CN111978728A - Preparation method of high-frequency antenna base material resin slurry - Google Patents
Preparation method of high-frequency antenna base material resin slurry Download PDFInfo
- Publication number
- CN111978728A CN111978728A CN202010906101.0A CN202010906101A CN111978728A CN 111978728 A CN111978728 A CN 111978728A CN 202010906101 A CN202010906101 A CN 202010906101A CN 111978728 A CN111978728 A CN 111978728A
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- CN
- China
- Prior art keywords
- resin
- base material
- fluorinated polyimide
- frequency antenna
- cyanate ester
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a preparation method of resin slurry for a high-frequency antenna substrate, which comprises the steps of adding fluorinated polyimide resin and polyphenyl ether into cyanate ester, adding a mixed solvent, and heating and refluxing for 10-60 minutes to obtain the resin slurry. The copper-clad plate base material prepared from the fluorinated polyimide resin modified cyanate ester antenna base material resin slurry prepared by the method has excellent comprehensive properties of good toughness, excellent mechanical property, high dielectric property, low moisture absorption rate, high dimensional stability and the like, and meanwhile, the raw material source range is wide, the cost is low, and the copper-clad plate base material is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of high-frequency flexible communication materials and high-frequency flexible printed circuits, in particular to a preparation method of high-frequency antenna base material resin slurry.
Background
Cyanate (CE) resin is a novel thermosetting resin, the properties of which combine the high temperature resistance of Polyimide (PI) and the good processability of epoxy resin, and the cured product of the resin has good humidity and heat resistance, solubility, high dimensional stability and excellent dielectric property, thus becoming one of the attractive high-performance polymers and being widely applied to high-tech fields such as multilayer printed circuit boards, high-speed base materials of optoelectronic devices, radar radomes, high-gain antennas, stealth aircrafts and the like. Since CE is suitable for various molding processes such as press molding, transfer molding, hot pressing, winding, and pultrusion, and the main disadvantage thereof is that the brittleness of the cured resin is large, researchers have proposed many modification approaches, of which two methods commonly used are blending and copolymerization modification. The blending modification is mainly to add a small amount of rubber or high-performance thermoplastic resin into CE. The addition of the thermoplastic resin reduces the heat resistance of the CE to various degrees. The commonly used modifiers are mainly epoxy resins, Bismaleimides (BMI) or compounds with unsaturated double bonds. The cyanate ester and bismaleimide copolymer (BT resin) is widely applied to large-scale integrated printed circuit boards, high-performance wave-transmitting structure materials and the like and aerospace structure materials due to excellent electrical property, mechanical property and heat resistance. However, the BT resin also has problems of large brittleness and poor molding process.
In the prior patent (ZL201310040555.4), the cyanate ester resin (with the structure shown as formula I) is modified by the thioether bismaleimide resin, and although the performance is greatly improved, the overall performance of the resin, such as dielectric performance, moisture absorption performance, dimensional stability and the like, can not meet the high-frequency and high-speed requirements of 5G communication on antenna substrates.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of high-frequency antenna substrate resin slurry.
The invention is realized by the following technical scheme:
a preparation method of high-frequency antenna substrate resin slurry is characterized by comprising the following steps: adding the fluorinated polyimide resin and polyphenyl ether into cyanate ester, adding a mixed solvent, and heating and refluxing for 10-60 minutes to obtain the fluorinated polyimide resin cyanate ester: fluorinated polyimide resin: the weight ratio of polyphenylene oxide is 30: 7.5-75: 1-10, wherein the weight ratio of the cyanate ester to the mixed solvent is 30: 70-250.
The preparation method of the resin slurry for the base material of the high-frequency antenna is characterized in that the mixed solvent is a mixture of two or three of tetrahydrofuran, dioxane and ethylene glycol monomethyl ether.
The preparation method of the resin paste for the base material of the high-frequency antenna is characterized in that the cyanate ester is bisphenol A cyanate ester and has a structure shown in a formula I:
the preparation method of the resin paste for the base material of the high-frequency antenna is characterized in that the fluorinated polyimide resin is a maleic anhydride terminated polyimide copolymer which has a structure shown in the following formula II:
wherein R is F; r1 is H or trifluoromethyl;
r2 is
One or more of the above;
r3 is
r4 is H or CH 3;
the polymerization degrees m and n are 1, 2, 3 and 4 respectively.
The preparation method of the resin slurry for the base material of the high-frequency antenna is characterized in that the polyphenyl ether has a structure shown in a formula III:
compared with the prior art, the invention has the beneficial effects that:
the preparation method adopts the fluorinated polyimide resin with better molding process and cyanate ester copolymerization, and adopts the low boiling point solvent, thereby being beneficial to the preparation of the high-frequency copper-clad plate base material.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
30g of CY-1 bisphenol A cyanate (BADCy) resin and 5g of polyphenyl ether sold by Hubei Jusheng science and technology limited under the trade name of 30g and self-made fluorinated polyimide resin M170 g are weighed at room temperature and placed in a reaction bottle, and dioxane is added: ethylene glycol monomethyl ether: the volume ratio of tetrahydrofuran is 5: 3: 228ml (229g) of the mixed solvent of 2 was refluxed with stirring for 10 minutes to obtain a fluorinated polyimide resin-modified cyanate ester syrup.
Example 2
30g of CY-1 bisphenol A cyanate (BADCy) resin and 5g of polyphenylene oxide, which are sold by Hubei Jusheng science and technology Limited and have the commodity numbers of CY-1, are weighed at room temperature, the self-made fluorinated polyimide resin M130 g is placed in a reaction bottle, and dioxane is added: the volume ratio of ethylene glycol monomethyl ether is 6: 142ml (151g) of the mixed solvent of 4 was refluxed with stirring for 30 minutes to obtain a fluorinated polyimide resin-modified cyanate ester slurry.
Example 3
30g of CY-1 bisphenol A cyanate (BADCy) and 10g of polyphenyl ether, which are sold by Jusheng science and technology Limited in Hubei, are weighed at room temperature, 14.5 g of self-made fluorinated polyimide resin is placed in a reaction bottle, and dioxane is added: the volume ratio of tetrahydrofuran is 5: 5 (76g) was refluxed with stirring for 60 minutes to obtain a fluorinated polyimide resin-modified cyanate ester slurry.
Example 4
30g of CY-1 bisphenol A cyanate (BADCy) resin and 5g of polyphenyl ether which are sold by Hubei Jusheng science and technology limited under the trade numbers of 30g and self-made fluorinated polyimide resin M375 g are weighed and placed in a reaction bottle at room temperature, and ethylene glycol monomethyl ether is added: the volume ratio of tetrahydrofuran is 4: 231ml (226g) of the mixed solvent of 6 was refluxed with stirring for 15 minutes to obtain a fluorinated polyimide resin-modified cyanate ester slurry.
Example 5
30g of CY-1 bisphenol A cyanate (BADCy) resin and 5g of polyphenyl ether sold by Hubei Jusheng technology Limited under the trade number are weighed at room temperature, self-made fluorinated polyimide resin M330 g is placed in a reaction bottle, 150ml (145g) of ethylene glycol monomethyl ether solvent is added, and after stirring and refluxing for 30 minutes, fluorinated polyimide resin modified cyanate slurry is obtained.
Example 6
30g of CY-1 bisphenol A cyanate (BADCy) resin, 10g of polyphenyl ether and 33.5 g of self-made fluorinated polyimide resin sold by Jusheng technology Co., Ltd in a reaction bottle are weighed at room temperature, 72ml (70g) of tetrahydrofuran solvent is added, and the mixture is refluxed for 60 minutes under stirring to obtain fluorinated polyimide resin modified cyanate slurry.
Example 7
30g of CY-1 bisphenol A cyanate (BADCy) resin and 5g of polyphenyl ether which are sold by Shanbei Jusheng science and technology limited company under the trade numbers of 30g and 5g of self-made fluorinated polyimide resin M575 g are weighed at room temperature and placed in a reaction bottle, 238ml (246g) of dioxane solvent is added, then the temperature is raised to 100 ℃ under stirring, and after 10 minutes of reflux, the fluorinated polyimide resin modified cyanate ester slurry is obtained.
Example 8
30g of CY-1 bisphenol A cyanate (BADCy) resin and 5g of polyphenyl ether sold by Hubei Jusheng technology Limited under the trade designation of self-made fluorinated polyimide resin M530 g are weighed at room temperature and placed in a reaction bottle, 150ml (155g) of dioxane solvent is added, and after stirring and refluxing for 15 minutes, the fluorinated polyimide resin modified cyanate slurry is obtained.
Example 9
30g of CY-1 bisphenol A cyanate (BADCy) resin and 5g of polyphenyl ether which are sold by Hubei Jusheng science and technology limited under the commodity numbers are weighed at room temperature, 53.5 g of self-made fluorinated polyimide resin is placed in a reaction bottle, and dioxane is added: ethylene glycol monomethyl ether: the volume ratio of tetrahydrofuran is 4: 3: 80ml (80g) of the mixed solvent of 3 was refluxed with stirring for 30 minutes to obtain a fluorinated polyimide resin-modified cyanate ester slurry.
Example 10
30g of CY-1 bisphenol A cyanate (BADCy) resin, 5g of polyphenyl ether and 55.5 g of self-made fluorinated polyimide resin which are sold by Hubei Jusheng technology Limited are weighed at room temperature and placed in a reaction bottle, 90ml (93g) of dioxane solvent is added, and the mixture is refluxed for 60 minutes under stirring to obtain the fluorinated polyimide resin modified cyanate slurry.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A preparation method of high-frequency antenna substrate resin slurry is characterized by comprising the following steps: adding the fluorinated polyimide resin and polyphenyl ether into cyanate ester, adding a mixed solvent, and heating and refluxing for 10-60 minutes to obtain the fluorinated polyimide resin cyanate ester: fluorinated polyimide resin: the weight ratio of polyphenylene oxide is 30: 7.5-75: 1-10, wherein the weight ratio of the cyanate ester to the mixed solvent is 30: 70-250.
2. The method for preparing resin paste for a base material of a high-frequency antenna according to claim 1, wherein the mixed solvent is a solvent in which two or three of tetrahydrofuran, dioxane and ethylene glycol monomethyl ether are mixed.
3. The method for preparing resin paste for a base material of a high-frequency antenna according to claim 1, wherein the cyanate ester is bisphenol a cyanate ester having a structure represented by formula i:
4. the method for preparing resin paste for a base material of a high-frequency antenna according to claim 1, wherein said fluorinated polyimide resin is a maleic anhydride-terminated polyimide copolymer having a structure represented by the following formula II:
wherein R is F; r1 is H or trifluoromethyl;
r2 is
One or more of the above;
r3 is
One or more of the above;
r4 is H or CH 3.
5. The method for producing a resin paste for a substrate of a high-frequency antenna as claimed in claim 1, wherein the polyphenylene ether has a structure represented by formula III:
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| CN202010906101.0A CN111978728A (en) | 2020-09-01 | 2020-09-01 | Preparation method of high-frequency antenna base material resin slurry |
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| CN202010906101.0A CN111978728A (en) | 2020-09-01 | 2020-09-01 | Preparation method of high-frequency antenna base material resin slurry |
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| CN202010906101.0A Pending CN111978728A (en) | 2020-09-01 | 2020-09-01 | Preparation method of high-frequency antenna base material resin slurry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114349726A (en) * | 2021-12-31 | 2022-04-15 | 华南理工大学 | 2,2 ' -difluoro-4, 4 ', 5,5 ' -biphenyl tetracarboxylic dianhydride monomer and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007099803A (en) * | 2005-09-30 | 2007-04-19 | Jsr Corp | Resin composition and its cured product |
| CN102190798A (en) * | 2011-03-24 | 2011-09-21 | 中国科学院长春应用化学研究所 | Method for preparing modified cyanate resin |
| CN103965472A (en) * | 2013-02-02 | 2014-08-06 | 中山职业技术学院 | Preparation method for thioether bismaleimide resin modified cyanate ester prepreg |
| CN105440283A (en) * | 2016-01-07 | 2016-03-30 | 中国科学院长春应用化学研究所 | Modified cyanate ester resin and preparation method of modified cyanate ester resin |
| CN106498557A (en) * | 2016-09-19 | 2017-03-15 | 中山职业技术学院 | A kind of preparation method of modified nano fiber thin film |
| CN110028787A (en) * | 2018-01-11 | 2019-07-19 | 航天特种材料及工艺技术研究所 | Low-k, low-loss cyanate ester resin, wave-penetrating composite material and preparation method |
-
2020
- 2020-09-01 CN CN202010906101.0A patent/CN111978728A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007099803A (en) * | 2005-09-30 | 2007-04-19 | Jsr Corp | Resin composition and its cured product |
| CN102190798A (en) * | 2011-03-24 | 2011-09-21 | 中国科学院长春应用化学研究所 | Method for preparing modified cyanate resin |
| CN103965472A (en) * | 2013-02-02 | 2014-08-06 | 中山职业技术学院 | Preparation method for thioether bismaleimide resin modified cyanate ester prepreg |
| CN105440283A (en) * | 2016-01-07 | 2016-03-30 | 中国科学院长春应用化学研究所 | Modified cyanate ester resin and preparation method of modified cyanate ester resin |
| CN106498557A (en) * | 2016-09-19 | 2017-03-15 | 中山职业技术学院 | A kind of preparation method of modified nano fiber thin film |
| CN110028787A (en) * | 2018-01-11 | 2019-07-19 | 航天特种材料及工艺技术研究所 | Low-k, low-loss cyanate ester resin, wave-penetrating composite material and preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114349726A (en) * | 2021-12-31 | 2022-04-15 | 华南理工大学 | 2,2 ' -difluoro-4, 4 ', 5,5 ' -biphenyl tetracarboxylic dianhydride monomer and preparation method and application thereof |
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Application publication date: 20201124 |
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