Composition containing waterborne epoxy emulsion and polyphenyl ether emulsion as well as preparation method and application of composition

Abstract

The invention discloses a composition containing waterborne epoxy emulsion and polyphenyl ether emulsion as well as a preparation method and application of the composition. The composition comprises the following raw materials in parts by weight: 10-50 parts of waterborne epoxy emulsion; 10 to 50 parts of a polyphenyl ether emulsion; 10-70 parts of a water-based curing agent emulsion; 10 to 30 parts of filler; 10 to 30 parts of a flame retardant; and 0.5-1 part of a silane coupling agent. In the composition disclosed by the invention, the waterborne epoxy and the curing agent can be well compatible with PPO after being cured, so that the problem of poor compatibility of a conventional system is solved. Compared with a composition without polyphenyl ether emulsion, the composition provided by the invention can significantly reduce dielectric constant and dielectric loss, and meets strict requirements of high-frequency electronic equipment on dielectric properties of materials.

Description

Technical Field

[0001] The present invention relates to a composition containing an aqueous epoxy emulsion and a polyphenylene ether emulsion, and a preparation method and application thereof, belonging to the technical field of aqueous epoxy materials. Background Art

[0002] With the continuous development of the electronics industry, the performance requirements for copper clad laminates and prepregs are increasing day by day. In high-frequency and high-speed circuit applications, the dielectric properties of materials become key factors. Traditional compositions have limitations in meeting low dielectric constant and dielectric loss, and compatibility problems also affect the overall performance and reliability of materials. Therefore, there is an urgent need for a new type of composition to improve the existing situation and enhance the application performance of copper clad laminates and prepregs in the high-end electronics field. Summary of the Invention

[0003] Object of the Invention: To solve the above technical problems, the present invention provides a composition containing an aqueous epoxy emulsion and a polyphenylene ether emulsion, and a preparation method and application thereof. This composition has good compatibility and excellent low dielectric properties, and is suitable for the manufacture of copper clad laminates and prepregs.

[0004] Technical Solution: To achieve the above object, the present invention adopts the following technical solutions:

[0005] A composition containing an aqueous epoxy emulsion and a polyphenylene ether emulsion, the composition comprising the following raw materials in parts by weight:

[0006] 10 - 50 parts of aqueous epoxy emulsion;

[0007] 10 - 50 parts of polyphenylene ether emulsion;

[0008] 10 - 70 parts of aqueous curing agent emulsion;

[0009] 10 - 30 parts of filler;

[0010] 10 - 30 parts of flame retardant;

[0011] 0.5 - 1 part of silane coupling agent.

[0012] As a specific implementation, the aqueous epoxy emulsion is selected from liquid bisphenol A / F epoxy emulsion or solid bisphenol A / F epoxy emulsion.

[0013] As a specific implementation, the aqueous epoxy curing agent emulsion is selected from one or several of amine-based, phenolic resin-based or anhydride-based curing agents.

[0014] As a specific implementation, the filler is selected from one or a combination of silica powder, talc powder, mica powder.

[0015] As a specific embodiment, the flame retardant is selected from one or a combination of several of aluminum diethylphosphinate, aluminum hydroxide, and magnesium hydroxide.

[0016] As a specific embodiment, the silane coupling agent is selected from one or a combination of several of epoxy group silane coupling agents, amino group silane coupling agents, phenylamino group silane coupling agents, vinyl group silane coupling agents, isocyanate group silane coupling agents, propenyl group silane coupling agents, isobutenyl group silane coupling agents, styryl group silane coupling agents, ureido group silane coupling agents, chloropropyl group silane coupling agents, sulfhydryl group silane coupling agents, and sulfide group silane coupling agents.

[0017] The present invention also provides a method for preparing the composition containing the aqueous epoxy emulsion and the polyphenylene ether emulsion, comprising the following steps:

[0018] Add the aqueous epoxy emulsion, polyphenylene ether emulsion, aqueous curing agent emulsion, filler, flame retardant, and silane coupling agent into a reaction vessel, stir, and mix evenly to obtain the composition.

[0019] As a specific embodiment, the stirring speed is 200 - 1000 rpm, and the temperature is 30 - 60 °C.

[0020] Finally, the present invention provides the application of the composition containing the aqueous epoxy emulsion and the polyphenylene ether emulsion in the preparation of copper clad laminates or prepregs.

[0021] As a specific embodiment, the application includes coating the composition on a copper foil, drying, and curing to prepare a copper clad laminate.

[0022] In the composition of the present invention, the aqueous epoxy and the curing agent are well compatible with PPO after curing, overcoming the problem of poor compatibility in the previous systems. Compared with the composition without the polyphenylene ether emulsion, the composition of the present invention can significantly reduce the dielectric constant and dielectric loss, meeting the strict requirements of high-frequency electronic devices for the dielectric properties of materials.

[0023] Beneficial effects: Compared with the prior art, the present invention has the following advantages:

[0024] 1. It provides a lower dielectric constant and dielectric loss, which is beneficial to the transmission of high-frequency signals and improves the performance of electronic devices.

[0025] 2. Good compatibility ensures the stability of the material during the curing process, avoids quality problems such as delamination and cracking, and improves the reliability and service life of copper clad laminates and prepregs.

[0026] 3. Through reasonable component ratios, other important indicators such as the mechanical properties and adhesion properties of the material are taken into account, making it more advantageous in practical applications. Specific embodiments

[0027] The present invention will be further illustrated below in conjunction with specific examples.

[0028] Unless otherwise defined herein, scientific and technical terms used in this application shall have the meanings commonly understood by those of ordinary skill in the art.

[0029] 1) The raw materials of the following examples and comparative examples are specifically as follows:

[0030] Waterborne bisphenol A liquid epoxy emulsion (purchased from Handai Chemical, 60% solid content, HDL-1200);

[0031] Polyphenylene oxide emulsion (PPO powder SA90 purchased from Sabic, emulsified with a modified polyether-type epoxy resin active emulsifier (JT-801, purchased from Foshan Juntu New Materials Co., Ltd.), particle size 200-600 nm);

[0032] Phenolic resin curing agent emulsion (40% solid content, curing agent powder purchased from Shandong Shengquan, emulsified with a modified polyether-type epoxy resin active emulsifier (JT-801, purchased from Foshan Juntu New Materials Co., Ltd.), particle size 100-500 nm);

[0033] The filler is spherical silica (5 μm, purchased from Jiangsu Lianrui);

[0034] The flame retardant is aluminum diethyl phosphinate (purchased from Qingdao Opurui);

[0035] The silane coupling agent is KH-560 (purchased from Nanjing Shuguang).

[0036] 2) The product performance test methods of the following examples and comparative examples are as follows:

[0037] The peel strength is tested according to the standard of

IPC-TM650 2.4.8

[0038] Dk and Df: Tested by the SPDR (split post dielectric resonator) method, referring to the standard of

【IPC-TM650

[0039] 2.5.5.13】, the test conditions are state A and the frequency is 10 GHz;

[0040] Example 1

[0041] Add 40 parts of waterborne epoxy emulsion, 20 parts of polyphenylene oxide emulsion, 10 parts of amine curing agent emulsion (purchased from Handai Chemical, HDL-1201), 15 parts of filler, 20 parts of flame retardant, and 0.5 part of silane coupling agent into a reaction vessel, and mix evenly under specific stirring speed (500 rpm) and temperature conditions (45 °C) to obtain Composition A.

[0042] The composition A was coated on a copper foil (35 um, purchased from Kingboard Chemical Holdings Limited), and after drying (170 °C for 4 minutes) and curing (200 °C for 1.5 hours), a copper clad laminate sample 1 was prepared.

[0043] The dielectric properties of sample 1 were tested. The results showed that both its dielectric constant and dielectric loss reached the expected low levels, and it had obvious advantages compared with the comparative sample (without polyphenylene ether emulsion).

[0044] Example 2

[0045] Same as Example 1, except that the curing agent was replaced with a phenolic resin-based curing agent emulsion (HDL-1202, purchased from Handai Chemical), and a composition was obtained, and then a copper clad laminate sample was prepared.

[0046] Example 3

[0047] Same as Example 1, except that the curing agent was replaced with a liquid anhydride curing agent (methyltetrahydrophthalic anhydride), and the filler was replaced with talc powder (WF-051, purchased from Jiangsu Qunxin Technology Co., Ltd., average particle size 3.5 microns), with a dosage of 15 parts, and a composition was obtained, and then a copper clad laminate sample was prepared.

[0048] Comparative Example 1

[0049] Similar to Example 1, except that the polyphenylene ether emulsion was not added, and the dosage of the waterborne epoxy emulsion was equal to the total dosage of the waterborne epoxy emulsion and the polyphenylene ether emulsion in Example 1 to obtain a composition, and then a copper clad laminate sample was prepared.

[0050] Comparative Example 2

[0051] Similar to Example 2, except that the polyphenylene ether emulsion was not added, and the dosage of the waterborne epoxy emulsion was equal to the total dosage of the waterborne epoxy emulsion and the polyphenylene ether emulsion in Example 2 to obtain a composition, and then a copper clad laminate sample was prepared.

[0052] The samples prepared above were subjected to performance tests, and the test results are shown in the following table:

[0053]

[0054] The above test results indicate that the samples containing polyphenylene ether with different curing agent systems all exhibit good low dielectric properties and excellent peel strength, further verifying the effectiveness and practicality of the composition of the present invention.

[0055] Finally, it should be noted that the above specific embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to the examples, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solutions of the present invention, and they should all be covered within the scope of the claims of the present invention.

Claims

1. A composition comprising an aqueous epoxy emulsion and a polyphenylene ether emulsion, characterized in that: The composition comprises the following raw materials in parts by weight: 10-50 parts of water-based epoxy emulsion; 10-50 parts of polyphenylene ether emulsion; 10-70 parts of water-based curing agent emulsion; 10-30 parts of filler; Flame retardant 10-30 parts; Silane coupling agent 0.5-1 part.

2. The composition of aqueous epoxy emulsion and polyphenylene ether emulsion according to claim 1, characterized in that: The aqueous epoxy emulsion is selected from liquid bisphenol A type / F type epoxy emulsion or solid bisphenol A type / F type epoxy emulsion.

3. The composition of aqueous epoxy emulsion and polyphenylene ether emulsion according to claim 1, characterized in that: The waterborne epoxy curing agent emulsion is selected from one or more of amine, phenolic resin or acid anhydride curing agents.

4. The composition of aqueous epoxy emulsion and polyphenylene ether emulsion according to claim 1, characterized in that: The filler is selected from one or a combination of silicon micropowder, talcum powder, and mica powder.

5. The composition of aqueous epoxy emulsion and polyphenylene ether emulsion according to claim 1, characterized in that: The flame retardant is selected from one or a combination of diethyl aluminum phosphinate, aluminum hydroxide, and magnesium hydroxide.

6. The composition of aqueous epoxy emulsion and polyphenylene ether emulsion according to claim 1, characterized in that: The silane coupling agent is selected from one or a combination of epoxy silane coupling agent, amino silane coupling agent, phenylamino silane coupling agent, vinyl silane coupling agent, isocyanate silane coupling agent, acryl silane coupling agent, isobutylene silane coupling agent, styrene silane coupling agent, urea silane coupling agent, chloropropyl silane coupling agent, sulfur silane coupling agent and sulfurized silane coupling agent.

7. A method for preparing a composition of an aqueous epoxy emulsion and a polyphenylene ether emulsion according to any one of claims 1 to 6, characterized in that: The following steps are involved: Add water-based epoxy emulsion, polyphenylene ether emulsion, water-based curing agent emulsion, filler, flame retardant and silane coupling agent into a reaction container, stir and mix evenly to obtain the composition.

8. The method for preparing the composition of aqueous epoxy emulsion and polyphenylene ether emulsion according to claim 7, characterized in that: The stirring speed is 200-1000 rpm and the temperature is 30-60 degrees Celsius.

9. Use of the composition of aqueous epoxy emulsion and polyphenylene ether emulsion according to any one of claims 1 to 6 in the preparation of copper-clad laminates or prepregs.

10. The use according to claim 9, characterized in that: The application comprises coating the composition on a copper foil, drying, and curing to prepare a copper clad laminate.

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