenolic resin curing agent. According to the phenolic resin curing agent and the preparation method thereof, no halogen is contained, and addition of other organic phosphorus flame retardants is not needed, so that plastic sealing materials and copper clad laminates prepared from the phenolic resin curing agent have the features of intrinsic flame retardance, high heat resistance, high reliability, low water absorption, and low coefficient of thermal expansion.

Description

technical field [0001] The invention relates to a phenolic resin curing agent and a preparation method thereof. Background technique [0002] In recent years, with the increasing calls for environmental protection, people are looking for environmentally friendly alternative flame retardant products. The flame retardant properties of flame retardant plastic sealing compounds and copper clad laminates are mainly achieved by using additive flame retardants or flame retardant curing agents. Common additive flame retardants containing phosphorus and nitrogen such as phosphate esters and polyphosphoric acid Amine, melamine cyanurate, aluminum hydroxide, magnesium hydroxide, etc., or phenolic resin containing phosphorus and nitrogen, due to the large amount of addition, the glass transition temperature (Tg), heat resistance, processability and other properties of the plate will be reduced. ; The use of added phosphorus-containing flame retardants will also increase the water absor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/32C08G59/62
CPCC08G8/32C08G59/62
Inventor 戚永玮
Owner 嘉兴市东方万达新材料股份有限公司
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