CN105542408A - Modified wholly aromatic liquid crystal polyester resin composition and preparation method thereof - Google Patents
Modified wholly aromatic liquid crystal polyester resin composition and preparation method thereof Download PDFInfo
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- CN105542408A CN105542408A CN201511010425.1A CN201511010425A CN105542408A CN 105542408 A CN105542408 A CN 105542408A CN 201511010425 A CN201511010425 A CN 201511010425A CN 105542408 A CN105542408 A CN 105542408A
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
- C08L67/03—Polyesters derived from dicarboxylic acids and dihydroxy compounds the dicarboxylic acids and dihydroxy compounds having the carboxyl- and the hydroxy groups directly linked to aromatic rings
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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Abstract
The invention belongs to the technical field of high-molecular composite materials, and particularly discloses a modified wholly aromatic liquid crystal polyester resin composition and a preparation method thereof. The composition is prepared from the following components in parts by weight: 50-70 parts of liquid crystal polyester resin, 0.5-5 parts of additive, 0-40 parts of filler I and 0-30 parts of filler II. The wholly aromatic liquid crystal polyester resin composition has the most prominent performance of low dielectric constant, and is excellent in other performances, such as mechanical performance, heat resistance and the like, has low melt viscosity, and finally shows excellent processing performance. Therefore, the modified wholly aromatic liquid crystal polyester resin composition can be widely applied to the field of high-frequency electronic parts.
Description
Technical field
The present invention relates to technical field of polymer composite materials, particularly relate to a kind of modification all aromatic liquid crystal polyester resin mixture and preparation method thereof.
Background technology
Because all aromatic liquid crystal polyester resin (English abbreviation: LCP) has excellent thermotolerance, dimensional stability and melt fluidity, be highly suitable for the starting material doing precision instrument parts.Especially again in conjunction with it, there is excellent electrical insulation characteristics, therefore, high-end electronic material membrane and substrate raw materials can also be widely used in, and application prospect is very optimistic.
Along with the high speed development of electronics and information industry, electronics is further obvious to the trend of high frequency future development, especially the high speed development of electronic product, communication goods, satellite transmission, information products move towards at a high speed and high frequency gradually, based on this material needing performance more excellent.Therefore, this also proposes requirements at the higher level to the performance as the raw-material LCP of electronic unit.And the high frequency tolerant characteristic of material is determined by its dielectricity the subject of knowledge and the object of knowledge, because the transfer rate of signal and the square root of material dielectric constant are inversely proportional to, high-k easily causes signal transmission delay, therefore, in the electronic unit in future, the specific inductivity (Dk) of LCP material must be little and stable.But current LCP mixture due to its dielectric properties not good, during electronic devices and components field for high frequency, postpone long, the loss of signal is large, often causes final signal distortion.
Based on existing defect, this patent, by optimizing the formula of LCP mixture, solves the problems referred to above to the LCP mixture by providing a kind of specific inductivity significantly to reduce.
Summary of the invention
The present invention solves the large problem of existing all aromatic liquid crystal polyester resin mixture specific inductivity, provides a kind of modification all aromatic liquid crystal polyester resin mixture and preparation method thereof.
To achieve the above object of the invention, the embodiment of the present invention have employed following technical scheme:
A kind of modification all aromatic liquid crystal polyester resin mixture, comprises the component that parts by weight are following:
And a kind of preparation method of modification all aromatic liquid crystal polyester resin mixture, at least comprises the following steps:
S01, take liquid-crystal polyester resin as above, additive, filler one and filler two in proportion;
S02, respectively the described liquid-crystal polyester resin taken, additive, filler one and filler two is carried out drying treatment;
S03, liquid-crystal polyester resin, additive, filler one and filler two by after S02 process carry out mixing treatment;
S04, the mixture that S03 obtains is carried out melting mixing, extrudes, tie rod, cooling, granulation process.
The above embodiment of the present invention only adopts additive, filler one and filler two pairs of liquid-crystal polyester resins to carry out modification, mechanical property can be obtained, Good Heat-resistance, melt viscosity reduce and the modification all aromatic liquid crystal polyester resin mixture that obviously reduces of specific inductivity, meanwhile, this modification Wholly aromatic liquid crystal polyester tree mixture also has good processing characteristics.
The preparation method of the modification all aromatic liquid crystal polyester resin mixture that the embodiment of the present invention provides, raw materials for production are simple, without the need to adding too much auxiliary agent, the technique adopting liquid-crystal polyester resin and additive and two kinds of fillers to carry out mixing treatment to melt extrude again, what can make uniform filling is scattered in liquid-crystal polyester resin, finally obtains the mixture that performance is more excellent.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides a kind of modification all aromatic liquid crystal polyester resin mixture, comprises the component that parts by weight are following:
Wherein,
In any one embodiment, liquid-crystal polyester resin refers to all aromatic liquid crystal polyester resin.The all aromatic liquid crystal polyester resin related to is prepared in the following manner:
At least two kinds of monomers are adopted to carry out polycondensation, to synthesize Wholly aromatic liquid crystal polyester prepolyer; Then solid phase polycondensation is carried out to the Wholly aromatic liquid crystal polyester prepolyer obtained, finally obtain all aromatic liquid crystal polyester resin.
Here the monomer related to comprises at least one in free aromatic diol, aromatic diamine and aromatic series azanol and fragrant race dicarboxylic acid.Further, monomer can also comprise at least one in aromatic hydroxy-carboxylic and aromatic amine yl carboxylic acid.
In all aromatic liquid crystal polyester resin that any one embodiment is all, all there is the feature of repeating unit.
Wherein, the repeating unit that free aromatic diol comprises is :-O-Ar-O-;
The repeating unit that aromatic diamine comprises is:
The repeating unit that aromatic series azanol comprises is:
The repeating unit that aromatic dicarboxylic acid comprises is:
The repeating unit that aromatic hydroxy-carboxylic comprises is:
The repeating unit that aromatic amine yl carboxylic acid comprises is:
In above repeating unit, Ar represents that penylene, biphenylene, naphthalene or two penylenes carry out the aromatics of bonding by the element of carbon or non-carbon; Or penylene, biphenylene, naphthalene or two penylenes carry out by the element of carbon or non-carbon the aromatics that at least one protium in the aromatics that bonding formed replaced by other elements.
In the preparation process of above-mentioned all aromatic liquid crystal polyester resin, can solution polycondensation be adopted, also can adopt bulk polycondensation method.And in order to promote polycondensation, can the materials such as acylation agent be used to carry out pre-treatment to raw material in the process of synthesis Wholly aromatic liquid crystal polyester prepolyer, ethanoyl agent especially can be adopted to carry out pre-treatment.
In above-mentioned solid phase polycondensation (solid state condensation reaction), need to provide suitable heat to Wholly aromatic liquid crystal polyester prepolyer, concrete heat supply is by methods such as hot-plate, hot blast, high temperature fluids, and in order to remove the by product of solid state condensation reaction, inert gas purge can be utilized or utilize vacuum removing.
In any embodiment, additive is Polyhedral oligomeric silsesquioxanes (English name: polyhedraloligomericsilsesquioxame; English abbreviation: POSS).
Particularly, the physical size of POSS is 0.7-3nm, and molecular formula is (RSiO
1.5) Σ n, wherein, Σ n is the multiple of 2, and minimum value is 6.
In above-mentioned molecular formula, R represents any one of hydrogen atom, alkyl, phenyl, cycloalkyl, carboxyl, epoxy group(ing), alkyl, vinyl, styryl.The additive of this type can reduce the specific inductivity of mixture.
In arbitrary embodiment, filler one is at least one in glass fibre, whisker, poly-carbon fiber, tetrafluoroethylene.The interpolation of filler one, can strengthen mixture mechanical property, thermotolerance.
In arbitrary embodiment, filler two is at least one in wollastonite, talcum powder, mica, titanium dioxide, carbon black, calcium carbonate, clay, barium sulfate, silicon-dioxide.The interpolation of filler two can strengthen mixture thermotolerance, electrical property.
The modification all aromatic liquid crystal polyester resin mixture that the above embodiment of the present invention provides, all aromatic liquid crystal polyester resin and Polyhedral oligomeric silsesquioxanes have good consistency, without the need to adding other compatilizers, obtained modification all aromatic liquid crystal polyester resin mixture has good mechanical properties and resistance toheat, and melt viscosity and specific inductivity low, and have good processing characteristics.
Correspondingly, the present invention, on the basis of above-described embodiment, further provides the preparation method of embodiment of the present invention modification all aromatic liquid crystal polyester resin mixture.In one embodiment, the preparation method of described modification all aromatic liquid crystal polyester resin mixture at least comprises the following steps:
S01, take liquid-crystal polyester resin as above, additive, filler one and filler two in proportion;
S02, respectively the described liquid-crystal polyester resin taken, additive, filler one and filler two is carried out drying treatment;
S03, liquid-crystal polyester resin, additive, filler one and filler two by after S02 process carry out mixing treatment;
S04, the mixture that S03 obtains is carried out melting mixing, extrudes, tie rod, cooling, granulation process.
Wherein, in step S02, the temperature of drying treatment is 130 DEG C ~ 160 DEG C, and the treatment time is 4 ~ 6h.The object of drying treatment mainly makes raw material fully dry, avoids moisture on the impact of final product performance.
In step S03, the object that liquid-crystal polyester resin, Polyhedral oligomeric silsesquioxanes, filler one and filler two first carry out mixing makes filler disperse in the composite more evenly, to improve composite properties, automatic blender can be selected to mix.Certainly, automatic blender is not limited to.
In step S04, preferred twin screw extruder carries out melting mixing.Fuse under the screw speed of 300RPM-600RPM, barrel temperature is 320 DEG C ~ 370 DEG C, controls vacuum tightness at 0.5MPa ~ 0.8MPa.
The preparation method of the modification all aromatic liquid crystal polyester resin mixture that the above embodiment of the present invention provides, raw materials for production are simple, without the need to adding too much auxiliary agent, the technique adopting liquid-crystal polyester resin, additive and two kinds of fillers first to carry out combination treatment to carry out again melt extruding, what can make uniform filling is scattered in resin, obtains the mixture that performance is more excellent.
No matter be the above-mentioned modification all aromatic liquid crystal polyester resin mixture provided or the modification all aromatic liquid crystal polyester resin mixture having above-mentioned preparation method to prepare, all can be applied in high frequency electronic component field.Certainly, be applied to the Application Areas that high frequency electronic component is the modification all aromatic liquid crystal polyester resin mixture that the embodiment of the present invention provides, the modification all aromatic liquid crystal polyester resin mixture provided due to the embodiment of the present invention is except having low specific inductivity, also there is excellent mechanical property and resistance toheat, and there is the advantages such as melt viscosity is low, so its Application Areas is not limited only to high frequency electronic component.
In order to modification all aromatic liquid crystal polyester resin mixture that the embodiment of the present invention provides and preparation method thereof is better described, all crosses embodiment below and be illustrated.
Embodiment 1
A kind of modification all aromatic liquid crystal polyester resin mixture, comprises the component that parts by weight are following:
The preparation method of the modification all aromatic liquid crystal polyester resin mixture that embodiment 1 provides is as follows:
Step S01, by all aromatic liquid crystal polyester resin (water special material Manufacturing Co., Ltd provides by Jiangsu) 64.5 parts, ten phenylbenzene POSS0.5 parts, 25 parts, glass fibre, talcum powder 10 parts to be placed at 130 DEG C of temperature dry 4 hours;
Step S02, by dried all aromatic liquid crystal polyester resin, ten phenylbenzene POSS, glass fibre and talcum powder drop into automatic blender mix, obtain mixture;
Step S03, the mixture obtained by step S02 drop into twin screw extruder and carry out melting mixing, and then through extruding, tie rod, cooling, granulation, obtains modification all aromatic liquid crystal polyester resin mixture.
Embodiment 2
A kind of modification all aromatic liquid crystal polyester resin mixture, comprises the component that parts by weight are following:
The preparation method of the modification all aromatic liquid crystal polyester resin mixture that embodiment 2 provides is as follows:
Step S01, by all aromatic liquid crystal polyester resin (water special material Manufacturing Co., Ltd provides by Jiangsu) 64 parts, ten phenylbenzene POSS1 parts, 25 parts, glass fibre, talcum powder 10 parts to be placed at 130 DEG C of temperature dry 4 hours;
Step S02, by dried all aromatic liquid crystal polyester resin, ten phenylbenzene POSS, glass fibre and talcum powder drop into automatic blender mix, obtain mixture;
Step S03, the mixture obtained by step S02 drop into twin screw extruder and carry out melting mixing, and then through extruding, tie rod, cooling, granulation, obtains modification all aromatic liquid crystal polyester resin mixture.
Embodiment 3
A kind of modification all aromatic liquid crystal polyester resin mixture, comprises the component that parts by weight are following:
The preparation method of the modification all aromatic liquid crystal polyester resin mixture that embodiment 1 provides is as follows:
Step S01, by all aromatic liquid crystal polyester resin (water special material Manufacturing Co., Ltd provides by Jiangsu) 64 parts, ten phenylbenzene POSS5 parts, 25 parts, glass fibre, talcum powder 6 parts to be placed at 130 DEG C of temperature dry 4 hours;
Step S02, by dried all aromatic liquid crystal polyester resin, ten phenylbenzene POSS, glass fibre and talcum powder drop into automatic blender mix, obtain mixture;
Step S03, the mixture obtained by step S02 drop into twin screw extruder and carry out melting mixing, and then through extruding, tie rod, cooling, granulation, obtains modification all aromatic liquid crystal polyester resin mixture.
Comparative example 1
A kind of modification all aromatic liquid crystal polyester resin mixture, comprises the component that parts by weight are following:
All aromatic liquid crystal polyester resin 65;
Glass fibre 25;
Talcum powder 10.
The preparation method of the modification all aromatic liquid crystal polyester resin mixture that comparative example 1 provides is as follows:
Step S01, by all aromatic liquid crystal polyester resin (water special material Manufacturing Co., Ltd provides by Jiangsu) 65 parts, 25 parts, glass fibre, talcum powder 10 parts to be placed at 130 DEG C of temperature dry 4 hours;
Step S02, by dried all aromatic liquid crystal polyester resin, glass fibre and talcum powder drop into automatic blender mix, obtain mixture;
Step S03, the mixture obtained by step S02 drop into twin screw extruder and carry out melting mixing, and then through extruding, tie rod, cooling, granulation, obtains modification all aromatic liquid crystal polyester resin mixture.
In order to verify composite properties prepared by the embodiment of the present invention 1 ~ 3 and comparative example 1, mixture above-described embodiment 1-3 and comparative example 1 obtained respectively is as injection raw material, use injection moulding machine injection moulding, then the performance of mixture in test and Evaluation operation example and comparative example by the following method:
(1) tensile strength
The tensile strength that the embodiment of the present invention relates to is tested by ASTMD-638.
(2) heat-drawn wire
The heat-drawn wire that the embodiment of the present invention relates to is tested by ASTMD-648.
(3) specific inductivity
The specific inductivity that the embodiment of the present invention relates to is tested by ASTMD-150, and test frequency is 1KHz and 1MHz.
(4) melt viscosity
Melt viscosity that the embodiment of the present invention relates to uses capillary rheometer (RH2000) to measure under the condition of 330 DEG C and 1000/s.
Above-mentioned test result is added up in table 1.
Composite properties test result in table 1 embodiment and comparative example
From upper table 1, the resin complexes of its mixture of modification all aromatic liquid crystal polyester resin mixture prepared by embodiment 1-3 preparation in the specific inductivity of 1KHz and 1MHz is than comparative example 1 obviously reduces, and other performances are as the excellence such as mechanical property, resistance toheat; Meanwhile, melt viscosity is low, shows good processing characteristics.Thus, the LCP mixture prepared according to the embodiment of the present invention can be used for high frequency electronic component field.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement or improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a modification all aromatic liquid crystal polyester resin mixture, comprises the component that parts by weight are following:
2. modification all aromatic liquid crystal polyester resin mixture as claimed in claim 1, is characterized in that: described liquid-crystal polyester resin is all aromatic liquid crystal polyester resin.
3. modification all aromatic liquid crystal polyester resin mixture as claimed in claim 2, is characterized in that: the step preparation as described below of described all aromatic liquid crystal polyester resin:
A, employing at least two kinds of monomers carry out condensation polymerization and help aromatic liquid-crystal polyester prepolymer;
B, described Wholly aromatic liquid crystal polyester prepolyer is carried out solid state condensation reaction;
Wherein, described monomer is at least one in free aromatic diol, aromatic diamine and aromatic series azanol and aromatic dicarboxylic acid.
4. modification all aromatic liquid crystal polyester resin mixture as claimed in claim 3, is characterized in that: described monomer also comprises at least one in aromatic hydroxy-carboxylic and aromatic amine yl carboxylic acid.
5. the modification all aromatic liquid crystal polyester resin mixture as described in as arbitrary in claim 2-4, is characterized in that: described free aromatic diol, aromatic diamine, aromatic series azanol, aromatic dicarboxylic acid, aromatic hydroxy-carboxylic and aromatic amine yl carboxylic acid comprise following repeating unit respectively :-O-Ar-O-,
Wherein, Ar is penylene, biphenylene, naphthalene or two penylenes carry out the aromatics of bonding by the element of carbon or non-carbon; Or the protium that penylene, biphenylene, naphthalene or two penylenes to be undertaken in the aromatics of bonding at least one by the element of carbon or non-carbon replace by other elements the aromatics formed.
6. modification all aromatic liquid crystal polyester resin mixture as claimed in claim 1, is characterized in that: described additive is Polyhedral oligomeric silsesquioxanes.
7. the modification all aromatic liquid crystal polyester resin mixture as described in as arbitrary in claim 1-2, is characterized in that: described filler one is at least one in glass fibre, whisker, carbon fiber, tetrafluoroethylene; And/or described filler two is at least one in wollastonite, talcum powder, mica, titanium dioxide, carbon black, calcium carbonate, clay, barium sulfate, silicon-dioxide.
8. a preparation method for modification all aromatic liquid crystal polyester resin mixture, at least comprises the following steps:
S01, in proportion take as arbitrary in claim 1-7 as described in liquid-crystal polyester resin, additive, filler one and filler two;
S02, respectively the described liquid-crystal polyester resin taken, additive, filler one and filler two is carried out drying treatment;
S03, liquid-crystal polyester resin, additive, filler one and filler two by after S02 process carry out mixing treatment;
S04, the mixture that S03 obtains is carried out melting mixing, extrudes, tie rod, cooling, granulation process.
9. the preparation method of modification all aromatic liquid crystal polyester resin mixture as claimed in claim 8, is characterized in that: the temperature of described drying treatment is 130 DEG C ~ 160 DEG C, and the treatment time is 4 ~ 6h.
10. the preparation method of modification all aromatic liquid crystal polyester resin mixture as claimed in claim 8, is characterized in that: the equipment of described melting mixing is twin screw extruder.
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| CN106633680A (en) * | 2016-12-29 | 2017-05-10 | 江苏沃特特种材料制造有限公司 | Modified liquid crystal polyester resin composition, preparation method thereof and application of composition |
| CN109937230A (en) * | 2016-11-18 | 2019-06-25 | 住友化学株式会社 | The manufacturing method of foam molding and foam molding |
| CN110218464A (en) * | 2019-06-30 | 2019-09-10 | 瑞声新材料科技(常州)有限公司 | Polymer, adhesive sheet and its preparation method and application |
| CN111073258A (en) * | 2019-12-24 | 2020-04-28 | 江苏沃特特种材料制造有限公司 | Polyphenyl ether composite material and preparation method thereof |
| CN113121962A (en) * | 2019-12-30 | 2021-07-16 | 深圳市沃特新材料股份有限公司 | Polytetrafluoroethylene/liquid crystal polymer composite material and preparation method thereof |
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Application publication date: 20160504 |