CN102532886B - 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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CN102532886B
CN102532886B CN201110426967.2A CN201110426967A CN102532886B CN 102532886 B CN102532886 B CN 102532886B CN 201110426967 A CN201110426967 A CN 201110426967A CN 102532886 B CN102532886 B CN 102532886B
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composite material
polyphthalamide
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titanium dioxide
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CN102532886A (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

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 take the semi-aromatic nylon that phthalic acid is raw material, is a kind of hemicrystalline thermoplasticity functional type material.PPA matrix material has excellent comprehensive physical property, outstanding resistance to elevated temperatures, and high rigidity, high strength, splendid dimensional precision and stability and low warpage properties, good chemical resistant properties, having good performance aspect heat, electricity, physics and chemical resistant properties.This makes PPA matrix material all gather around and have wide practical use in fields such as electric, mechanical engineerings.
High whiteness PPA material is more and more extensive in field application such as LED supports.But in actual production, find, existing PPA material thermostability, bad mechanical property, limited its application.Therefore, exploitation not only has high whiteness but also have stronger thermostability, mechanicalness PPA material seems particularly urgent and important, is to be badly in need of at present the technical barrier of solution.
Summary of the invention
The object 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 is to provide a kind of technique, easy to operate, the polyphthalamide composite material preparation method of high efficiency.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
, comprise the recipe ingredient of following parts by weight:
Figure BDA0000122054120000021
And a kind of polyphthalamide composite material preparation method, comprises the following steps:
According to the formula of above-mentioned polyphthalamide composite material, take each component;
The described polyphthalamide taking, TLCP are mixed, form the first mixture;
The described zirconium white taking, titanium dioxide are mixed, form the second mixture;
Described the first mixture is added in the opening for feed of forcing machine, described the second mixture is added in the side spout of forcing machine simultaneously and melt extrude, granulation, obtains described polyphthalamide composite material.
Above-mentioned polyphthalamide composite material interacts in melt extruding process by 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 dioxide are composite, make this polyphthalamide composite material have high whiteness, have improved thermostability, the mechanical property of matrix material, TLCP has characteristic compared with polyphthalamide: the less and long-term light decay of water absorbability is less, and TLCP in extrusion with polyphthalamide effect, and can form microfibrillar structure in polyphthalamide matrix, intensity and the thermostability of this polyphthalamide composite material have been improved, 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 polyphthalamide composite material processing characteristics, and effectively avoid polyphthalamide composite material to be oxidized in the course of processing, degraded and consequent degradation.
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 high speed shear effect, reduced viscosity, strengthened the dispersiveness of each component, thus make that this polyphthalamide composite material whiteness is even, whiteness is high, thermostability and mechanical property strong.And this polyphthalamide composite material can implement on conventional melt extruder, needn't be by specific installation, operating process is simple and easy to do, and technique is simple, high efficiency, cost is low, is suitable for suitability for industrialized production.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is polyphthalamide composite material preparation method's of the present invention process flow diagram.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides that a kind of whiteness is high, 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 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 can form microfibrillar structure in polyphthalamide matrix, improved the intensity of this polyphthalamide composite material.
Above-mentioned zirconium white is preferably at least one in the zirconium white of monocline, four directions, cubic crystal phase morphology, the zirconium white of the tetragonal phase form of more preferably processing through 3moL% stabilized with yttrium oxide, and this stabilizing treatment adopts the existing method in this area to process.Above-mentioned titanium dioxide 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 by 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 table 1 that vide infra.Wherein, zirconium white and titanium dioxide are composite, make this polyphthalamide composite material have high whiteness, have improved thermostability, the mechanical property of matrix material, TLCP has the less characteristic of the less and long-term light decay of water absorbability compared with polyphthalamide, in extrusion with polyphthalamide effect, and can form microfibrillar structure in polyphthalamide matrix, improved the intensity 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 polyphthalamide composite material processing characteristics, and effectively avoid polyphthalamide composite material to be oxidized in the course of processing, degraded and consequent degradation.
The embodiment of the present invention also provides above-mentioned polyphthalamide composite, preparation method, and its technical process as shown in Figure 1.The method comprises the steps:
S01. take recipe ingredient: according to the formula of above-mentioned polyphthalamide composite material, take each component;
S02. prepare the first mixture: the polyphthalamide taking, TLCP are mixed, form the first mixture;
S03. prepare the second mixture: the zirconium white taking, titanium dioxide are mixed, form the second mixture;
S04. melt extrude: this first mixture is added in the opening for feed of forcing machine, the second mixture is added in the side spout of forcing machine simultaneously and melt extrude, granulation, obtains described polyphthalamide composite material.
Particularly, in above-mentioned steps S01, each component preferred content in the formula of polyphthalamide composite material and formula and kind as mentioned above, in order to save length, do not repeat them here.
In above-mentioned steps S02, the mixing of polyphthalamide, TLCP can adopt and mix as mixing tank, can certainly adopt the miscellaneous equipment of this area to mix.Wherein, the mixing of this two component preferably mixes 10~40 minutes under the condition of middling speed, more preferably mixes 20 minutes.
In above-mentioned steps S03, the mixing of zirconium white, titanium dioxide also can adopt and mix as mixing tank, can certainly adopt the miscellaneous equipment of this area to mix.Wherein, the mixing of this two component preferably mixes 25~35 minutes under the condition of middling speed.
In above-mentioned steps S04, adopt the mode of side loading, make the first mixture realize evenly and mixing in melt extruding process with this second mixture.Wherein, this is extruded preferred employing twin screw extruder and extrudes, the first mixture and the temperature of the second mixture in described twin screw extruder are preferably respectively: 260~300 ℃ of district's temperature, two 270~310 ℃ of district's temperature, three 270~310 ℃ of district's temperature, four 260~300 ℃ of district's temperature 260~300 ℃, five district's temperature.Other the first mixture and the 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 the interworking of first dividing into groups, the mode of side charging is extruded each component melts again, make each component under high speed shear effect, reduced viscosity, strengthened the dispersiveness of each component, and mutually, have an effect, thereby make that this polyphthalamide composite material whiteness is even, whiteness is high, thermostability and mechanical property strong.And this polyphthalamide composite material can implement on conventional melt extruder, needn't be by specific installation, operating process is simple and easy to do, and technique is simple, high efficiency, cost is low, is suitable for suitability for industrialized production.
Formula and the preparation method of concrete polyphthalamide composite material of now take is example, and the present invention is further elaborated.
Embodiment 1
The recipe ingredient of polyphthalamide composite material parts by weight is as follows:
68 parts of polyphthalamides, 1 part of TLCP, 1 part of zirconium white, 30 parts of titanium dioxide.Wherein, the PPA A-1000 of this polyphthalamide Wei Su prestige 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 dioxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is as follows:
S11: take each component according to the formula of above-mentioned polyphthalamide composite material;
S12: the polyphthalamide taking, TLCP component are placed in to mixing machine, and mix 10 minutes under the condition of middling speed, obtain the first mixture;
S13: the zirconium white taking, titanium dioxide component are placed in to mixing machine, and mix 30 minutes under the condition of middling speed, obtain the second mixture;
S14: the opening for feed that the first mixture is placed in to twin screw extruder feeds, adopt weight-loss metering to claim the second mixture to feed from the side material mouth of twin screw extruder simultaneously, and through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, twin screw extruder processing condition are: 290 ℃, 280 290 300 300 ℃, 5th district, ℃, 4th district, ℃, 3rd district, ℃, 2nd district, a district, and 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 as follows:
65 parts of polyphthalamides, 5 parts of TLCP, 5 parts of zirconium whites, 25 parts of titanium dioxide.Wherein, the A-4000 of polyphthalamide Wei Su prestige 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 dioxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is as follows:
S21: take each component according to the formula of above-mentioned polyphthalamide composite material;
S22: the polyphthalamide taking, TLCP component are placed in to mixing machine, and mix 15 minutes under the condition of middling speed, obtain the first mixture;
S23: the zirconium white taking, titanium dioxide component are placed in to mixing machine, and mix 35 minutes under the condition of middling speed, obtain the second mixture;
S24: the opening for feed that the first mixture is placed in to twin screw extruder feeds, adopt weight-loss metering to claim the second mixture to feed from the side material mouth of twin screw extruder simultaneously, and through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, twin screw extruder processing condition are: 290 ℃, 280 290 300 300 ℃, 5th district, ℃, 4th district, ℃, 3rd district, ℃, 2nd district, a district, and 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 as follows:
60 parts of polyphthalamides, 10 parts of TLCP, 10 parts of zirconium whites, 20 parts of titanium dioxide.Wherein, the PPA A-1000 of polyphthalamide Wei Su prestige company, TLCP is the Vectra type TLCP that Ticona company produces, and zirconium white is the cubic polycrystal zirconia (3Y-TZP) of 3mol% stabilized with yttrium oxide, and titanium dioxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is as follows:
S31: take each component according to the formula of above-mentioned polyphthalamide composite material;
S32: the polyphthalamide taking, TLCP component are placed in to mixing machine, and mix 20 minutes under the condition of middling speed, obtain the first mixture;
S33: the zirconium white taking, titanium dioxide component are placed in to mixing machine, and mix 35 minutes under the condition of middling speed, obtain the second mixture;
S34: the opening for feed that the first mixture is placed in to twin screw extruder feeds, adopt weight-loss metering to claim the second mixture to feed from the side material mouth of twin screw extruder simultaneously, and through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, twin screw extruder processing condition are: 290 ℃, 275 285 300 290 ℃, 5th district, ℃, 4th district, ℃, 3rd district, ℃, 2nd district, a district, and 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 as follows:
55 parts of polyphthalamides, 15 parts of TLCP, 15 parts of zirconium whites, 25 parts of titanium dioxide.Wherein, the A-4000 of polyphthalamide Wei Su prestige company, TLCP is the Vectra type TLCP that Ticona company produces, and zirconium white is the cubic polycrystal zirconia (3Y-TZP) of 3mol% stabilized with yttrium oxide, and titanium dioxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is as follows:
S41: take each component according to the formula of above-mentioned polyphthalamide composite material;
S42: the polyphthalamide taking, TLCP component are placed in to mixing machine, and mix 40 minutes under the condition of middling speed, obtain the first mixture;
S43: the zirconium white taking, titanium dioxide component are placed in to mixing machine, and mix 25 minutes under the condition of middling speed, obtain the second mixture;
S44: the opening for feed that the first mixture is placed in to twin screw extruder feeds, adopt weight-loss metering to claim the second mixture to feed from the side material mouth of twin screw extruder simultaneously, and through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, twin screw extruder processing condition are: 280 ℃, 285 295 300 290 ℃, 5th district, ℃, 4th district, ℃, 3rd district, ℃, 2nd district, a district, and 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 as follows:
45 parts of polyphthalamides, 20 parts of TLCP, 25 parts of zirconium whites, 10 parts of titanium dioxide.Wherein, the PPA A-1000 of polyphthalamide Wei Su prestige 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 dioxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is as follows:
S51: take each component according to the formula of above-mentioned polyphthalamide composite material;
S52: the polyphthalamide taking, TLCP component are placed in to mixing machine, and mix 20 minutes under the condition of middling speed, obtain the first mixture;
S53: the zirconium white taking, titanium dioxide component are placed in to mixing machine, and mix 28 minutes under the condition of middling speed, obtain the second mixture;
S54: the opening for feed that the first mixture is placed in to twin screw extruder feeds, adopt weight-loss metering to claim the second mixture to feed from the side material mouth of twin screw extruder simultaneously, and through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, twin screw extruder processing condition are: 285 ℃, 270 285 300 300 ℃, 5th district, ℃, 4th district, ℃, 3rd district, ℃, 2nd district, a district, and 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 as follows:
70 parts of polyphthalamides, 30 parts of titanium dioxide.Wherein, the PPA A-1000 of this polyphthalamide Wei Su prestige company, titanium dioxide is rutile titanium dioxide.
The preparation method of polyphthalamide composite material is as follows:
S11: take each component according to the formula of above-mentioned polyphthalamide composite material;
S12: the opening for feed that polyphthalamide is placed in to twin screw extruder feeds, adopt weight-loss metering to claim titanium dioxide to feed from the side material mouth of twin screw extruder simultaneously, and through twin screw extruder melt extrude, granulation, obtain polyphthalamide composite material; Wherein, twin screw extruder processing condition are: 290 ℃, 280 290 300 300 ℃, 5th district, ℃, 4th district, ℃, 3rd district, ℃, 2nd district, a district, and this mixture time of delivery in the screw rod of twin screw extruder is 3min, pressure is 16MPa.
Performance evaluation criterion and performance index:
Above-described embodiment 1~5 and the prepared polyphthalamide composite material of comparison example are carried out to related mechanical properties evaluation by following detection method and standard:
Above-described embodiment 1~5 and the prepared polyphthalamide composite material particle of comparison example are dried to 4 hours respectively in the convection oven of 140 ℃, by the injection moulding sample preparation on 80T injection moulding machine of dry particle, in sample making course, keep mould temperature between 70~100 ℃ again.
Stretching strength determination: test by GB/T 1040 standards; Specimen types is 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: by GB/T 9341 standards, test; Specimen types is specimen size (mm): (80 ± 2) * (10 ± 0.2) * (4 ± 0.2), rate of bending is 20mm/min.
Heat-drawn wire is measured: by GB/T 1634.2 standards, test, load is 1.80MPa, and span is 100mm.
Flame retardant properties is measured: according to UL 94 standards, detect specimen size (mm): 130 (length) * (20 ± 0.2) (end width) * (1.6 ± 0.2) (thickness).
The prepared polyphthalamide composite material correlated performance test result of above-described embodiment 1~5 and comparison example is respectively as table 1:
Polyphthalamide composite material performance test prepared by table 1: embodiment 1~5 and comparison example
Figure BDA0000122054120000111
From upper table 1 data, can find out, compare with comparison example, the polyphthalamide composite material of embodiment 1~5 have that whiteness is even, whiteness is high and there is 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, related mechanical properties and the thermal stability of polyphthalamide composite material strengthen thereupon.This is because TLCP has the less characteristic of the less and long-term light decay of water absorbability compared with polyphthalamide, and TLCP in extrusion with polyphthalamide effect, and can form microfibrillar structure in polyphthalamide matrix, intensity and the thermostability of this polyphthalamide composite material have been improved, 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 polyphthalamide composite material processing characteristics, and effectively avoid polyphthalamide composite material to be oxidized in the course of processing, degraded and consequent degradation.As can be seen here, titanium dioxide and zirconium white and TLCP are composite, make this polyphthalamide composite material have high whiteness, have improved thermostability, the mechanical property of matrix material.Therefore, formula by above-described embodiment polyphthalamide composite material with and preparation method thereof, the embodiment of the present invention has been prepared not only there is high whiteness but have good thermal stability can and the polyphthalamide composite material of mechanical property, overcome the deficiency that existing PPA material only has good whiteness, thermostability and bad mechanical property.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.

Claims (7)

1. a polyphthalamide composite material, comprises the recipe ingredient of following parts by weight:
45~68 parts of polyphthalamides
1~20 part of TLCP
1~25 part of zirconium white
10~30 parts of titanium dioxide;
Described TLCP is backbone chain type TLCP, and described backbone chain type TLCP is aromatic copolyester, and its fusion range is 260~350 ℃.
2. polyphthalamide composite material according to claim 1, is characterized in that, described zirconium white is at least one in the zirconium white of monocline, four directions, cubic crystal phase morphology.
3. polyphthalamide composite material according to claim 1, is characterized in that, described zirconium white is the zirconium white through the tetragonal phase form of 3moL% stabilized with yttrium oxide processing.
4. according to the polyphthalamide composite material described in claim 1 or 2 or 3, it is characterized in that, described titanium dioxide is anatase titanium dioxide and/or rutile titanium dioxide.
5. according to the polyphthalamide composite material described in claim 1 or 2 or 3, it is characterized in that, described titanium dioxide is rutile titanium dioxide.
6. a polyphthalamide composite material preparation method, comprises the following steps:
According to the formula of the arbitrary described polyphthalamide composite material of claim 1~5, take each component;
The described polyphthalamide taking, TLCP are mixed, form the first mixture;
The described zirconium white taking, titanium dioxide are mixed, form the second mixture;
Described the first mixture is added in the opening for feed of forcing machine, described the second mixture is added in the side spout of forcing machine simultaneously and melt extrude, granulation, obtains described polyphthalamide composite material.
7. polyphthalamide composite material preparation method according to claim 6, it is characterized in that, described extruding is to adopt twin screw extruder to extrude, described the first mixture and the temperature of the second mixture in described twin screw extruder are respectively: 260~300 ℃ of district's temperature, two 270~310 ℃ of district's temperature, three 260~300 ℃ of district's temperature 270~310 ℃, tetra-district's temperature 260~300 ℃, five district's temperature; Described the first mixture and the second mixture time of delivery in the screw rod of twin screw extruder is 2~5 minutes, and pressure is 12~20MPa.
CN201110426967.2A 2011-12-19 2011-12-19 Poly phthalimide amide composite material and preparation method thereof Expired - Fee Related CN102532886B (en)

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