CN102532886A - Poly phthalimide amide composite material and preparation method thereof - Google Patents

Poly phthalimide amide composite material and preparation method thereof Download PDF

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CN102532886A
CN102532886A CN2011104269672A CN201110426967A CN102532886A CN 102532886 A CN102532886 A CN 102532886A CN 2011104269672 A CN2011104269672 A CN 2011104269672A CN 201110426967 A CN201110426967 A CN 201110426967A CN 102532886 A CN102532886 A CN 102532886A
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composite material
polyphthalamide
mixture
polyphthalamide composite
tlcp
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CN102532886B (en
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徐东
徐永
谢建达
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Polymer Science Shenzhen New Materials Co Ltd
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Polymer Science Shenzhen New Materials Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/78Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/875Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92514Pressure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895Barrel or housing

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  • Mechanical Engineering (AREA)
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  • Thermal Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

The invention discloses a poly phthalimide amide composite material and a preparation method thereof. The poly phthalimide amide composite material comprises components of the following weight portions: 45-68 portions of poly phthalimide amide, 1-20 portion(s) of heat-set liquid crystalline polymer, 1-25 portion(s) of zirconia and 10-30 portions of titanium dioxide. The components of appropriate contents interact during fusion and extrusion, so the poly phthalimide amide composite material has high whiteness, thermal stability and mechanical properties. In the preparation method of the poly phthalimide amide composite material, all the components are molten and extruded via side feeding, the preparation can be implemented on a conventional fusion extruder, no special equipment is needed, the operation and the process are simple, the efficiency is high, and the cost is low. Therefore, the preparation method is suitable for industrial production.

Description

A kind of polyphthalamide composite material and preparation method thereof
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of polyphthalamide composite material and preparation method thereof.
Background technology
Polyphthalamide (PPA) is to be the semi-aromatic nylon of raw material with the phthalic acid, is a kind of hemicrystalline thermoplasticity functional type material.The PPA matrix material has the excellent comprehensive rerum natura, outstanding resistance to elevated temperatures, and high rigidity, HS, splendid dimensional precision and stability and low warpage properties, favorable chemical resistance are all having good performance aspect heat, electricity, physics and the chemical resistant properties.This makes the PPA matrix material all have application prospects in fields such as electric, mechanical engineerings.
High whiteness PPA material is used more and more widely in fields such as led supports.But find that in actual production existing P PA material thermostability, bad mechanical property have limited its application.Therefore, exploitation not only has high whiteness but also have stronger thermostability, mechanicalness PPA material seems particularly urgent and important, is the technical barrier of being badly in need of solution at present.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency of prior art, provide a kind of whiteness high, the polyphthalamide composite material that thermostability and mechanical property are strong.
It is simple that another object of the present invention provides a kind of technology, easy to operate, the polyphthalamide composite material preparation method of high efficiency.
In order to realize the foregoing invention purpose, technical scheme of the present invention is following:
A kind of polyphthalamide composite material comprises the recipe ingredient of following parts by weight:
And a kind of polyphthalamide composite material preparation method may further comprise the steps:
Prescription according to above-mentioned polyphthalamide composite material takes by weighing each component;
The said polyphthalamide that takes by weighing, TLCP are mixed, form first mixture;
The said zirconium white that takes by weighing, titanium oxide are mixed, form second mixture;
Said first mixture is added in the opening for feed of forcing machine, melt extrude in the side spout with said second mixture adding forcing machine simultaneously, granulation obtains said polyphthalamide composite material.
Above-mentioned polyphthalamide composite material interacts in melt extruding process through each component of proper content scope, makes polyphthalamide composite material whiteness of the present invention high, and thermostability and mechanical property are strong.Wherein, zirconium white and titanium oxide are composite, make this polyphthalamide composite material have high whiteness, have improved thermostability, the mechanical property of matrix material; TLCP has characteristic than polyphthalamide: the littler and secular light decay of water absorbability is littler; And TLCP in extrusion with the polyphthalamide effect; And in the polyphthalamide matrix, can form microfibrillar structure; Improve the intensity and the thermostability of this polyphthalamide composite material, simultaneously, can effectively reduce the melt viscosity that this polyphthalamide composite material adds man-hour; Improve melt flow rate(MFR); Reduce processing temperature, shearing resistance, and then improve the polyphthalamide composite material processing characteristics, and avoid polyphthalamide composite material that oxidation, degraded and consequent degradation take place in the course of processing effectively.
The preparation method of above-mentioned polyphthalamide composite material adopts the mode of side charging that each component melts is extruded; Make each component under the high speed shear effect; Reduced viscosity; Strengthened the dispersiveness of each component, thereby made that this polyphthalamide composite material whiteness is even, whiteness is high, thermostability and mechanical property be strong.And this polyphthalamide composite material can implement in melt extruding on the machine of routine, needn't be by specific installation, and operating process is simple and easy to do, and technology is simple, high efficiency, cost is low, is suitable for suitability for industrialized production.
Description of drawings
To combine accompanying drawing and embodiment that the present invention is described further below, in the accompanying drawing:
Fig. 1 is polyphthalamide composite material preparing method's of the present invention process flow diagram.
Embodiment
Clearer for technical problem, technical scheme and beneficial effect that the present invention will be solved, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
The embodiment of the invention provides a kind of whiteness height, thermostability, polyphthalamide composite material that mechanical property is strong.This polyphthalamide composite material comprises the recipe ingredient of following parts by weight:
Figure BDA0000122054120000031
Particularly, above-mentioned polyphthalamide does not have particular requirement, can commercially obtain.
Above-mentioned TLCP is the backbone chain type TLCP.Wherein, this backbone chain type TLCP is preferably aromatic copolyester, and its fusion range is 260~350 ℃.This preferred TLCP has the rheological characteristics of better strong shear shinning; In extrusion with the composite synergy of polyphthalamide; And in the polyphthalamide matrix, can form microfibrillar structure, improved the intensity of this polyphthalamide composite material.
Above-mentioned zirconium white is preferably at least a in the zirconium white of monocline, four directions, cube crystalline phase form, the zirconium white of the tetragonal phase morphology of more preferably handling through the 3moL% stabilized with yttrium oxide, and this stabilizing treatment adopts the existing method in this area to handle and gets final product.Above-mentioned titanium oxide is anatase titanium dioxide and/or rutile titanium dioxide, more preferably rutile titanium dioxide.This preferred zirconium white and titanium dioxide performance, stable physical property, can be better and other components in melt extruding process, act synergistically, give polyphthalamide composite material high whiteness, high thermal stability, mechanical property.
Like this, above-mentioned polyphthalamide composite material interacts in melt extruding process through each component of proper content scope, makes polyphthalamide composite material whiteness of the present invention high, and thermostability and mechanical property are strong.The whiteness of this polyphthalamide composite material, thermostability and the related mechanical properties experimental data in the table 1 that vide infra.Wherein, zirconium white and titanium oxide are composite, make this polyphthalamide composite material have high whiteness, have improved thermostability, the mechanical property of matrix material; TLCP has the littler characteristic of the littler and long-term light decay of water absorbability than polyphthalamide; In extrusion,, and in the polyphthalamide matrix, can form microfibrillar structure, improve the intensity of this polyphthalamide composite material with the polyphthalamide effect; Simultaneously; Can effectively reduce this polyphthalamide composite material and add the melt viscosity in man-hour, improve melt flow rate(MFR), reduce processing temperature, shearing resistance; And then improve the polyphthalamide composite material processing characteristics, and avoid polyphthalamide composite material that oxidation, degraded and consequent degradation take place in the course of processing effectively.
The embodiment of the invention also provides above-mentioned polyphthalamide composite, preparation method, and its technical process is as shown in Figure 1.This method comprises the steps:
S01. take by weighing recipe ingredient: the prescription according to above-mentioned polyphthalamide composite material takes by weighing each component;
S02. prepare first mixture: the polyphthalamide that takes by weighing, TLCP are mixed, form first mixture;
S03. prepare second mixture: the zirconium white that takes by weighing, titanium oxide are mixed, form second mixture;
S04. melt extrude: this first mixture is added in the opening for feed of forcing machine, melt extrude in the side spout with second mixture adding forcing machine simultaneously, granulation obtains said polyphthalamide composite material.
Particularly, among the above-mentioned steps S01, each component preferred content in the prescription of polyphthalamide composite material and the prescription and kind in order to practice thrift length, repeat no more at this as stated.
Among the above-mentioned steps S02, the mixing of polyphthalamide, TLCP can be adopted like mixing tank and mix, and can certainly adopt the miscellaneous equipment of this area to mix.Wherein, the mixing of this two component preferably mixed under the condition of middling speed 10~40 minutes, more preferably mixed 20 minutes.
Among the above-mentioned steps S03, the mixing of zirconium white, titanium oxide also can be adopted like mixing tank and mix, and can certainly adopt the miscellaneous equipment of this area to mix.Wherein, the mixing of this two component preferably mixed under the condition of middling speed 25~35 minutes.
Among the above-mentioned steps S04, adopt the mode of side loading, make win mixture and this second mixture in melt extruding process, realize uniform mixing.Wherein, This is extruded preferred employing twin screw extruder and extrudes; First mixture and the temperature of second mixture in said twin screw extruder are preferably respectively: 260~300 ℃ of district's temperature, 270~310 ℃ of two district's temperature, 270~310 ℃ of three district's temperature; 260~300 ℃ of four district's temperature, 260~300 ℃ of five district's temperature.Other first mixture and second mixture time of delivery in the screw rod of twin screw extruder is preferably 2~5 minutes, and pressure is preferably 12~20MPa.This preferred expressing technique can better make each component mix, and has an effect each other, gives the high whiteness of polyphthalamide composite material of the present invention, stronger thermostability and mechanical property.
The preparation method of above-mentioned polyphthalamide composite material adopts and divides into groups earlier to join mutually; The mode of side charging is extruded each component melts again; Make each component under the high speed shear effect, reduced viscosity, strengthened the dispersiveness of each component; And have an effect mutually, thereby make that this polyphthalamide composite material whiteness is even, whiteness is high, thermostability and mechanical property be strong.And this polyphthalamide composite material can implement in melt extruding on the machine of routine, needn't be by specific installation, and operating process is simple and easy to do, and technology is simple, high efficiency, cost is low, is suitable for suitability for industrialized production.
Existing prescription and preparation method with concrete polyphthalamide composite material is example, and the present invention is further elaborated.
Embodiment 1
The recipe ingredient of polyphthalamide composite material parts by weight is following:
68 parts of polyphthalamides, 1 part of TLCP, 1 part of zirconium white, 30 parts of titanium oxide.Wherein, This polyphthalamide is the PPA A-1000 of Su Wei company; TLCP is the Zenite type TLCP that U.S. Dupont company produces; Zirconium white is the cubic polycrystal zirconia (3Y-TZP) of 3mol% stabilized with yttrium oxide, and titanium oxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is following:
S11: the prescription according to above-mentioned polyphthalamide composite material takes by weighing each component;
S12: the polyphthalamide that takes by weighing, TLCP component are placed mixing machine, and under the condition of middling speed, mixed 10 minutes, obtain first mixture;
S13: the zirconium white that takes by weighing, titanium oxide component are placed mixing machine, and under the condition of middling speed, mixed 30 minutes, obtain second mixture;
S14: place the opening for feed of twin screw extruder to feed first mixture; Adopt weight-loss metering to claim second mixture is fed from the side material mouth of twin screw extruder simultaneously; And through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, the twin screw extruder processing condition are: 280 ℃ in a district, and 290 ℃ in two districts, 300 ℃ in three districts, 300 ℃ in four districts, 290 ℃ in five districts, this mixture time of delivery in the screw rod of twin screw extruder is 3min, pressure is 16MPa.
Embodiment 2
The recipe ingredient of polyphthalamide composite material parts by weight is following:
65 parts of polyphthalamides, 5 parts of TLCPs, 5 parts of zirconium whites, 25 parts of titanium oxide.Wherein, Polyphthalamide is the A-4000 of Su Wei company; TLCP is the Zenite type TLCP that U.S. Dupont company produces, and zirconium white is the cubic polycrystal zirconia (3Y-TZP) of 3mol% stabilized with yttrium oxide, and titanium oxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is following:
S21: the prescription according to above-mentioned polyphthalamide composite material takes by weighing each component;
S22: the polyphthalamide that takes by weighing, TLCP component are placed mixing machine, and under the condition of middling speed, mixed 15 minutes, obtain first mixture;
S23: the zirconium white that takes by weighing, titanium oxide component are placed mixing machine, and under the condition of middling speed, mixed 35 minutes, obtain second mixture;
S24: place the opening for feed of twin screw extruder to feed first mixture; Adopt weight-loss metering to claim second mixture is fed from the side material mouth of twin screw extruder simultaneously; And through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, the twin screw extruder processing condition are: 280 ℃ in a district, and 290 ℃ in two districts, 300 ℃ in three districts, 300 ℃ in four districts, 290 ℃ in five districts, this mixture time of delivery in the screw rod of twin screw extruder is 2min, pressure is 20MPa.
Embodiment 3
The recipe ingredient of polyphthalamide composite material parts by weight is following:
60 parts of polyphthalamides, 10 parts of TLCPs, 10 parts of zirconium whites, 20 parts of titanium oxide.Wherein, Polyphthalamide is the PPA A-1000 of Su Wei company; The Vectra type TLCP that TLCP is produced for Ticona company, zirconium white is the cubic polycrystal zirconia (3Y-TZP) of 3mol% stabilized with yttrium oxide, titanium oxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is following:
S31: the prescription according to above-mentioned polyphthalamide composite material takes by weighing each component;
S32: the polyphthalamide that takes by weighing, TLCP component are placed mixing machine, and under the condition of middling speed, mixed 20 minutes, obtain first mixture;
S33: the zirconium white that takes by weighing, titanium oxide component are placed mixing machine, and under the condition of middling speed, mixed 35 minutes, obtain second mixture;
S34: place the opening for feed of twin screw extruder to feed first mixture; Adopt weight-loss metering to claim second mixture is fed from the side material mouth of twin screw extruder simultaneously; And through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, the twin screw extruder processing condition are: 275 ℃ in a district, and 285 ℃ in two districts, 300 ℃ in three districts, 290 ℃ in four districts, 290 ℃ in five districts, this mixture time of delivery in the screw rod of twin screw extruder is 3min, pressure is 15MPa.
Embodiment 4
The recipe ingredient of polyphthalamide composite material parts by weight is following:
55 parts of polyphthalamides, 15 parts of TLCPs, 15 parts of zirconium whites, 25 parts of titanium oxide.Wherein, Polyphthalamide is the A-4000 of Su Wei company; The Vectra type TLCP that TLCP is produced for Ticona company, zirconium white is the cubic polycrystal zirconia (3Y-TZP) of 3mol% stabilized with yttrium oxide, titanium oxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is following:
S41: the prescription according to above-mentioned polyphthalamide composite material takes by weighing each component;
S42: the polyphthalamide that takes by weighing, TLCP component are placed mixing machine, and under the condition of middling speed, mixed 40 minutes, obtain first mixture;
S43: the zirconium white that takes by weighing, titanium oxide component are placed mixing machine, and under the condition of middling speed, mixed 25 minutes, obtain second mixture;
S44: place the opening for feed of twin screw extruder to feed first mixture; Adopt weight-loss metering to claim second mixture is fed from the side material mouth of twin screw extruder simultaneously; And through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, the twin screw extruder processing condition are: 285 ℃ in a district, and 295 ℃ in two districts, 300 ℃ in three districts, 290 ℃ in four districts, 280 ℃ in five districts, this mixture time of delivery in the screw rod of twin screw extruder is 3min, pressure is 14MPa.
Embodiment 5
The recipe ingredient of polyphthalamide composite material parts by weight is following:
45 parts of polyphthalamides, 20 parts of TLCPs, 25 parts of zirconium whites, 10 parts of titanium oxide.Wherein, Polyphthalamide is the PPA A-1000 of Su Wei company; TLCP is the Zenite type TLCP that U.S. Dupont company produces, and zirconium white is the cubic polycrystal zirconia (3Y-TZP) of 3mol% stabilized with yttrium oxide, and titanium oxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is following:
S51: the prescription according to above-mentioned polyphthalamide composite material takes by weighing each component;
S52: the polyphthalamide that takes by weighing, TLCP component are placed mixing machine, and under the condition of middling speed, mixed 20 minutes, obtain first mixture;
S53: the zirconium white that takes by weighing, titanium oxide component are placed mixing machine, and under the condition of middling speed, mixed 28 minutes, obtain second mixture;
S54: place the opening for feed of twin screw extruder to feed first mixture; Adopt weight-loss metering to claim second mixture is fed from the side material mouth of twin screw extruder simultaneously; And through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, the twin screw extruder processing condition are: 270 ℃ in a district, and 285 ℃ in two districts, 300 ℃ in three districts, 300 ℃ in four districts, 285 ℃ in five districts, this mixture time of delivery in the screw rod of twin screw extruder is 5min, pressure is 12MPa.
Comparison example
The recipe ingredient of polyphthalamide composite material parts by weight is following:
70 parts of polyphthalamides, 30 parts of titanium oxide.Wherein, this polyphthalamide is the PPA A-1000 of Su Wei company, and titanium oxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is following:
S11: the prescription according to above-mentioned polyphthalamide composite material takes by weighing each component;
S12: place the opening for feed of twin screw extruder to feed polyphthalamide; Adopt weight-loss metering to claim titanium oxide is fed from the side material mouth of twin screw extruder simultaneously; And through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, the twin screw extruder processing condition are: 280 ℃ in a district, and 290 ℃ in two districts, 300 ℃ in three districts, 300 ℃ in four districts, 290 ℃ in five districts, this mixture time of delivery in the screw rod of twin screw extruder is 3min, pressure is 16MPa.
Performance evaluation criterion and performance index:
The foregoing description 1~5 and the prepared polyphthalamide composite material of comparison example are carried out the related mechanical properties evaluation by following detection method and standard:
The polyphthalamide composite material particle that the foregoing description 1~5 and comparison example is prepared in 140 ℃ convection oven dry 4 hours respectively; With the injection moulding sample preparation on the 80T injection moulding machine of exsiccant particle, keep the mould temperature in the sample making course between 70~100 ℃ again.
Stretching strength determination: test by GB/T 1040 standards; Specimen types is the I type, batten size (mm): 170 (length) * (20 ± 0.2) (end width) * (4 ± 0.2) (thickness), draw speed is 50mm/min.
Flexural strength and modulus in flexure are measured: test by GB/T 9341 standards; Specimen types is specimen size (mm): (80 ± 2) * (10 ± 0.2) * (4 ± 0.2), rate of bending are 20mm/min.
Heat-drawn wire is measured: test by GB/T 1634.2 standards, load is 1.80MPa, and span is 100mm.
Flame retardant properties is measured: detect specimen size (mm) according to UL 94 standards: 130 (length) * (20 ± 0.2) (end width) * (1.6 ± 0.2) (thickness).
The prepared polyphthalamide composite material correlated performance test result of the foregoing description 1~5 and comparison example is respectively like table 1:
The polyphthalamide composite material performance test of table 1: embodiment 1~5 and comparison example preparation
Figure BDA0000122054120000101
Figure BDA0000122054120000111
Can find out from last table 1 data, compare with comparison example, the polyphthalamide composite material of embodiment 1~5 have that whiteness is even, whiteness is high and have better thermostability and mechanical property strong.Wherein, along with the increase of content of titanium dioxide and PPA, polyphthalamide composite material whiteness, viscosity also increase accordingly.And along with the increase of zirconium white and TLCP content, the related mechanical properties and the thermal stability of polyphthalamide composite material strengthen thereupon.This is because TLCP has the littler characteristic of the littler and secular light decay of water absorbability than polyphthalamide; And TLCP in extrusion with the polyphthalamide effect; And in the polyphthalamide matrix, can form microfibrillar structure; Improve the intensity and the thermostability of this polyphthalamide composite material, simultaneously, can effectively reduce the melt viscosity that this polyphthalamide composite material adds man-hour; Improve melt flow rate(MFR); Reduce processing temperature, shearing resistance, and then improve the polyphthalamide composite material processing characteristics, and avoid polyphthalamide composite material that oxidation, degraded and consequent degradation take place in the course of processing effectively.This shows that titanium oxide and zirconium white and TLCP are composite, make this polyphthalamide composite material have high whiteness, improved thermostability, the mechanical property of matrix material.Therefore; Prescription through the foregoing description polyphthalamide composite material with and preparation method thereof; Make the embodiment of the invention prepare not only to have high whiteness but have good thermal stability can and the polyphthalamide composite material of mechanical property, overcome existing PPA material and only had the deficiency of good whiteness, thermostability and bad mechanical property.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.

Claims (9)

1. polyphthalamide composite material comprises the recipe ingredient of following parts by weight:
Figure FDA0000122054110000011
2. polyphthalamide composite material according to claim 1 is characterized in that, said zirconium white is at least a in the zirconium white of monocline, four directions, cube crystalline phase form.
3. polyphthalamide composite material according to claim 1 is characterized in that, said zirconium white is the zirconium white through the tetragonal phase morphology of 3moL% stabilized with yttrium oxide processing.
4. according to claim 1 or 2 or 3 described polyphthalamide composite materials, it is characterized in that said titanium oxide is anatase titanium dioxide and/or rutile titanium dioxide.
5. according to claim 1 or 2 or 3 described polyphthalamide composite materials, it is characterized in that said titanium oxide is rutile titanium dioxide.
6. according to claim 1 or 2 or 3 described polyphthalamide composite materials, it is characterized in that said TLCP is the backbone chain type TLCP.
7. polyphthalamide composite material according to claim 6 is characterized in that, said backbone chain type TLCP is an aromatic copolyester, and its fusion range is 260~350 ℃.
8. polyphthalamide composite material preparation method may further comprise the steps:
Prescription according to the arbitrary said polyphthalamide composite material of claim 1~7 takes by weighing each component;
The said polyphthalamide that takes by weighing, TLCP are mixed, form first mixture;
The said zirconium white that takes by weighing, titanium oxide are mixed, form second mixture;
Said first mixture is added in the opening for feed of forcing machine, melt extrude in the side spout with said second mixture adding forcing machine simultaneously, granulation obtains said polyphthalamide composite material.
9. polyphthalamide composite material preparation method according to claim 8; It is characterized in that said extruding is to adopt twin screw extruder to extrude, said first mixture and the temperature of second mixture in said twin screw extruder are respectively: 260~300 ℃ of district's temperature; 270~310 ℃ of two district's temperature; 270~310 ℃ of three district's temperature, 260~300 ℃ of four district's temperature, 260~300 ℃ of five district's temperature; Said first mixture and second mixture time of delivery in the screw rod of twin screw extruder is 2~5 minutes, and pressure is 12~20MPa.
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CN103509339A (en) * 2013-09-24 2014-01-15 惠州市昌亿新材料有限公司 High-performance and high-shading PPA polymer, and preparation method and application thereof
CN108219448A (en) * 2018-01-02 2018-06-29 杭州本松新材料技术股份有限公司 A kind of thermoplastic resin composition

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CN1919788A (en) * 2006-09-20 2007-02-28 景德镇市新纪元精密陶瓷有限公司 Environment-friendly type nanometer ceramic knife and manufacture method thereof
CN101831171A (en) * 2010-04-21 2010-09-15 深圳市科聚新材料有限公司 Flame retardant reinforced polyphthalamide composite material and preparation method thereof
CN102067719A (en) * 2008-04-22 2011-05-18 达泰克涂料股份公司 Thick film high temperature thermoplastic insulated heating element

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CN1919788A (en) * 2006-09-20 2007-02-28 景德镇市新纪元精密陶瓷有限公司 Environment-friendly type nanometer ceramic knife and manufacture method thereof
CN102067719A (en) * 2008-04-22 2011-05-18 达泰克涂料股份公司 Thick film high temperature thermoplastic insulated heating element
CN101831171A (en) * 2010-04-21 2010-09-15 深圳市科聚新材料有限公司 Flame retardant reinforced polyphthalamide composite material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103509339A (en) * 2013-09-24 2014-01-15 惠州市昌亿新材料有限公司 High-performance and high-shading PPA polymer, and preparation method and application thereof
CN103509339B (en) * 2013-09-24 2017-01-04 惠州市集和光电科技有限公司 A kind of high-performance height shading PPA polymer and its preparation method and application
CN108219448A (en) * 2018-01-02 2018-06-29 杭州本松新材料技术股份有限公司 A kind of thermoplastic resin composition

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