CN106674938A - Dust-free liquid crystal polyester compound and preparation method and application thereof - Google Patents
Dust-free liquid crystal polyester compound and preparation method and application thereof Download PDFInfo
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- CN106674938A CN106674938A CN201611253548.2A CN201611253548A CN106674938A CN 106674938 A CN106674938 A CN 106674938A CN 201611253548 A CN201611253548 A CN 201611253548A CN 106674938 A CN106674938 A CN 106674938A
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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
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/52—Liquid crystal materials characterised by components which are not liquid crystals, e.g. additives with special physical aspect: solvents, solid particles
- C09K19/54—Additives having no specific mesophase characterised by their chemical composition
- C09K19/542—Macromolecular compounds
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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Abstract
The invention discloses a dust-free liquid crystal polyester compound and a preparation method and application thereof. The dust-free liquid crystal polyester compound disclosed by the invention comprises the following components in parts by weight: 40 to 80 parts of liquid crystal polyester resin, 5 to 20 parts of polyphenylene sulfide resin, and 20 to 40 parts of filler. According to the dust-free liquid crystal polyester compound disclosed by the invention, the liquid crystal polyester resin is used as a basic resin component and is modified by the contained components of the polyphenylene sulfide resin, the filler and the like, so that a low friction coefficient and high mechanical strength are given to the dust-free liquid crystal polyester compound disclosed by the invention; the dust-free liquid crystal polyester compound accords with the dust-free production requirement; the preparation method of the dust-free liquid crystal polyester compound is easy to control in process; prepared materials are stable in performance; production cost of the dust-free liquid crystal polyester compound is effectively reduced.
Description
Technical field
The invention belongs to technical field of polymer composite materials, and in particular to it is a kind of without dust liquid crystal polyester complex and its
Preparation method and application.
Background technology
Liquid-crystal polyester resin (LCP) is due to excellent mobile performance, electrical insulation capability, heat resistance, dimensionally stable
Performance etc., therefore it is widely used in the fields such as electronics, electric, automobile, aerospace.Printed circuit board (PCB), food can also be used for
Packaging, artificial satellite electronic unit, electric and automobile component, even as spacecraft component materials.Electron trade is
First big consumption market of liquid crystal polyester material, at past 10 years with the fast development of the consumer electronics industry, such as mobile phone, flat
The first-class field of plate computer, vehicle-mounted pick-up, camera module demand steeply rises, and the wide market demand causes relevant industries to send out
Exhibition is swift and violent.
It is a kind of outstanding shooting due to the mobile performance that LCP materials are excellent, high intensity, thermostability and dimensional stability
Head mould group manufacture material, but with the development of industry, camera module is further harsh to the performance requirement of material, especially senior
Camera module requires that material not only has high intensity, and more requiring the part of material manufacture will not produce in use powder
Dirt, to avoid polluting camera lens, reduces the definition of photographic head, and conventional liquid crystal polyester material is often unable to reach these and wants
Ask.
The content of the invention
It is an object of the invention to overcome the shortcomings of that above-mentioned prior art is present, there is provided a kind of compound without dust liquid crystal polyester
Thing and preparation method and application, to solve available liquid crystal polyester resin coefficient of friction height, that non-dusting property is differed from is strong with machinery
The undesirable technical problem of degree.
In order to realize foregoing invention purpose, one aspect of the present invention, there is provided one kind is without dust liquid crystal polyester complex.It is described
Include the component of following parts by weight without dust liquid crystal polyester complex：
Liquid-crystal polyester resin 40-80 parts
Polyphenylene sulfide 5-20 parts
Filler 20-40 parts.
A kind of another aspect of the present invention, there is provided preparation method without dust liquid crystal polyester complex.The preparation method
Comprise the steps：
Each component raw material is weighed respectively without the constituent species and content contained by dust liquid crystal polyester complex according to the present invention；
The each component raw material for weighing is carried out into melting mixing extrusion process.
The another aspect of the embodiment of the present invention, there is provided a kind of present invention is without dust liquid crystal polyester complex or present invention system
Preparation Method prepare without dust liquid crystal polyester complex in camera module, precision connector, plug connector or electronic devices and components
Application.
Compared with prior art, the present invention is without dust liquid crystal polyester complex resin group based on liquid-crystal polyester resin
Point, it is modified to it by components such as contained polyphenylene sulfide, fillers, it is compound without dust liquid crystal polyester so as to give the present invention
The excellent mechanical performance of thing and low-friction coefficient, meet non-dusting production requirement.
The present invention is without dust liquid crystal polyester complex preparation method according to the present invention without contained by dust liquid crystal polyester complex
Constituent species and ratio directly each component is carried out into melting mixing extrusion process so that each component can be fully dispersed and each other
Between have an effect so that the mechanical performance excellent without dust liquid crystal polyester complex of extrusion and low-friction coefficient, meet nothing
The production requirement of dust.In addition, preparation method technique of the present invention is easily-controllable, the strong mechanical property of preparation effectively reduces its life
Produce cost.
There is excellent mechanical performance, low-friction coefficient without dust liquid crystal polyester complex just because of the present invention, meet
Non-dusting production requirement, effectively extends its range of application, is such as particularly well-suited to camera module material, effectively increases phase
Answer the quality of product such as camera module and the stability of work.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention
Limit the present invention.
The weight of embodiment of the present invention Related Component noted in the disclosure not only may refer to the concrete of each component
Content, it is also possible to represent the proportionate relationship of weight between each component, therefore, as long as according to embodiment of the present invention description relevant group
The content divided is scaled up or reduced within embodiment of the present invention description scope of disclosure.Specifically, the present invention is real
It can be mass unit known to the chemical fields such as μ g, mg, g, kg to apply the weight described in a description.
On the one hand, the embodiment of the present invention provides one kind without dust liquid crystal polyester complex.It is described multiple without dust liquid crystal polyester
Compound includes the component of following parts by weight：
Liquid-crystal polyester resin 40-80 parts
Polyphenylene sulfide 5-20 parts
Filler 20-40 parts.
So, the present embodiment is without dust liquid crystal polyester complex resin Composition based on liquid-crystal polyester resin, by institute
The components such as the polyphenylene sulfide, the filler that contain are modified to it, so as to give the present invention without the high machine of dust liquid crystal polyester complex
Tool intensity and low coefficient of friction, meet the requirement without dust production.
Specifically, in the above-mentioned liquid crystal polyester complex embodiment without dust, the liquid-crystal polyester resin selects all aromatic
Liquid-crystal polyester resin.In one embodiment, all aromatic liquid crystal polyester resin number-average molecular weight is 10000-100000, should
The molecular resin measurer of scope has can give the excellent mobility of complex and processing characteristics.As one embodiment of the invention,
Above-mentioned all aromatic liquid crystal polyester resin is at least containing following any one repetitive：
(1) from the repetitives of aromatic diol：-O-Ar-O-；
(2) from the repetitives of aromatic diamine：-HN-Ar-NH-；
(3) from the repetitives of aromatic series azanol：-HN-Ar-O-；
(4) from the repetitives of aromatic dicarboxylic acid：-OC-Ar-CO-；
(5) from the repetitives of aromatic hydroxy-carboxylic：-O-Ar-CO-；
(6) from the repetitives of aromatic amine yl carboxylic acid：-HN-Ar-CO-.
Wherein, the Ar groups in above-mentioned (1) to the repetitives shown in (6) be penylene, biphenylene, naphthalene, two penylenes by
The aromatic compound that the element of carbon or non-carbon is bonded any one, or for penylene, biphenylene, naphthalene, two penylenes by carbon or
The aromatic compound that more than one hydrogen in the aromatic compound that the element of non-carbon is bonded is replaced by other elements.
Thus all aromatic liquid crystal polyester resin of construction unit monomer manufacture has excellent resistance to elevated temperatures and mobility, processing
Property.
Above-mentioned liquid-crystal polyester resin can with but be not only prepared as follows acquisition：
First the first monomer and second comonomer are carried out into polycondensation reaction, then the polycondensation reaction is synthesized into Wholly aromatic liquid crystal
Polyester prepolyer carries out solid state polycondensation and prepares.
Wherein, first monomer is at least one in free aromatic diol, aromatic diamine, aromatic series azanol,
The second comonomer is at least one in aromatic dicarboxylic acid, aromatic hydroxy-carboxylic, aromatic amine yl carboxylic acid.It is specifically fragrant
Fragrant race's glycol, aromatic diamine, aromatic series azanol, aromatic dicarboxylic acid, aromatic hydroxy-carboxylic, aromatic amine yl carboxylic acid
To be but not only from conventional respective compound.
In a further embodiment, above-mentioned first monomer and/or second comonomer be before above-mentioned polycondensation reaction is carried out, in advance
By acylation agent pretreatment, to improve reactive monomeric.Specifically, the acylation agent is at least in acetyl group agent
Kind.It is specific such as when acylation agent for acetyl group agent when, the monomer of pretreatment first and/or second comonomer are improving the first monomer
And/or the acetylizad monomer of second comonomer reactivity.
During polycondensation reaction synthesis Wholly aromatic liquid crystal polyester prepolyer to be carried out solid state polycondensation, by solid phase
Polycondensation reaction carries the molecular weight of product, obtains the suitable liquid-crystal polyester resin of molecular weight.Need in the solid state polycondensation process
Heat treated, such as can adopt can provide heat energy using heating plate, hot blast, high temperature fluid method to solid state polycondensation.For
The by-product of solid state polycondensation is removed, using inert gas purge or vacuum removing is utilized.
The surface that the above-mentioned polyphenylene sulfide without contained by dust liquid crystal polyester complex can improve composite article is smooth
Property improves the toughness of material to reduce coefficient of friction.In one embodiment, the polyphenylene sulfide can directly from commercially available poly-
Diphenyl sulfide resin.
The above-mentioned filler without contained by dust liquid crystal polyester complex can rise with polyphenylene sulfide to liquid-crystal polyester resin
To synergistic effect, matrix liquid-crystal polyester resin is acted on, be effectively improved the mechanical performance without dust liquid-crystal polyester resin and reduction
The coefficient of friction of material so that it meets the non-dusting requirement of production.In one embodiment, filler be glass fibre, whisker,
One or two kinds of in wollastonite, Pulvis Talci, Muscovitum, titanium dioxide, white carbon black, Calcium Carbonate, clay, barium sulfate, silicon dioxide
Mixture above.Wherein, the preferred size of glass fibre and/or whisker is diameter 5-15um, and length 2-6mm, wollastonite is sliding
Stone powder, Muscovitum, titanium dioxide, white carbon black, Calcium Carbonate, clay, barium sulfate, any one preferable particle size scope is 200- in silicon dioxide
1250 mesh.
Therefore, it is above-mentioned without dust liquid crystal polyester complex logical polyphenylene sulfide, filler to liquid-crystal polyester resin based on
Resin Composition is acted on, so as to give the present invention without the excellent mechanical performance of dust liquid crystal polyester complex and low-friction coefficient, symbol
Close non-dusting production requirement.
On the other hand, embodiments provide the one kind without dust liquid crystal polyester complex in above-described embodiment to prepare
Method.In one embodiment, it is described to comprise the steps without dust liquid crystal polyester complex preparation method：
Step S01：Weigh respectively without the constituent species and content contained by dust liquid crystal polyester complex as described above
Each component raw material；
Step S02：The each component raw material for weighing is carried out into melting mixing extrusion process.
Wherein, the content of each component for weighing in above-mentioned steps S01 and selected composition are as described above without dust
Described in liquid crystal polyester complex, in order to save length, will not be described here.
In above-mentioned steps S02, each component raw material in the presence of the high pressure and hyperpyrexia that melting mixing is extruded it is fully dispersed simultaneously
Have an effect each other, so as to realize to liquid-crystal polyester resin act on so that Jing melting mixings extrusion obtain target product without
Dust liquid crystal polyester complex, and give there is low coefficient of friction and excellent mechanicalness without dust liquid crystal polyester complex
Can, meet non-dusting production requirement.In one embodiment, the melting mixing extrusion temperature is 310-350 DEG C, so that respectively
Group is sufficiently mixed in the molten state uniform and abundant effect, reduces without dust liquid crystal polyester complex coefficient of friction, improves it
Mechanical strength.
In one embodiment, above-mentioned melting mixing extrusion can with but not only lead to weight-loss type automatic feeder and throw in original in proportion
Material, by double screw extruder melting mixing extrusion process is carried out.
In addition, before above-mentioned steps S02 are carried out, also including that each component raw material to weighing is dried process, such as exist
It is dried 4 hours at 130-160 DEG C.
After treating step S02, can also include to the generation of melting mixing extrusion process without dust liquid crystal polyester complex
Carry out the subsequent steps such as tie rod, cooling, pelletize.
Therefore, the embodiment of the present invention without dust liquid crystal polyester complex preparation method as described above without dust liquid crystal
Each component is directly carried out melting mixing extrusion process by the constituent species and ratio contained by polyester complexes so that each component can
It is fully dispersed and have an effect each other so that, and the machinery low without dust liquid crystal polyester complex coefficient of friction of extrusion
Intensity is high, meets non-dusting production requirement.In addition, the preparation method technique is easily-controllable, the strong mechanical property of preparation, effectively drop
Low its production cost.
Based on it is above-mentioned without dust liquid crystal polyester complex and preparation method thereof on the basis of, just because of the present invention without dust
Liquid crystal polyester complex has that coefficient of friction is low, mechanical strength, and production can be reached without dust requirement, effectively extended
Its range of application, is such as particularly well-suited to camera module material, because the resin material of such as camera module has low friction,
High mechanical strength, can reach production without dust requirement, effectively increase the quality such as camera module, and, it is to avoid powder
Dustiness contaminates camera lens, it is ensured that the definition of photographic head.
It is described in detail without dust liquid crystal polyester complex and preparation method thereof to above-mentioned below in conjunction with specific embodiment.
Embodiment 1
One kind is present embodiments provided without dust liquid crystal polyester complex and preparation method thereof.It is described without dust liquid crystal polyester
Complex includes the component and content of the parts by weight in table 1 below.Wherein, liquid-crystal polyester resin average molecular weight is 45000, glass
The size of glass fiber be 10 μm of diameter, length 4.5mm.
Preparation method without dust liquid crystal polyester complex is as follows：
S11. the preparation of liquid-crystal polyester resin：Resin structure unit be P-hydroxybenzoic acid, p-phthalic acid, xenol,
6- hydroxyl -2- naphthoic acids and M-phthalic acid, acetylizing agent is acetic anhydride；
S12. according to the parts by weight described in embodiment 1 in table 1, the liquid-crystal polyester resin (Wholly aromatic liquid crystal that will be selected
Polyester resin, Jiangsu water special material Manufacturing Co., Ltd) 50 parts, 20 parts of polyphenylene sulfide, 30 parts of glass fibre is 130
DEG C drying 4 hours；
S13. by the dried liquid-crystal polyester resin of step S12, polyphenylene sulfide glass fibre input weight-loss type feeding
Machine, melting mixing is carried out by feeding machine by raw material input double screw extruder according to formula proportion at 330 DEG C, is then passed through
Extrusion, tie rod, cooling, pelletize is produced without dust liquid crystal polyester complex.
Embodiment 2
One kind is present embodiments provided without dust liquid crystal polyester complex and preparation method thereof.It is described without dust liquid crystal polyester
Complex includes the component and content of the parts by weight in table 1 below.Wherein, liquid-crystal polyester resin average molecular weight is 45000, sliding
The size of stone powder is 325 mesh.
Preparation method without dust liquid crystal polyester complex is as follows：
S21. the preparation of liquid-crystal polyester resin：Resin structure unit be P-hydroxybenzoic acid, p-phthalic acid, xenol,
6- hydroxyl -2- naphthoic acids and M-phthalic acid, acetylizing agent is acetic anhydride；
S22. according to the parts by weight described in embodiment 2 in table 1, the liquid-crystal polyester resin (Wholly aromatic liquid crystal that will be selected
Polyester resin, Jiangsu water special material Manufacturing Co., Ltd) 50 parts, 20 parts of polyphenylene sulfide, 30 parts of Pulvis Talci be at 130 DEG C
It is dried 4 hours；
S23. by the dried liquid-crystal polyester resin of step S22, polyphenylene sulfide, Pulvis Talci input weight-loss type feeding
Machine, melting mixing is carried out by feeding machine by raw material input double screw extruder according to formula proportion at 330 DEG C, is then passed through
Extrusion, tie rod, cooling, pelletize is produced without dust liquid crystal polyester complex.
Embodiment 3
One kind is present embodiments provided without dust liquid crystal polyester complex and preparation method thereof.It is described without dust liquid crystal polyester
Complex includes the component and content of the parts by weight in table 1 below.Wherein, liquid-crystal polyester resin average molecular weight is 45000, glass
The size of glass fiber be 10 μm of diameter, length 4.5mm.
Preparation method without dust liquid crystal polyester complex is as follows：
S31. the preparation of liquid-crystal polyester resin：Resin structure unit be P-hydroxybenzoic acid, p-phthalic acid, xenol,
6- hydroxyl -2- naphthoic acids and M-phthalic acid, acetylizing agent is acetic anhydride；
S32. according to the parts by weight described in embodiment 3 in table 1, the liquid-crystal polyester resin (Wholly aromatic liquid crystal that will be selected
Polyester resin, Jiangsu water special material Manufacturing Co., Ltd) 65 parts, 5 parts of polyphenylene sulfide, 30 parts of glass fibre be 130
DEG C drying 4 hours；
S33. by the dried liquid-crystal polyester resin of step S32, polyphenylene sulfide, glass fibre input weight-loss type feeding
Machine, melting mixing is carried out by feeding machine by raw material input double screw extruder according to formula proportion at 330 DEG C, is then passed through
Extrusion, tie rod, cooling, pelletize is produced without dust liquid crystal polyester complex.
Comparative example 1
A kind of liquid-crystal polyester resin complex is provided, it includes the component and content of the parts by weight in table 1 below.Its system
Preparation method of the Preparation Method with reference to embodiment 1.
Comparative example 2
A kind of liquid-crystal polyester resin complex is provided, it includes the component and content of the parts by weight in table 1 below.Its system
Preparation method of the Preparation Method with reference to embodiment 1.
The test of respective performances
The liquid crystal provided without dust liquid crystal polyester complex and comparative example 1,2 that above-described embodiment 1 to embodiment 3 is provided
Polyester resin complex respectively as injection raw material, using injection moulding machine injection mo(u)lding, then by following examination criteria pair
It carries out performance test and is tested respectively, and test result is as described in Table 2：
(1) bending strength：Test by ASTM D-790.
(2) coefficient of friction：Tested by ASTM D1894 methods.
Table 1
Table 2
With reference to above-mentioned table 2, embodiment 1-3 has more compared with the liquid-crystal polyester resin complex manufactured in comparative example 1,2
Low coefficient of friction, while possess higher bending strength, can be used as camera module material.
Specific embodiment used herein is set forth to the principle and embodiment of the present invention, the explanation of embodiment
It is only intended to help and understands the method for the present invention and its core concept, the foregoing is only presently preferred embodiments of the present invention,
Not to limit the present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc.,
Should be included within the scope of the present invention.
Claims (10)
1. one kind is without dust liquid crystal polyester complex, it is characterised in that including the component of following parts by weight：
Liquid-crystal polyester resin 40-80 parts
Polyphenylene sulfide 5-20 parts
Filler 20-40 parts.
2. according to claim 1 without dust liquid crystal polyester complex, it is characterised in that：Described filler be glass fibre,
One kind in whisker, wollastonite, Pulvis Talci, Muscovitum, titanium dioxide, white carbon black, Calcium Carbonate, clay, barium sulfate, silicon dioxide or
Two or more mixture.
3. according to claim 1 and 2 without dust liquid crystal polyester complex, it is characterised in that：The liquid-crystal polyester resin
For all aromatic liquid crystal polyester resin, all aromatic liquid crystal polyester resin number-average molecular weight is 10000-100000.
4. according to claim 3 without dust liquid crystal polyester complex, it is characterised in that：The Wholly aromatic liquid crystal polyester
Resin is at least containing following any one repetitive：
-O-Ar-O-、-HN-Ar-NH-、-HN-Ar-O-、-OC-Ar-CO-、-O-Ar-CO-、-HN-Ar-CO-；
And the Ar groups in the repetitives are that penylene, biphenylene, naphthalene, two penylenes are bonded by the element of carbon or non-carbon
Aromatic compound any one, or the virtue being bonded by the element of carbon or non-carbon for penylene, biphenylene, naphthalene, two penylenes
The aromatic compound that more than one hydrogen in fragrant compounds of group is replaced by other elements.
5. arbitrary described without dust liquid crystal polyester complex according to claim 3-4, it is characterised in that：The all aromatic liquid
Brilliant polyester prepolyer is first the first monomer and second comonomer to be carried out into polycondensation reaction, then by the full fragrance of polycondensation reaction synthesis
Race's liquid crystal polyester prepolymer carries out solid state polycondensation and prepares；Wherein, first monomer is free aromatic diol, virtue
At least one in fragrant race's diamidogen, aromatic series azanol, the second comonomer is aromatic dicarboxylic acid, aromatic hydroxy-carboxylic, virtue
At least one in fragrant race's amino carboxylic acid.
6. according to claim 5 without dust liquid crystal polyester complex, it is characterised in that：First monomer and/or
Two monomers are in advance by acylation agent pretreatment.
7. according to claim 6 without dust liquid crystal polyester complex, it is characterised in that：The acylation agent is acetyl group
At least one in agent.
8. a kind of preparation method without dust liquid crystal polyester complex, comprises the steps：
Weigh respectively without the constituent species and content contained by dust liquid crystal polyester complex according to claim 1-7 is arbitrary described
Each component raw material；
The each component raw material for weighing is carried out into melting mixing extrusion process.
9. preparation method according to claim 8, it is characterised in that：The temperature of the melting mixing extrusion process is 310-
350℃。
10. claim 1-7 is arbitrary described without dust liquid crystal polyester complex or by the arbitrary described system of claim 8-9
Preparation Method prepare without dust liquid crystal polyester complex in camera module, precision connector, plug connector or electronic devices and components
Application.
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| US12104010B2 (en) | 2021-02-04 | 2024-10-01 | Ticona Llc | Polymer composition for an electric circuit protection device |
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| CN111417681B (en) * | 2017-12-05 | 2023-08-22 | 提克纳有限责任公司 | Aromatic polymer composition for camera module |
| US11086200B2 (en) | 2019-03-20 | 2021-08-10 | Ticona Llc | Polymer composition for use in a camera module |
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Application publication date: 20170517 |