CN101376728A - Reinforced polypropylene composite material and preparation thereof - Google Patents
Reinforced polypropylene composite material and preparation thereof Download PDFInfo
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- CN101376728A CN101376728A CNA2008102164388A CN200810216438A CN101376728A CN 101376728 A CN101376728 A CN 101376728A CN A2008102164388 A CNA2008102164388 A CN A2008102164388A CN 200810216438 A CN200810216438 A CN 200810216438A CN 101376728 A CN101376728 A CN 101376728A
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Abstract
The invention discloses a reinforced polypropylene compound material and a preparation method. The reinforced polypropylene compound material includes the following components and weight portions: 100 portions of PP resin, 10 to 50 portions of reinforced modifier, 2 to 10 portions of macromolecular compatilizer, 0.1 to 0.5 portion of coupling agent as well as 0.1 to 0.5 portion of antioxidant; wherein, the PP resin is homo PP; the reinforced modifier is hollow glass beads; the macromolecular compatilizer is maleic anhydride-grafted polypropylene; the coupling agent is a silane coupling agent. The invention also discloses a preparation method for manufacturing the reinforced polypropylene compound material. The reinforced polypropylene compound material not only has the advantages of good toughness, high intensity and less contraction, but also has the advantages of smooth surface and low specific gravity.
Description
[technical field]
The present invention relates to the high molecule plastic technical field, relate in particular to a kind of reinforced polypropylene compound material and preparation method thereof.
[background technology]
Polypropylene (PP) is one of five big general-purpose plastics, and density is 0.90g/cm
3, be that (only greater than polymethylpentene, density is 0.85g/cm to the existing resin second light macromolecular material
3).Performance is good, proportion is little, be easy to characteristics such as forming process because of it has, and is widely used in automotive industry, household electrical appliance, electronic instrument industry, the textile industry.
Yet because the mechanical property of PP resin is lower, tensile strength 30MPa, the flexural strength 36MPa that only has an appointment that only has an appointment wherein makes it be subjected to a certain degree restriction when need to be applied to some structural parts of holding capacity.This just requires to develop enhanced PP matrix material, significantly promote material mechanical property, have excellent toughness and smooth surface, to satisfy people's demand.
In the prior art, people have done a large amount of work when the production reinforced polypropylene compound material.Reinforced polypropylene compound material mainly is to add glass fibre and make in acrylic resin.But by studies show that, though significantly improve with glass fibre enhanced polypropylene matrix material mechanical strength, the surface floating fiber of material has had a strong impact on the visual appearance of material, and higher proportion also is unfavorable for reducing cost.People also attempt to replace glass to open dimension with hollow glass micropearl and come Reinforced Polypropylene, to improve the surface gloss of material, solve the floating fine tight problem that gets.Yet a ubiquitous problem is troubling everybody all the time, is exactly that hollow glass micropearl very easily breaks in the course of processing and to make material property get the increasing degree degree little, can't reach the enhanced effect.
Owing to traditional increase strong polypropylene composite material and can't satisfy product mechanical strength height, good toughness, low, the ganoid requirement of proportion simultaneously.Thereby develop a kind of good toughness, intensity height, shrink for a short time, and smooth surface, novel enhanced polypropylene material that proportion is low seem especially important.
[summary of the invention]
The technical problem to be solved in the present invention provides a kind of not only intensity height, good toughness, and low, the ganoid reinforced polypropylene compound material of proportion.
The present invention will provide the preparation method of this reinforced polypropylene compound material.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, a kind of reinforced polypropylene compound material, and this material comprises following composition and parts by weight:
PP resin 100
Reinforced modifier 10--50
High molecular compatible agent 3--10
Coupling agent 0.1--0.5
Oxidation inhibitor 0.1--0.5
Wherein, described PP resin is a homopolymerization PP, and described reinforced modifier is a hollow glass micropearl, and described high molecular compatible agent is maleic anhydride graft PP, and described coupling agent is a silane coupling agent.
Above-described Reinforced Polypropylene material, described oxidation inhibitor are that phosphite ester kind antioxidant 168 and Hinered phenols antioxidant 1010 form by mass parts 2:1 is composite.
Above-described Reinforced Polypropylene material, the particle diameter of described hollow glass micropearl are 10 to 200 microns.
The preparation method of above-described reinforced polypropylene compound material may further comprise the steps:
1) takes by weighing PP resin 100 by umber, reinforced modifier 10-50, high molecular compatible agent 2-10, coupling agent 0.1--0.5, oxidation inhibitor 0.1--0.5;
2) composition that step 301 is taken by weighing mixed in high-speed mixer 3--5 minute;
3) mixed raw material is placed single screw extrusion machine through melt extrude, granulation, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02~-0.04MPa.。
The present invention uses hollow glass micropearl to substitute traditional glass fibre and does reinforced modifier, and the gained material surface is smooth, and proportion reduces, and has kept higher intensity and good toughness.The present invention uses silane coupling agent to improve the surfactivity of hollow glass micropearl, uses maleic anhydride graft PP to do the high molecular compatible agent, has significantly improved the comixing compatibility between acrylic resin and the hollow glass micropearl; The preparation method that the present invention proposes uses single screw extrusion machine to carry out extruding pelletization, greatly reduce and melt extrude the hollow glass micropearl that causes because of screw rod shearing in the granulation process degree of breaking, not only strengthen and improve toughness, the intensity of polypropylene material, and reduce the proportion of material greatly; By adding oxidation inhibitor, make the heatproof oxidation performance of material to be improved, solve material xanthochromia phenomenon.
[embodiment]
Below by embodiment the present invention is further set forth:
The reinforced polypropylene compound material that the present invention proposes need be used following starting material: PP resin, reinforced modifier, high molecular compatible agent, coupling agent, oxidation inhibitor.
Wherein, the PP resin is the homopolymerization PP V30G of Guangzhou petrochemical industry, reinforced modifier is that particle diameter that emperor's glass microballon company limited of the Qin produces is hollow glass micropearl phase of 10-200 micron to finish K-180, the high molecular compatible agent is the maleic anhydride graft PP PC-1 that South Sea Bai Chen polymer novel material company limited produces, coupling agent is the silane resin acceptor kh-550 that Hangzhou boiling point chemical industry company limited produces, and oxidation inhibitor is that the phosphite ester kind antioxidant 168 produced of vapour crust fine chemistry industry and Hinered phenols antioxidant 1010 are by the composite self-control Compositional type that forms of mass parts 2:1.
Embodiment all uses given raw material of the present invention and preparation method; Raw material in the Comparative Examples all is the given raw material of the present invention, and the preparation method is traditional parallel double-screw extruder.
Embodiment 1
By weight, with PP resin 100, reinforced modifier hollow glass micropearl 10, maleic anhydride graft PP 3, silane coupling agent 0.1, oxidation inhibitor 0.1, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed single screw extrusion machine through fusion squeeze, granulation, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.
Embodiment 2
By weight, with PP resin 100, reinforced modifier hollow glass micropearl 30, maleic anhydride graft PP 7, silane coupling agent 0.3, oxidation inhibitor 0.3, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed single screw extrusion machine through fusion squeeze, granulation, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.
Embodiment 3
By weight, with PP resin 100, reinforced modifier hollow glass micropearl 50, maleic anhydride graft PP 10, silane coupling agent 0.5, oxidation inhibitor 0.5, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed single screw extrusion machine through fusion squeeze, granulation, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.
Performance to prepared material in the embodiment of the invention describes below:
With the particulate material of finishing granulation as stated above under 80-90 ℃ baking oven dry 2 hours in advance, then that drying is good particulate material injected the standard testing batten on injection moulding machine.
Tensile property is undertaken by ISO 527, and specimen size is 150 * 10 * 4 millimeters, and draw speed is 50 mm/min; Bending property is undertaken by ISO 178, and specimen size is 80 * 10 * 4 millimeters, and rate of bending is 2 mm/min, and span is 50 millimeters; The simply supported beam notched Izod impact strength is undertaken by ISO 180, and specimen size is 80 * 10 * 4 millimeters, and notch depth is 1/3 of a sample thickness; The examination of thermal distortion temperature is undertaken by ISO 75, and specimen size is 120 * 15 * 10 millimeters, and load is 1.82MPa; Proportion is undertaken by ISO 1183; Shrinking percentage is undertaken by ISO 2577.
The numerical value and the product surface quality of tensile strength, the elongation at break of the over-all properties of material by the test gained, flexural strength, modulus in flexure, IZOD notched Izod impact strength, heat-drawn wire, proportion, shrinking percentage are passed judgment on.
The prescription of embodiment 1 to 3 and every The performance test results see the following form (one):
Table (one) embodiment 1 to 3 performance formula synopsis
Material name transitivity parameter | Example 1 | Example 2 | Example 3 |
The PP resin | 100 | 100 | 100 |
Hollow glass micropearl | 10 | 30 | 50 |
Maleic anhydride graft PP | 3 | 7 | 10 |
Silane coupling agent | 0.1 | 0.3 | 0.5 |
The oxidation inhibitor self-control is composite | 0.1 | 0.3 | 0.5 |
Tensile strength (MPa) | 36 | 48 | 60 |
Elongation at break (%) | 20 | 15 | 12 |
Flexural strength (MPa) | 42 | 60 | 75 |
Modulus in flexure (MPa) | 2200 | 4000 | 5600 |
IZOD notched Izod impact strength (KJ/M2) | 10 | 12 | 15 |
Melting index (g/10 minute) | 15 | 10 | 8 |
Heat-drawn wire (℃) | 130 | 140 | 155 |
Proportion (g/cm3) | 0.92 | 0.98 | 1.02 |
Shrinking percentage (%) | 1.2 | 1.0 | 0.6 |
Product surface quality | Smooth | Smooth | Smooth |
As can be seen, along with the increase of reinforced modifier hollow glass micropearl, high molecular compatible agent maleic anhydride graft PP, silane coupling agent, oxidation inhibitor addition, the tensile strength of material, flexural strength, modulus in flexure significantly rise from table (); The IZOD notched Izod impact strength of material, heat-drawn wire all are significantly improved; The melting index of material significantly reduces; The shrinking percentage of material significantly reduces; The proportion of material slightly increases; And the product surface quality of material does not all have the glass emergence on the surface phenomenon, is smooth shape.
Comparative Examples 1
By weight, with PP resin 100, reinforced modifier hollow glass micropearl 10, maleic anhydride graft PP 3, silane coupling agent 0.1, oxidation inhibitor 0.1, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed cocurrent and parallel twin screw bar forcing machine through fusion squeeze, granulation, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.
Comparative Examples 2
By weight, with PP resin 100, reinforced modifier hollow glass micropearl 30, maleic anhydride graft PP7, silane coupling agent 0.3, oxidation inhibitor 0.3, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed the cocurrent and parallel twin screw extruder through fusion squeeze, granulation, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.
Comparative Examples 3
By weight, with PP resin 100, reinforced modifier hollow glass micropearl 50, maleic anhydride graft PP 10, silane coupling agent 0.5, oxidation inhibitor 0.5, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed the cocurrent and parallel twin screw extruder through fusion squeeze, granulation, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.
Comparative Examples 4
By weight, with PP resin 100, maleic anhydride graft PP 3, silane coupling agent 0.1, oxidation inhibitor 0.1, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed cocurrent and parallel twin screw bar forcing machine through fusion squeeze, granulation, add glass fibre 10 in the extrusion, expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.
Comparative Examples 5
By weight, with PP resin 100, maleic anhydride graft PP7, silane coupling agent 0.3, oxidation inhibitor 0.3, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed the cocurrent and parallel twin screw extruder through fusion squeeze, granulation, add glass fibre 30 in the extrusion, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.
Comparative Examples 6
Rate 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02---0.04MPa.By weight, with PP resin 100, maleic anhydride graft PP10, silane coupling agent 0.5, oxidation inhibitor 0.5, mixed 3--5 minute in high-speed mixer, the high-speed mixer rotating speed is 600 rev/mins; Then mixed raw material is placed the cocurrent and parallel twin screw extruder through fusion squeeze, granulation, add glass fibre 50 in the extrusion, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding are frequently
The prescription of Comparative Examples 1 to 3 and every The performance test results see the following form (two):
Table (two) Comparative Examples 1 to 3 performance formula synopsis
Material name transitivity parameter | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 |
The PP resin | 100 | 100 | 100 |
Hollow glass micropearl | 10 | 30 | 50 |
Maleic anhydride graft PP | 3 | 7 | 10 |
Silane coupling agent | 0.1 | 0.3 | 0.5 |
The oxidation inhibitor self-control is composite | 0.1 | 0.3 | 0.5 |
Tensile strength (MPa) | 20 | 32 | 40 |
Elongation at break (%) | 40 | 25 | 20 |
Flexural strength (MPa) | 32 | 40 | 52 |
Modulus in flexure (MPa) | 1500 | 2200 | 3600 |
IZOD notched Izod impact strength (KJ/M2) | 8 | 12 | 15 |
Melting index (g/10 minute) | 15 | 10 | 8 |
Heat-drawn wire (℃) | 110 | 140 | 155 |
Proportion (g/cm3) | 0.95 | 1.03 | 1.08 |
Shrinking percentage (%) | 1.2 | 1.0 | 0.6 |
Product surface quality | Smooth | Smooth | Smooth |
As can be seen, along with the increase of reinforced modifier hollow glass micropearl, high molecular compatible agent maleic anhydride graft PP, silane coupling agent, oxidation inhibitor addition, the tensile strength of material, flexural strength, modulus in flexure significantly rise from table (two); The IZOD notched Izod impact strength of material, heat-drawn wire all are significantly improved; The melting index of material significantly reduces; The shrinking percentage of material significantly reduces; The proportion of material slightly increases; And the product surface quality of material does not all have the glass emergence on the surface phenomenon, is smooth shape.
The prescription of Comparative Examples 4 to 6 and every The performance test results see the following form (three):
Table (three) Comparative Examples 4 to 6 performance formula synopsis
Material name transitivity parameter | Comparative Examples 4 | Comparative Examples 5 | Comparative Examples 6 |
The PP resin | 100 | 100 | 100 |
Glass fibre | 10 | 30 | 50 |
Maleic anhydride graft PP | 3 | 7 | 10 |
Silane coupling agent | 0.1 | 0.3 | 0.5 |
The oxidation inhibitor self-control is composite | 0.1 | 0.3 | 0.5 |
Tensile strength (MPa) | 32 | 45 | 40 |
Elongation at break (%) | 18 | 12 | 20 |
Flexural strength (MPa) | 40 | 56 | 52 |
Modulus in flexure (MPa) | 2000 | 3600 | 3600 |
IZOD notched Izod impact strength (KJ/M2) | 7 | 10 | 12 |
Melting index (g/10 minute) | 14 | 9 | 7 |
Heat-drawn wire (℃) | 120 | 130 | 145 |
Proportion (g/cm3) | 0.95 | 1.03 | 1.08 |
Shrinking percentage (%) | 1.2 | 1.0 | 0.6 |
Product surface quality | Obviously floating fine | Floating fine serious | Floating fine serious |
By showing (one) and showing (two) more as can be known, to compare with single screw extrusion machine, the material that uses the cocurrent and parallel twin screw extruder to produce: the amplification of tensile strength, flexural strength, modulus in flexure reduces greatly; The raising of IZOD notched Izod impact strength, heat-drawn wire is slow; The proportion increase is bigger; Shrinking percentage, melting index, surface quality have no significant change.This is because when using the cocurrent and parallel twin screw extruder to produce, the screwing element havoc of twin screw the form of hollow glass micropearl, make hollow breaking, and then fail to reach the purpose of enhancings, reduction proportion.
By showing (one) and showing (three) more as can be known, hollow glass micropearl Reinforced Polypropylene material with single screw extrusion machine production is compared with the glass fiber reinforced polypropylene material that uses the production of cocurrent and parallel twin screw extruder, the amplification of tensile strength, flexural strength, modulus in flexure rises greatly, also increasing of IZOD notched Izod impact strength, heat-drawn wire, proportion reduces greatly; Any surface finish and eliminated floating fibre, shrinking percentage, melting index have no significant change.This is because when using hollow glass micropearl Reinforced Polypropylene material, hollow glass micropearl is easier being uniformly dispersed of polypropylene internal ratio glass fibre, can as glass fibre, not produce reunion, thereby effectively solve the floating fine problem of product surface, make material surface smooth; And use single screw extrusion machine production, guarantee the complete of maintenance particle shape that hollow glass micropearl is can be big to the greatest extent in process of production possible, thereby played the enhanced effect.
In sum, the present invention significantly promotes tensile strength, flexural strength, the modulus in flexure of PP material by adding novel reinforced modifier hollow glass micropearl, high molecular compatible agent maleic anhydride graft PP, silane coupling agent; The IZOD notched Izod impact strength of material, heat-drawn wire obviously improve; The shrinking percentage of material significantly reduces; The proportion of material significantly reduces; The product surface of material is smooth, does not have floating fibre and exposes phenomenon; Thereby prepare a kind of not only mechanical strength height, good toughness but also proportion is low, shrinking percentage is little and the slick Reinforced Polypropylene material of product surface.Simultaneously, the present invention also introduced have the mechanical strength height, good toughness, proportion is low, shrinking percentage is little and unique preparation method of the slick Reinforced Polypropylene material of product surface.
Claims (4)
1, a kind of reinforced polypropylene compound material is characterized in that, this material comprises following composition and parts by weight:
PP resin 100
Reinforced modifier 10--50
High molecular compatible agent 3--10
Coupling agent 0.1--0.5
Oxidation inhibitor 0.1--0.5
Wherein, described PP resin is a homopolymerization PP, and described reinforced modifier is a hollow glass micropearl, and described high molecular compatible agent is maleic anhydride graft PP, and described coupling agent is a silane coupling agent.
2, Reinforced Polypropylene material according to claim 1 is characterized in that: described oxidation inhibitor is that phosphite ester kind antioxidant 168 and Hinered phenols antioxidant 1010 form by mass parts 2:1 is composite.
3, Reinforced Polypropylene material according to claim 1 is characterized in that: the particle diameter of described hollow glass micropearl is 10 to 200 microns.
4, the preparation method of the described reinforced polypropylene compound material of a kind of claim 1 is characterized in that, may further comprise the steps:
401) take by weighing PP resin 100 by umber, reinforced modifier 10-50, high molecular compatible agent 2-10, coupling agent 0.1--0.5, oxidation inhibitor 0.1--0.5;
402) composition that step 301 is taken by weighing mixed in high-speed mixer 3--5 minute;
403) mixed raw material is placed single screw extrusion machine through melt extrude, granulation, its expressing technique is: a district 170--180 ℃, two district 180--190 ℃, three district 180--190 ℃, four district 185--195 ℃, 300~350 rev/mins of screw speeds, feeding frequency 20~25Hz, melt pressure 3.0~4.0MPa, vacuum tightness-0.02~-0.04MPa.
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