CN106675021A - Modified wholly-aromatic liquid crystal polyester resin composite and preparation method thereof - Google Patents
Modified wholly-aromatic liquid crystal polyester resin composite and preparation method thereof Download PDFInfo
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- CN106675021A CN106675021A CN201611245237.1A CN201611245237A CN106675021A CN 106675021 A CN106675021 A CN 106675021A CN 201611245237 A CN201611245237 A CN 201611245237A CN 106675021 A CN106675021 A CN 106675021A
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- polyester resin
- crystal polyester
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/12—Polyester-amides
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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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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides modified wholly-aromatic liquid crystal/polyester resin composite, characterized by comprising, by weight, 40-90 parts of liquid crystal polyester resin, 5-30 parts of an additive, and 10-40 parts of filling material, wherein the liquid crystal polyester resin is wholly-aromatic liquid crystal polyester resin which is formed by polymerizing reaction monomers, the reaction monomers include at least one of free aromatic diamine and aromatic hydroxylamine, aromatic hydroxy carboxylic acid or aromatic amino carboxylic acid, aromatic diol, and aromatic dicarboxylic acid; the additive is polytetrafluoroethylene.
Description
Technical field
It is compound the invention belongs to field of polymer composite material, more particularly to a kind of modified all aromatic liquid crystal polyester resin
Thing and preparation method thereof.
Background technology
Flowed when all aromatic liquid crystal polyester resin (LCP) is due to excellent heat resistance, dimensional stability and melting
Property, therefore widely used as precision electronic components raw material.Particularly there is the full virtue of excellent heat resistance and electrical insulating property
Fragrant race's liquid-crystal polyester resin, it constantly expands as the prospect of high-end electronic material film and substrate raw material, especially exists
The frequency of use in electric power connector field is constantly lifted.But the electronic accessory parts of the electric power connector that LCP is made, on the one hand,
Easily make moist or be contaminated during manufacture and use, cause electric power connector to leak electricity, on the other hand, process is used in energization
In, deformation, cracking occur in the electronic accessory parts of the electric power connector that LCP is made even to be destroyed.
The content of the invention
It is an object of the invention to provide a kind of modified all aromatic liquid crystal polyester resin compound and preparation method thereof, purport
When electronic accessory parts materials of the LCP as electric power connector is solved, easily there is electric power connector electric leakage, electronic accessory parts and go out
Now deform, ftracture the problem even destroyed.
The present invention is achieved in that a kind of modified all aromatic liquid crystal polyester resin compound, by following parts by weight
Following component composition,
Liquid-crystal polyester resin 40-90 parts；
Additive 5-30 parts；
Filler 10-40 parts,
Wherein, the liquid-crystal polyester resin is all aromatic liquid crystal polyester resin, all aromatic liquid crystal polyester resin
It is polymerized by reaction monomers, the reaction monomers include at least one, the virtue in free aromatic diamine and aromatic series azanol
Fragrant race's hydroxycarboxylic acid or aromatic amine yl carboxylic acid, aromatic diol and aromatic dicarboxylic acid；The additive is polytetrafluoroethylene (PTFE).
And, a kind of preparation method of modified all aromatic liquid crystal polyester resin compound is comprised the following steps：
Formula according to above-mentioned modified all aromatic liquid crystal polyester resin compound weighs each component；
The all aromatic liquid crystal polyester resin, additive, filler are dried treatment；
The dried additive, filler are well mixed, mixture is obtained；
The mixture and all aromatic liquid crystal polyester resin are carried out into feeding treatment, is melted through double screw extruder
Extrusion, tie rod, cooling, granulation treatment.
The modified all aromatic liquid crystal polyester resin compound that the present invention is provided, it has good electrical insulating property, excellent
Mechanical performance and workability.Therefore all aromatic liquid crystal polyester resin that the present invention is provided, with than conventional phase higher
To creepage trace index, and good mechanical strength can be kept, can be used to make the former material of the electric power connector for using that is powered
Material.
The preparation method of the modified all aromatic liquid crystal polyester resin compound that the present invention is provided, first need to will only gather liquid crystal
After ester resin, additive, filler are dried, then additive, filler are mixed, mixed with liquid-crystal polyester resin, melted
Extrusion, granulation are i.e. available, the technical maturity, and method is simply controllable, it is easy to accomplish industrialization.Thus all aromatic for preparing
Brilliant polyester resin compound, it has relative discharge tracking index higher, and possesses good bending property, can be used for electronics
The raw material of connector.
Specific embodiment
In order that the technical problem to be solved in the present invention, technical scheme and beneficial effect become more apparent, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention, is not intended to limit the present invention.
A kind of modified all aromatic liquid crystal polyester resin compound is the embodiment of the invention provides, by following parts by weight
Following component is constituted,
Liquid-crystal polyester resin 40-90 parts；
Additive 5-30 parts；
Filler 10-40 parts,
Wherein, the liquid-crystal polyester resin is all aromatic liquid crystal polyester resin, all aromatic liquid crystal polyester resin
It is polymerized by reaction monomers, the reaction monomers include at least one, the virtue in free aromatic diamine and aromatic series azanol
Fragrant race's hydroxycarboxylic acid or aromatic amine yl carboxylic acid, aromatic diol and aromatic dicarboxylic acid；The additive is polytetrafluoroethylene (PTFE).
Specifically, in the embodiment of the present invention, the liquid-crystal polyester resin assigns the compound excellent as matrix composition
Heat resistance, dimensional stability and high-mechanical property.In the embodiment of the present invention, the liquid-crystal polyester resin is Wholly aromatic liquid crystal
Polyester resin.The number-average molecular weight of liquid-crystal polyester resin is 30000-60000, all aromatic liquid crystal polyester resin under height polymerization
With good electrical insulating property and excellent mechanical performance.
All aromatic liquid crystal polyester resin is polymerized by reaction monomers described in the embodiment of the present invention, specifically, described anti-
Answering monomer includes at least one in free aromatic diamine and aromatic series azanol, aromatic hydroxy-carboxylic or aromatic series aminocarboxylic
Acid, aromatic diol and aromatic dicarboxylic acid.There is all aromatic liquid crystal polyester resin of above-mentioned monomer composition, higher relative
There is more preferable heat endurance and intensity under creepage trace index.
Specific preferred, the liquid-crystal polyester resin contains at least one in following repeat units：
Repeat unit from aromatic diol：-O-Ar-O-；
Repeat unit from aromatic diamine：-HN-Ar-NH-；
Repeat unit from aromatic series azanol：-HN-Ar-O-；
Repeat unit from aromatic dicarboxylic acid：-OC-Ar-CO-；
Repeat unit from aromatic hydroxy-carboxylic：-O-Ar-CO-；
Repeat unit from aromatic amine yl carboxylic acid：-HN-Ar-CO-；
Wherein, the Ar be penylene and its derivative, biphenylene and its derivative, naphthalene and its derivative, two penylenes by
One kind in aromatic compound that the element of carbon or non-carbon is bonded and its derivative, the signified derivative of the embodiment of the present invention
Thing refers to the aromatic compound that the penylene, biphenylene, one or more hydrogen atoms on naphthalene are replaced by other elements.
Used as specific embodiment, the content of the liquid-crystal polyester resin is 40-90 parts, concretely 40 parts, 45 parts, 50
Part, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, the specific deals such as 90 parts.
In the embodiment of the present invention, the additive is polytetrafluoroethylene (PTFE), the addition of the polytetrafluoroethylene (PTFE) so that modified complete
Aromatic liquid crystal polyester resin compound has high resistance to chemical corrosion, for example the concentrated sulfuric acid,Nitric acid, hydrochloric acid, or even
Chloroazotic acidIn boil and also do not change, have sealing, high lubrication non-stick, electrical insulating property (1500 volts of high-tension electricities can be resisted) and
Good ageing resistance, heatproof are excellent (can the long-term work at a temperature of positive 250 DEG C to minus 180 DEG C), so as to significantly expand
The suitable application area of modified all aromatic liquid crystal polyester resin compound and use scope.As specific embodiment, the addition
The content of agent is 3-30 parts, concretely 3 parts, 10 parts, 15 parts, 20 parts, 25 parts, the specific deals such as 30 parts.
The effect of described filler can strengthen mechanical performance, the hot property of compound.Preferred described filler is glass fibers
At least one in dimension, whisker, carbon fiber.Used as specific embodiment, the content of described filler is 10-40 parts, concretely 10
Part, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, the specific deals such as 40 parts.
It should be noted that in the embodiment of the present invention, the content of each addO-on therapy need to meet above-mentioned requirements, if content mistake
It is low, it is difficult to play its corresponding effect；If content is too high, can be added on the contrary in the case where its effect for playing reaches saturation
Originally other performances can even, be influenceed, the raising of the liquid-crystal polyester resin compound quality is unfavorable on the contrary.
All aromatic liquid crystal polyester resin compound provided in an embodiment of the present invention, it has good electrical insulating property, excellent
Different mechanical performance and workability.The all aromatic liquid crystal polyester resin that the present invention is provided, with higher more relative than conventional
Creepage trace index, and good mechanical strength can be kept, can be used to make the raw material of the electric power connector for using that is powered.
Modified all aromatic liquid crystal polyester resin compound provided in an embodiment of the present invention, can be prepared by following methods
Obtain.
Accordingly, the embodiment of the invention provides a kind of preparation side of modified all aromatic liquid crystal polyester resin compound
Method, comprises the following steps：
S01. each component is weighed according to the formula of above-mentioned modified all aromatic liquid crystal polyester resin compound；
S02. all aromatic liquid crystal polyester resin, additive, filler are dried treatment；
S03. the dried additive, filler are well mixed, obtain mixture；
S04. the mixture and all aromatic liquid crystal polyester resin are carried out into feeding treatment, through double screw extruder
Melting extrusion, tie rod, cooling, granulation treatment.
Specifically, in above-mentioned steps S01, the formula of all aromatic liquid crystal polyester resin compound and its each preferred feelings
Condition, as described above, in order to save length, here is omitted.
Used as specific embodiment, all aromatic liquid crystal polyester resin is prepared by following methods, is specifically included
Following steps：
S011., at least two reaction monomers are provided, are carried out polycondensation reaction and is prepared liquid crystal polyester prepolyer；
S012. the liquid crystal polyester prepolymer is carried out into solid phase polycondensation and prepares liquid-crystal polyester resin.
In above-mentioned steps S011, the reaction monomers are as described above.As being preferable to carry out, the polycondensation reaction is being carried out
Before, also including being pre-processed using acylation agent to the reaction monomers.The reaction monomers can be improved by pretreatment
Reactivity, specifically, the acylation agent includes but is not limited to acetyl group agent, the acetyl group agent can be described anti-
Answering monomer carries out acetylation treatment, improves its reactivity.
The polycondensation reaction can be using the conventional method realization in this area, including but not limited to solution polycondensation, body
Condensation methods.
In above-mentioned steps S012, the solid state condensation reaction to above-mentioned liquid-crystal polyester resin prepolymer, it is necessary to be heated
Treatment.But, specific heating-up temperature is variant because of the selected reaction monomers, cannot limit in the lump herein.It is described
Heating can be by methods such as heating plate, hot blast, high temperature fluids.Additionally, the accessory substance in order to remove solid state condensation reaction, can
Using inert gas purge or utilize vacuum removing.
In above-mentioned steps S02, in order to avoid water content mistake in all aromatic liquid crystal polyester resin, additive, filler
It is high the modified all aromatic liquid crystal polyester resin composite properties that prepare to be adversely affected, it is necessary to by the liquid crystal polyester tree
Fat, additive, filler are dried treatment.Preferably, the temperature of the dried process is 120-140 DEG C, and drying time is 3-5
Hour, more preferably 4 hours.
In above-mentioned steps S03, the additive, filler are well mixed, and mixing can be realized using automatic blender, certainly,
Also can realize that mixed uniformly mode is realized using other.
In above-mentioned steps S04, the mixture and all aromatic liquid crystal polyester resin are carried out into feeding treatment, preferably
Fed from different spouts, so as to improve mixing uniformity.At double screw extruder melting extrusion, tie rod, cooling, granulation
Reason, you can obtain all aromatic liquid crystal polyester resin compound.
Used as a preferred embodiment, the additive is polytetrafluoroethylene (PTFE), and described filler is glass fibre.Selection and institute
The close polytetrafluoroethylene (PTFE) of all aromatic liquid crystal polyester resin machined parameters is stated, the injection moulding in later stage is more beneficial for, it is obtained
Liquid-crystal polyester resin compound there is relative discharge tracking index higher, and keep good mechanical strength.Thus obtain
Modified all aromatic liquid crystal polyester resin compound, can be used for the raw material of electric power connector, but be not limited only to be applied to this.
The preparation method of modified all aromatic liquid crystal polyester resin compound provided in an embodiment of the present invention, first will need to only will
After liquid-crystal polyester resin, additive, filler are dried, then additive, filler are mixed, mixed with liquid-crystal polyester resin, entered
Row melting extrusion, granulation are i.e. available, the technical maturity, and method is simply controllable, it is easy to accomplish industrialization.Thus what is prepared is complete
Aromatic series crystalline substance polyester resin compound, with more conventional relative discharge tracking index higher, and can keep it is good it is mechanical by force
Degree, can be used for the raw material of electric power connector.
Illustrated with reference to specific embodiment, wherein, all aromatic liquid crystal polyester resin is new by Jiangsu water
The limited public company of material manufacture provides, and PTFE is polytetrafluoroethylene (PTFE).
Embodiment 1
A kind of modified all aromatic liquid crystal polyester resin compound, contains each of weight percentage shown in the embodiment 1 of table 1
Component.
The preparation method of the modified all aromatic liquid crystal polyester resin compound, comprises the following steps：
S11. each component is weighed according to the formula of above-mentioned modified all aromatic liquid crystal polyester resin compound；
S12. by all aromatic liquid crystal polyester resin, additive, filler in 130 DEG C of dried process 4 hours；
S13. will be well mixed in the dried additive, filler input automatic blender, obtain mixture；
S14. the mixture and all aromatic liquid crystal polyester resin are carried out into feeding treatment, through double screw extruder
Melting extrusion, tie rod, cooling, granulation treatment.
Embodiment 2
A kind of modified all aromatic liquid crystal polyester resin compound, contains each of weight percentage shown in the embodiment 2 of table 1
Component.
The preparation method of the modified all aromatic liquid crystal polyester resin compound, it is same as Example 1.
Embodiment 3
A kind of modified all aromatic liquid crystal polyester resin compound, contains each of weight percentage shown in the embodiment 3 of table 1
Component.
The preparation method of the modified all aromatic liquid crystal polyester resin compound, it is same as Example 1.
Comparative example 1
A kind of modified all aromatic liquid crystal polyester resin compound, contains each of weight percentage shown in the comparative example 1 of table 1
Component.
The preparation method of the modified all aromatic liquid crystal polyester resin compound, it is same as Example 1.
Modified all aromatic liquid crystal polyester resin compound prepared by embodiment of the present invention 1-3 and comparative example 1 is used as note
Modeling raw material, using injection moulding machine injection moulding, then carries out performance test, and the method for performance test is as follows：
(1) relative discharge tracking index：Tested by ASTM D3638-93；
(2) bending strength：Tested by ASTM D-790.
Test result is as shown in table 2 below.
Table 1
Table 2
From upper table 2, the modified all aromatic liquid crystal polyester resin compound manufactured in embodiment 1-3 is relative to contrast
The resin complexes manufactured in example 1, with the increase of PTFE contents, its relative discharge tracking index significantly increases, while more
Good bending strength can be kept under relative discharge tracking index high in embodiment 1-3.Therefore, according to produced by the present invention complete
Aromatic liquid crystal polyester resin compound can be used as the raw material of electric power connector, but not only limit is applied to this.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (9)
1. a kind of modified all aromatic liquid crystal polyester resin compound, it is characterised in that by the following component of following parts by weight
Composition,
Liquid-crystal polyester resin 40-90 parts；
Additive 5-30 parts；
Filler 10-40 parts,
Wherein, the liquid-crystal polyester resin is all aromatic liquid crystal polyester resin, and all aromatic liquid crystal polyester resin is by anti-
Monomer is answered to be polymerized, the reaction monomers include at least one, the aromatic series in free aromatic diamine and aromatic series azanol
Hydroxycarboxylic acid or aromatic amine yl carboxylic acid, aromatic diol and aromatic dicarboxylic acid；The additive is polytetrafluoroethylene (PTFE).
2. be modified all aromatic liquid crystal polyester resin compound as claimed in claim 1, it is characterised in that the liquid crystal polyester
Resin contains at least one in following repeat units：
Repeat unit from aromatic diol：-O-Ar-O-；
Repeat unit from aromatic diamine：-HN-Ar-NH-；
Repeat unit from aromatic series azanol：-HN-Ar-O-；
Repeat unit from aromatic dicarboxylic acid：-OC-Ar-CO-；
Repeat unit from aromatic hydroxy-carboxylic：-O-Ar-CO-；
Repeat unit from aromatic amine yl carboxylic acid：-HN-Ar-CO-；
Wherein, the Ar be penylene and its derivative, biphenylene and its derivative, naphthalene and its derivative, two penylenes by carbon or
One kind in aromatic compound that the element of non-carbon is bonded and its derivative.
3. be modified all aromatic liquid crystal polyester resin compound as claimed in claim 1, it is characterised in that described filler is glass
At least one in glass fiber, whisker, carbon fiber.
4. a kind of preparation method of modified all aromatic liquid crystal polyester resin compound, comprises the following steps：
Formula according to the modified all aromatic liquid crystal polyester resin compound as described in claim 1-3 is any weighs each component；
The all aromatic liquid crystal polyester resin, additive, filler are dried treatment；
The dried additive, filler are well mixed, mixture is obtained；
The mixture and all aromatic liquid crystal polyester resin are carried out into feeding treatment, is squeezed through double screw extruder melting
Go out, tie rod, cooling, granulation treatment.
5. the preparation method of all aromatic liquid crystal polyester resin compound as claimed in claim 4 modified, it is characterised in that institute
The temperature for stating dried process is 120-140 DEG C.
6. the preparation method of all aromatic liquid crystal polyester resin compound as claimed in claim 4 modified, it is characterised in that institute
State all aromatic liquid crystal polyester resin to be prepared by following methods, specifically include following steps：
At least two reaction monomers are provided, are carried out polycondensation reaction and is prepared liquid crystal polyester prepolyer；
The liquid crystal polyester prepolymer is carried out into solid phase polycondensation and prepares liquid-crystal polyester resin.
7. the preparation method of all aromatic liquid crystal polyester resin compound as claimed in claim 6 modified, it is characterised in that institute
The method for stating polycondensation reaction is solution polycondensation or bulk polycondensation method.
8. the preparation method of modified all aromatic liquid crystal polyester resin compound as claimed in claims 6 or 7, its feature exists
In being pre-processed to the reaction monomers using acylting agent.
9. the preparation method of all aromatic liquid crystal polyester resin compound as claimed in claim 4 modified, it is characterised in that institute
Additive is stated for polytetrafluoroethylene (PTFE), described filler is glass fibre.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611245237.1A CN106675021A (en) | 2016-12-29 | 2016-12-29 | Modified wholly-aromatic liquid crystal polyester resin composite and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611245237.1A CN106675021A (en) | 2016-12-29 | 2016-12-29 | Modified wholly-aromatic liquid crystal polyester resin composite and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108822453A (en) * | 2018-05-30 | 2018-11-16 | 浙江德清科赛塑料制品有限公司 | A kind of high-strength polytetrafluoroethyl-ne material and its needle-like shut-off valve of preparation |
| US11917753B2 (en) | 2019-09-23 | 2024-02-27 | Ticona Llc | Circuit board for use at 5G frequencies |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923306A (en) * | 2014-04-08 | 2014-07-16 | 金发科技股份有限公司 | Liquid crystal polyester and liquid crystal polyester composition consisting of liquid crystal polyester and application of liquid crystal polyester composition |
| CN105602210A (en) * | 2015-12-29 | 2016-05-25 | 江苏沃特特种材料制造有限公司 | Light liquid crystal polyester resin compound and preparation method thereof |
-
2016
- 2016-12-29 CN CN201611245237.1A patent/CN106675021A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923306A (en) * | 2014-04-08 | 2014-07-16 | 金发科技股份有限公司 | Liquid crystal polyester and liquid crystal polyester composition consisting of liquid crystal polyester and application of liquid crystal polyester composition |
| CN105602210A (en) * | 2015-12-29 | 2016-05-25 | 江苏沃特特种材料制造有限公司 | Light liquid crystal polyester resin compound and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108822453A (en) * | 2018-05-30 | 2018-11-16 | 浙江德清科赛塑料制品有限公司 | A kind of high-strength polytetrafluoroethyl-ne material and its needle-like shut-off valve of preparation |
| US11917753B2 (en) | 2019-09-23 | 2024-02-27 | Ticona Llc | Circuit board for use at 5G frequencies |
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