CN102352259A - Liquid crystal polymer composition, preparation method and application thereof - Google Patents
Liquid crystal polymer composition, preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a liquid crystal polymer composition, a preparation method and application thereof. The liquid crystal polymer composition is prepared from the following components in percent by mass: 30-60 percent of liquid crystal polymer, 15-35 percent of inorganic reinforcing agent, 5-35 percent of filler and 2-5 percent of toughening component, wherein the toughening component comprises silicone powder and fluorochemicals. The liquid crystal polymer composition has better flexibility and weld mark strength, and overcomes the defects of low weld mark strength and easiness in crispness of the traditional TLCP (talline polymer).
Description
Technical field
The invention belongs to the special engineering plastics field, be specifically related to a kind of liquid-crystalline polymer composition and preparation method thereof and application.
Background technology
TLCP (TLCP) is compared with other organic polymer material, has comparatively distinctive molecular structure and thermal behavior, and its molecule is made up of the rigid rod macromolecular chain, forms a kind of liquid crystal state that has solid and liquid property concurrently after the melted by heating.The phase structure of this uniqueness is given TLCP following characteristic: have the self-enhancement effect; Coefficient of linear expansion is little; Excellent heat resistance; Have from flame retardant resistance; Melt viscosity is low, good fluidity; Molding shrinkage is little; Chemical proofing is good etc.
TLCP also has the weak point of self: during moulding in die cavity two strands of materials converge the place be along the bonding wire orientation, so weld mark strength is low because crystalline forms; There is fragility in thin molded article.Electron device more and more develops to thin-walled, miniaturization at present, and is therefore more and more higher to material requirements, not only requires material to have excellent flowability, and requires material to have thin-walled toughness preferably.
Chinese patent CN 101307174A discloses the method that obtains surface-mounting electronic component through liquid-crystalline polymer composition: compound as glass fibre and the liquid crystalline polymers of 100-20.0m as 4-8m, number average length through using number average diameter; The material warp for preparing is little; Reduced the problem that causes welding compound to move because of product distortion, but the toughness of not mentioning product there is improvement.
Chinese patent CN1974672A discloses the preparation of compositions method of a kind of liquid crystalline polymer blends and this mixture: the liquid crystal polymer (A) that with fusing point is 250-330 ℃; Compound according to 50: 50 to 90: 10 scope with fusing point more than or equal to 190 ℃ of liquid crystal polymers (B) less than 250 ℃; Resulting liquid-crystalline polymer composition shows good mechanical performance (as extending modulus) and good molded operability and low buckling deformation is arranged at low temperatures; It is high that but the method requires raw material sources; Be difficult for obtaining, the weld mark strength of gained material is not seen yet has improvement.
WIPO patent WO 96/06888 discloses a kind of liquid-crystalline polymer composition; Play interior lubrication through in liquid crystalline polymers, adding low molecular weight polyethylene; And can not influence the flame retardant resistance of liquid crystalline polymers during less than 2.5wt% at addition, but the weld mark strength of material does not see that improvement is arranged.
US Patent No. 4983688 discloses a kind of liquid-crystalline polymer composition; Can improve toughness, chemical resistant properties and the mechanical property of liquid crystalline polymers through interpolation multivalence attitude aromatic carboxylic acid metal-salt in liquid crystalline polymers; But this method requires the aromatic carboxylic acid metal-salt to have excellent thermotolerance; Otherwise can not satisfy service requirements, and the material weld mark strength of this patent does not see that improvement is arranged.
Summary of the invention
In order to overcome the defective of available liquid crystal polymkeric substance weld mark place's undercapacity and available liquid crystal polymkeric substance thin-walled goods poor toughness, primary and foremost purpose of the present invention be to provide a kind of flowability preferably, the higher liquid-crystalline polymer composition of weld mark place intensity.
Another object of the present invention is to provide the preparation method of above-mentioned liquid-crystalline polymer composition.
A further object of the present invention is to provide the application of above-mentioned liquid-crystalline polymer composition.
The object of the invention is realized through following technical proposals:
A kind of liquid-crystalline polymer composition is that the composition by following mass percent prepares:
Liquid crystalline polymers: 30-60%
Inorganic strengthening agent: 15-35%
Filler: 5-35%
Toughness reinforcing component: 2-5%;
Preferably, above-mentioned liquid-crystalline polymer composition is prepared by the composition of following mass percent:
Liquid crystalline polymers: 37-57%
Inorganic strengthening agent: 15-30%
Filler: 10-30%
Toughness reinforcing component: 2-3%;
Described liquid crystalline polymers is made up of 4-hydroxymethyl-benzoic acid (PHBA), terephthalic acid (TA), 6-hydroxynaphthoic acid (HNA) and '-biphenyl diphenol repeated structural units such as (BP); The structural formula of 4-hydroxymethyl-benzoic acid (PHBA), terephthalic acid (TA), 6-hydroxynaphthoic acid (HNA) and '-biphenyl diphenol repeated structural units such as (BP) is suc as formula shown in the I-IV:
Described liquid crystalline polymers is made up of by following molar content 4 kinds of above-mentioned repeated structural units:
Formula (I): 40-60%
Formula (II): 10-20%
Formula (III): 10-20%
Formula (IV): 20-40%;
The melt temperature of said liquid crystalline polymers is 310-350 ℃;
Described inorganic strengthening agent is a kind of in circular cross section glass fibre, oval cross section glass fibre, rectangular cross section glass fibre, sapphire whisker, carbon fiber, potassium titanate fiber, boric acid fibre or the wollastonite fibre; A kind of in circular cross section glass fibre, oval cross section glass fibre or the rectangular cross section glass fibre;
Described filler is a kind of in glass flake, mica, glass microballon, talcum powder, clay, wollastonite, graphite, lime carbonate, barium sulfate or the titanium dioxide;
Described toughness reinforcing component is made up of high molecular weight silicone powder and fluorochemicals;
Described fluorochemicals is a kind of in multipolymer (PFA) or the tetrafluoroethylene and the hexafluoropropylene copolymer (FEP) of multipolymer (ETFE), tetrafluoroethylene and perfluoroalkyl vinyl ether of tetrafluoroethylene and ethene.
The preparation method of above-mentioned liquid-crystalline polymer composition may further comprise the steps:
(1) liquid crystalline polymers is dry;
(2) liquid crystalline polymers that step (1) is obtained and toughness reinforcing component blend obtain the premix system;
(3) premix system, inorganic strengthening agent and the filler that step (2) is obtained joins in the forcing machine;
(4) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition;
Step (1) is described dry with liquid crystalline polymers, is at 170 ℃ of dry 4-6h, makes its moisture mass percent below 0.1%;
The described blend of step (2) is in high mixer, to carry out;
The described premix system that step (2) is obtained of step (3) joins in the forcing machine, is to join the forcing machine from twin screw extruder master spout through the weight-loss metering scale;
Step (3) is described to join inorganic strengthening agent and filler in the forcing machine, is respectively inorganic strengthening agent and filler to be joined the forcing machine from twin screw extruder side spout through the weight-loss metering scale;
Above-mentioned crystalline polymer can be used to make junctor, electrical condenser, switch, circuit wafer, pick up camera module and rly..
Principle of the present invention is: the toughness reinforcing component of excellent heat resistance; It is the combination of silicone powder and fluorochemicals; Can not only play good toughening effect to the liquid-crystalline polymer composition of gained; And can improve the flowability of liquid-crystalline polymer composition; Mobile improvement can promote that filler component better disperses, thereby reaches the purpose of improving the resulting product weld mark strength.
The present invention has following advantage and effect with respect to prior art:
(1) the present invention makes up through selecting suitable toughness reinforcing component and flow ability modifying agent, can not only play good toughening effect to institute's inventive composition, and can improve the weld mark strength of resulting product.
(2) toughness reinforcing component of the present invention is easy to get, and addition means is simple.
Description of drawings
Fig. 1 is the liquid-crystalline polymer composition sample figure that is used for the flowing property test.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Embodiment 1
A kind of preparation method of liquid-crystalline polymer composition may further comprise the steps:
(1) with liquid crystalline polymers Ueno LCP A2500 (constituting 340 ℃ of melt temperatures by PHBA/HNA/BP/TA) at 170 ℃ of dry 4-6h, make its moisture mass percent below 0.1%;
(2) get liquid crystalline polymers and 1% silicone powder, 1% tetrafluoroethylene and the hexafluoropropylene copolymer (FEP) that 38% step (1) obtains and place the high mixer blend, obtain the premix system;
(3) the premix system that step (2) is obtained joins the forcing machine from twin screw extruder master spout through the weight-loss metering scale; Circular cross section glass fibre with 30% and 30% talcum powder join the forcing machine from twin screw extruder side spout respectively through the weight-loss metering scale;
(4) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition;
Said per-cent is the per-cent that is equivalent to the liquid-crystalline polymer composition quality.
Embodiment 2
A kind of preparation method of liquid-crystalline polymer composition may further comprise the steps:
(1) with liquid crystalline polymers Ueno LCP A2500 (constituting 340 ℃ of melt temperatures by PHBA/HNA/BP/TA) at 170 ℃ of dry 4-6h, make its moisture mass percent below 0.1%;
(2) silicone powder, 2% tetrafluoroethylene and the multipolymer (ETFE) of ethene of getting liquid crystalline polymers that 37% step (1) obtains and 1% places the high mixer blend, obtains the premix system;
(3) the premix system that step (2) is obtained joins the forcing machine from twin screw extruder master spout through the weight-loss metering scale; Oval cross section glass fibre with 30% and 30% glass flake join the forcing machine from twin screw extruder side spout respectively through the weight-loss metering scale;
(4) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition;
Said per-cent is the per-cent that is equivalent to the liquid-crystalline polymer composition quality.
Embodiment 3
A kind of preparation method of liquid-crystalline polymer composition may further comprise the steps:
(1) with liquid crystalline polymers Ueno LCP A2500 (constituting 340 ℃ of melt temperatures by PHBA/HNA/BP/TA) at 170 ℃ of dry 4-6h, make its moisture mass percent below 0.1%;
(2) get liquid crystalline polymers and 1% silicone powder, 2% tetrafluoroethylene and the hexafluoropropylene copolymer (FEP) that 52% step (1) obtains and place the high mixer blend, obtain the premix system;
(3) the premix system that step (2) is obtained joins the forcing machine from twin screw extruder master spout through the weight-loss metering scale; Rectangular cross section glass fibre with 15% and 30% mica join the forcing machine from twin screw extruder side spout respectively through the weight-loss metering scale;
(4) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition;
Said per-cent is the per-cent that is equivalent to the liquid-crystalline polymer composition quality.
Embodiment 4
A kind of preparation method of liquid-crystalline polymer composition may further comprise the steps:
(1) with liquid crystalline polymers Ueno LCP A2500 (constituting 340 ℃ of melt temperatures by PHBA/HNA/BP/TA) at 170 ℃ of dry 4-6h, make its moisture mass percent below 0.1%;
(2) silicone powder, 2% tetrafluoroethylene and the multipolymer (PFA) of perfluoroalkyl vinyl ether of getting liquid crystalline polymers that 57% step (1) obtains and 1% places the high mixer blend, obtains the premix system;
(3) the premix system that step (2) is obtained joins the forcing machine from twin screw extruder master spout through the weight-loss metering scale; Circular cross section glass fibre with 30% and 10% glass microballon join the forcing machine from twin screw extruder side spout respectively through the weight-loss metering scale;
(4) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition;
Said per-cent is the per-cent that is equivalent to the liquid-crystalline polymer composition quality.
Comparative Examples 1
A kind of preparation method of liquid-crystalline polymer composition may further comprise the steps:
(1) with liquid crystalline polymers Ueno LCP A2500 (constituting 340 ℃ of melt temperatures by PHBA/HNA/BP/TA) at 170 ℃ of dry 4-6h, make its moisture mass percent below 0.1%;
(2) getting the liquid crystalline polymers that 55% step (1) obtains joins the forcing machine from twin screw extruder master spout through the weight-loss metering scale; Circular cross section glass fibre with 15% and 30% talcum powder join the forcing machine from twin screw extruder side spout respectively through the weight-loss metering scale;
(3) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition;
Said per-cent is the per-cent that is equivalent to the liquid-crystalline polymer composition quality.
Comparative Examples 2
A kind of preparation method of liquid-crystalline polymer composition may further comprise the steps:
(1) with liquid crystalline polymers Ueno LCP A2500 (constituting 340 ℃ of melt temperatures by PHBA/HNA/BP/TA) at 170 ℃ of dry 4-6h, make its moisture mass percent below 0.1%;
(2) get liquid crystalline polymers that 58% step (1) obtains and 2% silicone powder and place the high mixer blend, obtain the premix system;
(3) the premix system that step (2) is obtained joins the forcing machine from twin screw extruder master spout through the weight-loss metering scale; Circular cross section glass fibre with 30% and 10% talcum powder join the forcing machine from twin screw extruder side spout respectively through the weight-loss metering scale;
(4) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition;
Said per-cent is the per-cent that is equivalent to the liquid-crystalline polymer composition quality.
Comparative Examples 3
A kind of preparation method of liquid-crystalline polymer composition may further comprise the steps:
(1) with liquid crystalline polymers Ueno LCP A2500 (constituting 340 ℃ of melt temperatures by PHBA/HNA/BP/TA) at 170 ℃ of dry 4-6h, make its moisture mass percent below 0.1%;
(2) get the tetrafluoroethylene of liquid crystalline polymers that 58% step (1) obtains and 2% and the multipolymer (PFA) of perfluoroalkyl vinyl ether and place the high mixer blend, obtain the premix system;
(3) the premix system that step (2) is obtained joins the forcing machine from twin screw extruder master spout through the weight-loss metering scale; Circular cross section glass fibre with 30% and 10% talcum powder join the forcing machine from twin screw extruder side spout respectively through the weight-loss metering scale;
(4) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition;
Said per-cent is the per-cent that is equivalent to the liquid-crystalline polymer composition quality.
Liquid-crystalline polymer composition to embodiment and Comparative Examples obtain is tested, and testing method is following:
Flowing property is estimated: with liquid-crystalline polymer composition granulation material to be tested 160 ℃ of dryings after 4 hours; The injection moulding machine of mould that moulding spirrillum sample is equipped with in use with the die temperature of 350 ℃ barrel temperature and 120 ℃ with the pellet moulding; Obtain wide 5mm, thick 1.4mm spirrillum sample; Read sample length and observe the liquid-crystalline polymer composition flowability, sample as shown in Figure 1.
Mechanics Performance Testing: mechanical property is carried out according to the ISO testing standard, stretches and crooked test Instron electronic universal tester Impact Test Zwick radial-boom impact tester.
Weld mark strength: adopt the stretching weld mark strength to characterize, similar ISO 527 (tensile strength) testing method just guarantees to advance glue to guarantee producing a weld mark at the batten middle part from the two ends of batten when die design.
Each item The performance test results of the liquid-crystalline polymer composition that above embodiment and Comparative Examples are provided is seen table 1.
Each embodiment of table 1 and Comparative Examples liquid-crystalline polymer composition The performance test results
Can find out from last table: the toughness and the weld mark strength of embodiment 1-4 liquid-crystalline polymer composition are better than Comparative Examples.The present invention can not only improve the toughness of gained liquid-crystalline polymer composition, and can improve the weld mark strength of resulting product to a certain extent through selecting suitable toughner combination; It is all good not as the two combined effect to add silicone powder or fluorochemicals separately.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. liquid-crystalline polymer composition is characterized in that: be that composition by following mass percent prepares:
Liquid crystalline polymers: 30-60%
Inorganic strengthening agent: 15-35%
Filler: 5-35%
Toughness reinforcing component: 2-5%;
Described toughness reinforcing component is made up of silicone powder and fluorochemicals;
Described fluorochemicals is a kind of in multipolymer or the tetrafluoroethylene and the hexafluoropropylene copolymer of tetrafluoroethylene and ethylene copolymer, tetrafluoroethylene and perfluoroalkyl vinyl ether.
2. liquid-crystalline polymer composition according to claim 1 is characterized in that: be that composition by following mass percent prepares:
Liquid crystalline polymers: 37-57%
Inorganic strengthening agent: 15-30%
Filler: 10-30%
Toughness reinforcing component: 2-3%.
3. liquid-crystalline polymer composition according to claim 1 and 2 is characterized in that:
Described liquid crystalline polymers is made up of by following molar content four kinds of repeated structural units of formula I-IV:
Formula (I): 40-60%
Formula (II): 10-20%
Formula (III): 10-20%
Formula (IV): 20-40%;
The melt temperature of said liquid crystalline polymers is 310-350 ℃.
4. liquid-crystalline polymer composition according to claim 1 and 2 is characterized in that: described inorganic strengthening agent is a kind of in circular cross section glass fibre, oval cross section glass fibre, rectangular cross section glass fibre, sapphire whisker, carbon fiber, potassium titanate fiber, boric acid fibre or the wollastonite fibre.
5. liquid-crystalline polymer composition according to claim 1 and 2 is characterized in that: described inorganic strengthening agent is a kind of in circular cross section glass fibre, oval cross section glass fibre or the rectangular cross section glass fibre.
6. liquid-crystalline polymer composition according to claim 1 and 2 is characterized in that: described filler is a kind of in glass flake, mica, glass microballon, talcum powder, clay, wollastonite, graphite, lime carbonate, barium sulfate or the titanium dioxide.
7. the preparation method of claim 1 or 2 described liquid-crystalline polymer compositions is characterized in that may further comprise the steps:
(1) liquid crystalline polymers is dry;
(2) liquid crystalline polymers that step (1) is obtained and toughness reinforcing component blend obtain the premix system;
(3) premix system, inorganic strengthening agent and the filler that step (2) is obtained joins in the forcing machine;
(4) extrude, tie rod, cooling, granulation, obtain liquid-crystalline polymer composition.
8. the preparation method of liquid-crystalline polymer composition according to claim 7 is characterized in that:
Step (1) is described dry with liquid crystalline polymers, is at 170 ℃ of dry 4-6h, makes its moisture mass percent below 0.1%;
The described blend of step (2) is in high mixer, to carry out.
9. the preparation method of liquid-crystalline polymer composition according to claim 7 is characterized in that:
The described premix system that step (2) is obtained of step (3) joins in the forcing machine, is to join the forcing machine from twin screw extruder master spout through the weight-loss metering scale;
Step (3) is described to join inorganic strengthening agent and filler in the forcing machine, is respectively inorganic strengthening agent and filler to be joined the forcing machine from twin screw extruder side spout through the weight-loss metering scale.
10. the application of claim 1 or 2 described liquid-crystalline polymer compositions is characterized in that: be used to make junctor, electrical condenser, switch, circuit wafer, pick up camera module or rly..
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| CN103194080A (en) * | 2013-04-27 | 2013-07-10 | 苏州正豪塑胶电子有限公司 | Corrosion-resistant plug connector |
| CN103819927A (en) * | 2014-03-12 | 2014-05-28 | 华东理工大学 | Light-colored antistatic liquid crystal polymer composite material and preparation method thereof |
| WO2017114162A1 (en) * | 2015-12-30 | 2017-07-06 | 金发科技股份有限公司 | Liquid crystal polyester composition |
| CN108148433A (en) * | 2017-12-26 | 2018-06-12 | 上海普利特化工新材料有限公司 | A kind of low warpage high temperature resistant conduction liquid crystal polyester composite and preparation method thereof |
| WO2019109595A1 (en) * | 2017-12-05 | 2019-06-13 | Ticona Llc | Liquid crystalline polymer composition |
| CN110982297A (en) * | 2019-12-17 | 2020-04-10 | 东莞市德发塑胶科技有限公司 | 5G low dielectric strength LCP composite material and preparation method thereof |
| US20220380675A1 (en) * | 2019-12-11 | 2022-12-01 | Otsuka Chemical Co., Ltd. | Liquid crystal polymer composition, liquid crystal polymer molded body, and camera module |
| CN115785692A (en) * | 2022-12-08 | 2023-03-14 | 上海斯必特橡塑有限公司 | Modified LCP material for high-performance electronic and electrical appliances and preparation method thereof |
| US11722759B2 (en) | 2019-03-20 | 2023-08-08 | Ticona Llc | Actuator assembly for a camera module |
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| US11722759B2 (en) | 2019-03-20 | 2023-08-08 | Ticona Llc | Actuator assembly for a camera module |
| US20220380675A1 (en) * | 2019-12-11 | 2022-12-01 | Otsuka Chemical Co., Ltd. | Liquid crystal polymer composition, liquid crystal polymer molded body, and camera module |
| CN110982297B (en) * | 2019-12-17 | 2021-07-09 | 东莞市德发塑胶科技有限公司 | 5G low dielectric strength LCP composite material and preparation method thereof |
| CN110982297A (en) * | 2019-12-17 | 2020-04-10 | 东莞市德发塑胶科技有限公司 | 5G low dielectric strength LCP composite material and preparation method thereof |
| CN115785692A (en) * | 2022-12-08 | 2023-03-14 | 上海斯必特橡塑有限公司 | Modified LCP material for high-performance electronic and electrical appliances and preparation method thereof |
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