Active ester curing agent and epoxy resin composition

A technology of active ester curing agent and epoxy resin, which is applied in the field of copper clad laminates, can solve the problems of insufficient research on curing agents, and achieve the effects of low hygroscopicity, high reactivity, and low dielectric loss tangent

Inactive Publication Date: 2018-04-17
SHAANXI SHENGYI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the prior art, the research on the curing agent containing dicycl

Method used

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  • Active ester curing agent and epoxy resin composition
  • Active ester curing agent and epoxy resin composition
  • Active ester curing agent and epoxy resin composition

Examples

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preparation example Construction

[0032] A kind of preparation method of above-mentioned active ester curing agent is also provided in the embodiment of the present invention, it comprises:

[0033] S1. Carrying out addition reaction of phenol and dicyclopentadiene to obtain dicyclopentadiene phenol resin;

[0034] Wherein, the structural formula of the dicyclopentadiene phenol resin is

[0035]

[0036] In the formula, n includes any integer of 1-4.

[0037] Both phenol and dicyclopentadiene are commonly used industrial raw materials. They have a wide range of sources, are cheap and easy to obtain, and can effectively reduce the production cost of the active ester curing agent, which is beneficial to its large-scale industrial production.

[0038] Further, the above addition reaction is carried out under the action of an acid catalyst. The acid catalyst can stabilize the carbocation intermediate formed by dicyclopentadiene, and the carbocation intermediate acts as an electrophile to attack the benzene ri...

Embodiment 1

[0063] The present embodiment provides a kind of dicyclopentadiene phenol resin, and its preparation method is as follows:

[0064] Add 200 g of phenol and 31 mL of toluene into a four-necked flask equipped with a thermometer, dropping funnel, condenser, and stirrer. Remove toluene and water in the system by azeotropic distillation, then add 0.7mL of BF 3 ·Et 2 O and 1.5mL CCl 4 The mixed solution is heated up to 100°C, and 40g of dicyclopentadiene is slowly added dropwise within 4 to 5 hours, and then kept at a constant temperature for 1 hour. After the reaction is completed, excess phenol is removed by distillation under reduced pressure to obtain the required dicyclopentadiene Phenol resin (light yellow solid, hydroxyl equivalent 170-180mg / g).

Embodiment 2

[0066] The present embodiment provides a kind of active ester solidifying agent, and its preparation method is as follows:

[0067] Add 280g of benzoyl chloride and 1258g of benzene in a four-necked flask equipped with a thermometer, dropping funnel, condenser, and stirrer, and feed nitrogen to dissolve it. Then add the dicyclopentadiene phenol resin that 350g embodiment 1 provides, fully dissolve. The temperature was controlled at 60° C., and 300 g of 20 wt % sodium hydroxide aqueous solution was slowly added dropwise within 3 hours. Then keep the temperature at 60°C and continue to stir for 1h. After the reaction was completed, the aqueous layer was removed by static separation and liquid separation. Then, water was added to the toluene solution of the reactants, stirred and mixed for 15 min, and the water layer was separated and separated. This operation was repeated until the pH of the aqueous layer became 7. Then dehydrate by decanter, obtain the active ester solidify...

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Abstract

The invention provides an active ester curing agent and relates to the field of copper-cladding plates. The active ester curing agent has a dicyclopentadiene-phenyl ester alternate structure. On one hand, a dicyclopentadiene structure of the active ester curing agent is capable of well preserving excellent properties such as low hygroscopicity, dielectric constant and dielectric loss angle tangentcaused after the reaction between the curing agent and epoxy resin. On the other hand, the content of an active ester structure in the structure is relatively high, so that the curing agent has veryhigh reaction activity in the reaction with the epoxy resin. The preparation method of the active ester curing agent is easy in operation, the raw materials are easily available, and the large-scale industrial production can be realized. The invention further provides an epoxy resin composition. By virtue of reasonable matching of the active ester curing agent, the epoxy resin and an imidazole compound in a specific proportion, the epoxy resin composition is high in curing activity and has a good curing effect, and a cured condensate has excellent dielectricity and water absorption property and can be used for preparing prepregs, laminated boards and copper-cladding plates.

Description

technical field [0001] The invention relates to the field of copper clad laminates, in particular to an active ester curing agent and an epoxy resin composition. Background technique [0002] In recent years, with the development of high-performance, multi-functional, and networked information and communication systems, the high-speed transmission of signals and the processing of large-capacity information make the operating signals tend to be high-frequency, requiring substrate materials to have lower dielectric constants. Tangent to the dielectric loss angle. Therefore, good dielectric properties have become one of the development trends of epoxy resin compositions. Epoxy resin compositions based on epoxy resins and amine curing agents are widely used in the field of printed circuit boards due to their excellent heat resistance and insulation properties. However, common amine curing agents will produce more secondary hydroxyl groups when they react with epoxy resins, whi...

Claims

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Application Information

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IPC IPC(8): C08G59/42C08L63/00C08K5/5399C08K7/18C07C37/14C07C39/23C07C67/14C07C69/18C07C69/21C07C69/78
CPCC07C37/14C07C67/14C07C69/18C07C69/21C07C69/78C08G59/4223C08K5/5399C08K7/18C07C39/23
Inventor 杨菲李凡师剑英
Owner SHAANXI SHENGYI TECH
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