CN110499026A - Modified liquid crystal polymer film and its preparation method and application - Google Patents
Modified liquid crystal polymer film and its preparation method and application Download PDFInfo
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- CN110499026A CN110499026A CN201910857683.5A CN201910857683A CN110499026A CN 110499026 A CN110499026 A CN 110499026A CN 201910857683 A CN201910857683 A CN 201910857683A CN 110499026 A CN110499026 A CN 110499026A
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- liquid crystal
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
- H05K1/05—Insulated conductive substrates, e.g. insulated metal substrate
- H05K1/056—Insulated conductive substrates, e.g. insulated metal substrate the metal substrate being covered by an organic insulating layer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
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Abstract
The invention belongs to liquid crystal polymer technical fields, and in particular to a kind of modified liquid crystal polymer film and its preparation method and application.The modified liquid crystal polymer film comprising following component: polyhenylene benzo dithiazole, crosslinking agent, conducting particles, ultraviolet absorber, coupling agent and filler；The crosslinking agent is anilinomethyl triethoxysilane, and the coupling agent is the modified triethoxysilane of phthalic anhydride.Technical solution provided by the invention is by adding suitable crosslinking agent and coupling agent, solves the problems, such as the processing film forming of liquid crystal polymer, the PBT film of production has the excellent performances such as low moisture absorption, low-k, low-dielectric loss and high temperature resistant, and organic solvent-free participates in process, environmental-friendly.
Description
Technical field
The invention belongs to liquid crystal polymer technical fields, and in particular to a kind of modified liquid crystal polymer film and its preparation side
Method and application.
Background technique
Flexible circuit board (Flexible Printed Circuit Board) is also known as " FPC flexible board ", is with flexible
Printed circuit made of insulating substrate has the advantages that many rigid printed circuit boards do not have.It can be with free bend, volume
Around, fold, any arrangement can be required according to space layout, and arbitrarily move and flexible in three-dimensional space, to reach component
Assemble the integration connected with conducting wire.It can be substantially reduced the volume of electronic product using FPC flexible board, be applicable in electronic product to height
The needs that density, miniaturization, highly reliable direction are developed.
Copper foil base material (english abbreviation FCCL:Flexible Copper Clad Laminate), also known as are as follows: flexible
Copper-clad plate, flexible copper-clad plate, Flexible copper-clad plate, FCCL are the processing substrates of FPC.FCCL composition mainly includes three categories material:
Cover membrane material, metallic conductor foil and adhesive.Covering membrane material mainly has polyester (PET) film, polyimides (PI) at present
Film, polyesterimide film, fluorine carbon vinyl film, sub- nylon paper, polybutylene terephthalate film etc..Wherein, at present
Use to be most widely polyester film (PET film) and Kapton (PI film).
More polyimides is applied at present, and dielectric constant and fissipation factor are larger, Yi Fare, moisture absorption is big, thermally expand system
Number is uncontrollable, and properties of product are not sufficiently stable, and high-frequency transmission loss is serious, architectural characteristic is poor, can not adapt to current
The high-frequency high-speed development trend of FPC.
Liquid crystal polymer is also liquid crystal polymer, refer under certain condition can with high-molecular compound existing for liquid crystalline phase,
Its main feature is that molecule molecular weight with higher has ordered orientation again.Belong in the strand of the high polymer of this kind of material and contains
Rodlike or laminated structure mesomorphic unit makes Formation of liquid crystals rigidity or semi-rigid chain structure.Liquid crystal both had as liquid
Mobility and continuity, and the anisotropy the same with crystal.Because it is with low moisture absorption, low-k and low-dielectric loss
Characteristic, and with the epoch of 5G high-speed transfer arrive, the PI film for being now widely used for FCCL will be substituted.Because they
Orientation in a mold is too high, and molecular weight is excessive, therefore is difficult processing film forming.
Summary of the invention
The present invention provides modified liquid crystal polymer films and its preparation method and application, to solve current liquid crystal high score
The son problem difficult for FPC film forming.
In order to solve the above-mentioned technical problem, the technical scheme is that the modified liquid crystal polymer film comprising
Following component: polyhenylene benzo dithiazole (PBT), crosslinking agent, conducting particles, ultraviolet absorber, coupling agent and filler；The friendship
Connection agent is anilinomethyl triethoxysilane, and the coupling agent is the mixture of the modified triethoxysilane of phthalic anhydride, and phthalic anhydride changes
The triethoxysilicane alkyl structure of property is shown in formula I:
Optionally, the average number-average degree of polymerization of the PBT is 12000-30000.
Optionally, the modified triethoxysilane of the phthalic anhydride is with phthalic anhydride, allyl amine and triethoxysilane for original
Material is synthesized through imidization reaction, two step of catalyzing addition reaction of silicon with hydrogen.
Optionally, the conducting particles is fabricated in situ nano-silver colloid.Nano-silver colloid has polymolecularity.
Optionally, the ultraviolet absorbing agent is selected from septichen phenyl ester, 2- (- 5 ˊ of 2 ˊ-hydroxyl-aminomethyl phenyl) benzene
And triazole or 2,4 dihydroxyl benzophenone.
Optionally, the filler is silica.
Optionally, each component accounting by weight is as follows:
Optionally, the modified liquid crystal polymer film 3GHz dielectric constant 2.5-2.9, thermal expansion coefficient (CTE) are 15-
16PPM/ DEG C, water absorption rate 0.02-0.04%, transverse tensile strength 320-350MPa, endwise tensile strength 320-350MPa, loss
Factor 0.001-0.003.
The present invention also provides the preparation methods of above-mentioned modified liquid crystal polymer film comprising following steps: by each group
Divide and melt, be kneaded in double screw extruder, then extrusion, cooling, drying and pelletizing squeeze modified particle in twin-screw again
It is melted in machine out, carries out secondary mixing, finally squeezed out, be cast slab or blown film, last biaxial tension film forming.
Optionally, 350-380 DEG C of the melting temperature, 320-350 DEG C of the secondary melting temperature, longitudinal stretching multiple 5-
20, transverse stretch ratio 5-20.
The present invention also provides application of the above-mentioned modified liquid crystal polymer film in FPC industry.
Technical solution provided by the invention solves adding for liquid crystal polymer by adding suitable crosslinking agent and coupling agent
Work film forming problem, the PBT film of production have the excellent performances such as low moisture absorption, low-k, low-dielectric loss and high temperature resistant, and
And organic solvent-free participates in process, it is environmental-friendly.
Specific embodiment
In order to make it easy to understand, illustrating described modified liquid crystal polymer film and preparation method thereof below with reference to embodiment and answering
With, it should be appreciated that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
Raw materials used reagent is commercial goods, the equipment of process and use unless otherwise indicated in following embodiments
It is also method and apparatus commonly used in the art unless otherwise specified.
The preparation of 1 coupling agent of embodiment
In reaction flask, 14.8g phthalic anhydride and 180ml glacial acetic acid is added, 5.7g allyl is added after stirring and dissolving
Base amine reacts at room temperature 1h, is heated to reflux 4h, and 170ml water is added after being cooled to room temperature, is heated to boiling, be cooled to room temperature, there is white
Solid is precipitated, and filters, washing, then recrystallization purification.
In reaction flask, product 7.4g and 100ml toluene is walked in addition, is added after stirring and dissolving and contains platinum catalysis, agent, nitrogen
8.21g triethoxysilane is added in protection, 50 DEG C of activation 30min, and 70 DEG C are warming up to after adding, and reacts 3h, is cooled to room temperature,
After removing solvent, recrystallization obtains the modified triethoxysilane coupling agent of phthalic anhydride.
The group of 2 PBT film of embodiment is grouped as
The group of 3 PBT film of embodiment is grouped as
The preparation of 4 PBT film of embodiment
Each component in embodiment 2 or 3 is melted in double screw extruder, is kneaded, melting temperature is 350 DEG C, squeezes out, is cold
But, dry and pelletizing, then melts modified particle in double screw extruder again, carries out secondary mixing, secondary mixing temperature
Degree is 320 DEG C, finally extrusion, curtain coating slab and biaxial tension film forming, 8 times of longitudinal stretching, 8 times of cross directional stretch.
5 comparative experiments of embodiment
With embodiment 2 and 3 be raw material by the present invention, the film prepared with embodiment 4 compared with commercially available FCP PI film into
Row performance test, test result are shown in Table 1.
Table 1
As shown in table 1, modified liquid crystal polymer film provided by the invention has superior performance, more suitable to be used as FCP
Covering membrane material.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations.Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment, or some or all of the technical features are equal
Replacement, and these modifications or substitutions, the model for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (10)
1. a kind of modified liquid crystal polymer film, which is characterized in that including following component: polyhenylene benzo dithiazole, crosslinking agent,
Conducting particles, ultraviolet absorber, coupling agent and filler；The crosslinking agent is anilinomethyl triethoxysilane, the coupling agent
For the modified triethoxysilane of phthalic anhydride, the triethoxysilicane alkyl structure that phthalic anhydride is modified is shown in formula I:
2. being modified liquid crystal polymer film according to claim 1, which is characterized in that the polyhenylene benzo dithiazole is put down
Equal number-average degree of polymerization is 12000-30000.
3. being modified liquid crystal polymer film according to claim 1, which is characterized in that the modified triethoxysilicane of the phthalic anhydride
Alkane is to close using phthalic anhydride, allyl amine and triethoxysilane as raw material through imidization reaction, two step of catalyzing addition reaction of silicon with hydrogen
At.
4. being modified liquid crystal polymer film according to claim 1, which is characterized in that the conducting particles is received for fabricated in situ
Rice elargol.Nano-silver colloid has polymolecularity.
5. being modified liquid crystal polymer film according to claim 1, which is characterized in that the ultraviolet absorbing agent is selected from adjacent hydroxyl
Yl benzoic acid phenyl ester, 2- (- 5 ˊ of 2 ˊ-hydroxyl-aminomethyl phenyl) benzotriazole or 2,4 dihydroxyl benzophenone.
6. being modified liquid crystal polymer film according to claim 1, which is characterized in that the filler is silica.
7. being modified liquid crystal polymer film according to claim 1, which is characterized in that the modified liquid crystal polymer film
3GHz dielectric constant 2.5-2.9, thermal expansion coefficient (CTE) is 15-16PPM/ DEG C, water absorption rate 0.02-0.04%, to tensile strength
320-350MPa, endwise tensile strength 320-350MPa, loss factor 0.001-0.003.
8. the preparation method of any modified liquid crystal polymer film of claim 1-7, which is characterized in that including walking as follows
It is rapid: each component being melted in double screw extruder, is kneaded, squeezes out, is cooling, dry and pelletizing, then again by modified particle
It is melted in double screw extruder, carries out secondary mixing, finally squeezed out, be cast slab and biaxial tension film forming.
9. preparation method according to claim 8, which is characterized in that 350-380 DEG C of the melting temperature, the secondary mixing
320-350 DEG C of temperature, longitudinal stretching multiple 5-20, transverse stretch ratio 5-20.
10. application of any modified liquid crystal polymer film of claim 1-7 in FPC industry.
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| CN2019106120796 | 2019-07-08 | ||
| CN201910612079.6A CN110256850A (en) | 2019-07-08 | 2019-07-08 | Modified liquid crystal polymer film and its preparation method and application |
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| CN110499026B CN110499026B (en) | 2021-11-26 |
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Cited By (4)
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| CN112973637A (en) * | 2021-02-20 | 2021-06-18 | 杭州楠大环保科技有限公司 | High-efficiency waste gas treating agent and preparation method and application thereof |
| CN113246438A (en) * | 2021-07-06 | 2021-08-13 | 苏州固泰新材股份有限公司 | Single screw extruder for processing liquid crystal polymer and film forming method |
| CN113308111A (en) * | 2021-06-03 | 2021-08-27 | 宁夏清研高分子新材料有限公司 | Liquid crystal polymer film for flexible printed circuit board and preparation method thereof |
| CN114106579A (en) * | 2020-08-31 | 2022-03-01 | 宁波长阳科技股份有限公司 | Hollow mesoporous silicon sphere modified liquid crystal polymer film and preparation method thereof |
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| CN111690326A (en) * | 2020-05-12 | 2020-09-22 | 深圳市信维通信股份有限公司 | Preparation method of liquid crystal polymer film or liquid crystal polymer copper-clad plate |
| CN113480868B (en) * | 2021-06-29 | 2022-10-04 | 宁波长阳科技股份有限公司 | Liquid crystal polymer film and preparation method thereof |
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| CN113246438A (en) * | 2021-07-06 | 2021-08-13 | 苏州固泰新材股份有限公司 | Single screw extruder for processing liquid crystal polymer and film forming method |
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| Publication number | Publication date |
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| CN110499026B (en) | 2021-11-26 |
| CN110256850A (en) | 2019-09-20 |
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