CN101210087A - Nanometer calcium carbonate polypropylene composite material - Google Patents
Nanometer calcium carbonate polypropylene composite material Download PDFInfo
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- CN101210087A CN101210087A CNA2006101563235A CN200610156323A CN101210087A CN 101210087 A CN101210087 A CN 101210087A CN A2006101563235 A CNA2006101563235 A CN A2006101563235A CN 200610156323 A CN200610156323 A CN 200610156323A CN 101210087 A CN101210087 A CN 101210087A
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Abstract
The invention discloses nano calcium carbonate polypropylene composite material. The composite material comprises 100 portions of polypropylene resin, 1 to 15 portions of nano calcium carbonate, 1 to 20 portions of elastomer, and 0.1 to 1 portion of stabilizing agent. The composite material is prepared by method of melt compounding by adopting an internal mixer or double screw extruder. Good rigidity is kept when the toughness of the composite is obviously improved; the composite has good cold impact resistance performance, and is applicable to injection moulding production of automobile parts, i.e. bumper, mudguard, etc.
Description
Technical field:
The present invention relates to a kind of polypropylene composite material, the matrix material that particularly a kind of nano-calcium carbonate and polypropylene are formed.
Background technology:
In order to reach energy-saving and environmental protection and to reduce integral vehicle cost to improve the purpose of the market competitiveness, in recent years automotive industry to the material lightweight, recyclable, cheaply require more and more stronger.Plastics and matrix material thereof are one of most important car light materials.
Polypropylene light weight, inexpensive, easy processing, recyclable and modification technology is ripe relatively, the application on automobile component more and more widely.
Usually automobile component require material to have favorable rigidity and tough sexual balance, and promptly material not only has favorable shock resistance but also have higher modulus in flexure.Because shortcomings such as polypropylene is the high crystalline polymkeric substance, exists shock strength lower, and especially low temperature impact properties is poor, and dimensional stability is bad.So mostly the polypropylene material that uses on the automobile is the polypropylene composite material through chemistry or physically modified.The method that tradition is improved the polypropene impact-resistant performance mainly is to add the toughness that elastomerics (as terpolymer EP rubber (EPDM), ethylene-octene copolymerization thermoplastic elastomer (POE), styrene butadiene block copolymerization thermoplastic elastomer (SBS) or the like) increases material in acrylic resin.But elastomeric adding has reduced the rigidity and the intensity of material.For this reason, must add inorganic mineral fillers such as talcum powder again and improve bending elastic modulus, thereby reach rigidity and flexible balance.Because common inorganic mineral filler is improving the toughness that rigidity can reduce material simultaneously again, the resistance to impact shock of material is reduced, this adds more elastomerics with regard to needs and remedies and balance.Therefore, there are shortcomings such as cost height, density be big in traditional polypropylene compound system that is used for automobile component, can not adapt to automobile component low cost, light-weighted requirement.
The surface effects of nano inoganic particle, small-size effect make it can improve the macromolecular material performance significantly under lower addition.Along with inorganic nano-particles such as nano-calcium carbonate are realized low-cost suitability for industrialized production, the development of nano composite polymeric material, development and application become the research focus that receives much concern.
Chinese patent publication number CN1308099 (open day was: 2001.08.15), disclose a kind of nanometer calcium carbonate-polypropylene composite material and preparation method thereof.This matrix material mainly consists of polypropylene, wherein contains the nano-calcium carbonate of 0.25-30% (m/m).Preparation process is divided two steps: the first step is earlier the nano-calcium carbonate powder to be made the nano-calcium carbonate master batch with coupling agent treatment and with a certain proportion of polypropylene mixing granulation; Second step with the lime carbonate master batch of step 1 with certain proportion and the polypropene blended nanometer calcium carbonate-polypropylene composite material of making.The Izod notched Izod impact strength of this matrix material is 1-6 a times of virgin pp resin, and tensile strength, modulus in flexure, Rockwell hardness and heat-drawn wire also all improve than virgin pp, but the not mentioned low-temperature impact resistance that improves matrix material of this patent, and at automotive field, especially be applied to automobile exterior components such as collision bumper, splash pan, the lower temperature resistance of material is the performance that can not be ignored.
Summary of the invention:
The object of the present invention is to provide a kind of nanometer calcium carbonate polypropylene composite material, this material has light weight, intensity height, rigidity and tough sexual balance, characteristics such as low-temperature impact-resistant performance excellence.
The present invention is body material with the polypropylene, and elastomerics is strongthener as toughening material through active nano-calcium carbonate powder or the nano-calcium carbonate master batch of handling that organise, and nano-calcium carbonate plays the effect of coordination plasticizing simultaneously.
Specifically, the quality proportioning of each component is in the sodium rice calcium carbonate polypropylene composite material of the present invention:
100 parts of polypropylene (A)
1～15 part of nano-calcium carbonate (B)
1～20 part on elastomerics (C)
0.1～1 part of stablizer (D).
Nanometer calcium carbonate polypropylene composite material of the present invention mainly comprises A, B, four components of C, D.
As the acrylic resin of A component is that the melt flow rate (MFR) (MFR) of suitability for industrialized production is the acrylic resin of 1～60g/10min.This acrylic resin can be a homopolymer, can be the ethylene-propylene copolymer segmented copolymer of 5～30% (molar percentages) for ethylene content also.The acrylic resin of this component can be that polypropylene powder also can be a polypropylene granules.
Nano-calcium carbonate as the B component is the n-CaCO of carrier for the surface through the active nano-calcium carbonate powder of surface-modifying agents such as coupling agent processing or with the polypropylene
3Master batch.Nano-calcium carbonate is that median size is the light calcium carbonate of 20～100nm.
Elastomerics as the C component can be ethylene propylene rubber (EPR), terpolymer EP rubber (EPDM), ethylene-octene copolymerization thermoplastic elastomer (POE), styrene butadiene block copolymerization thermoplastic elastomer (SBS).These elastomericss can use separately as toughner, and use mutually also can combine.
Stablizer as the D component is made up of oxidation inhibitor, photostabilizer and halogen-absorber.Oxidation inhibitor wherein can be the oxidation inhibitor that improves the material thermal-oxidative aging property, (four [3-(3 to comprise Hinered phenols antioxidant such as lrganox 1010, the 5-di-tert-butyl-hydroxy phenyl) acid in] pentaerythritol ester), 1076 (β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid octadecanol ester), 7910 (four [B (3,5 one di-t-butyls, one 4 monohydroxy phenyl) propionic acid] season penta recessed alcohol ester), 264 (2, the 6-di-tert-butyl-4-methy phenol) etc., phosphite ester kind antioxidant is as 168 (tricresyl phosphites (2, the 4-di-tert-butyl-phenyl) ester), 626 (two (2,4-di-tert-butyl phenyl) phosphorous acid pentaerythritol ester) etc., thio-based oxidation inhibitor such as PS802FL (thio-2 acid dialkyl), DLTP (Tyox B), DSTP (thio-2 acid 2 stearyl ester) etc., and contain the composite antioxidant of above-mentioned substance; Photostabilizer can be the benzotriazole category UV light absorber, as UV-326 (2-(the 2-hydroxyl-3-tertiary butyl-5-aminomethyl phenyl)-5-chlorinated benzotriazole), UV-327 (2-(2--hydroxyl-3, the 5-di-tert-butyl-phenyl)-5-chloro benzo triazole) etc., hindered amine light stabilizer is as 622 (poly-(1-hydroxyethyls-2,2,6,6-tetramethyl--4-hydroxy piperidine) succinate); Halogen-absorber can be calcium stearate, Zinic stearas etc.
Nanometer calcium carbonate polypropylene composite material of the present invention also can comprise the polyolefine of introducing small amount of polar group on the molecular chain as compatilizer, as graft polypropylenes such as maleic anhydride, vinylformic acid; A spot of processing aid is as amine hydroxybenzene, erucicamide, ethylene bis stearic acid amide (EBS) etc.
Adopt nanometer CaCO
3Inorganic nano materials such as elastomerics carry out toughness reinforcing to plastics such as polypropylene, belong to the inorganic rigid particle toughened system.Its toughening mechanism is: the tiny nano-calcium carbonate of (1) particle size can bring out polypropylene to a certain extent and generate the β crystalline substance, and the brilliant hexagonal system structure that belongs to of β, helping the polypropylene flexible improves; (2) when the matrix material stress and deformation, the existence of Nano particles of calcium carbonate produces stress concentration effect, thereby the energy that polypropylene matrix generation deformation at yield is absorbed arrives and improves the flexible purpose; (3) for the polypropylene/elastomer system, the adding of undersized nano-calcium carbonate helps elastomeric dispersion, refinement on the one hand, makes giving full play to of elastomeric toughening effect, adds n-CaCO on the other hand
3After make in the matrix material disperse phase form elastomerics to comprise the nucleocapsid structure of inorganic rigid particle, thereby make matrix material when toughness is improved significantly, keep favorable rigidity.
In addition, because the present invention has added elastomerics in compound system, and utilize nano-calcium carbonate and the elastomerics coordination plasticizing effect good to acrylic resin, and make matrix material keep favorable rigidity and flexible simultaneously, low-temperature impact resistance is greatly improved.
The preparation method of matrix material of the present invention:
Method 1: with said components melting mixing in two roller Banbury mixeies, extruding pelletization.Processing temperature: 160 ℃～230 ℃.
Method 2: join twin screw extruder melting mixing, extruding pelletization after said components mixed in homogenizer.Extrusion temperature: 170 ℃～240 ℃, screw speed: 150～320rpm.
Embodiment:
Below, with the invention will be further described with Comparative Examples in conjunction with the embodiments.But the present invention is not subjected to the restriction of embodiment content.
Comparative Examples 1:100 part melt flow rate (MFR) is that the crushing-resistant copolymerization polypropylene of 20g/10min adds 20 parts of EPDM, 10 parts of talcum powder, 0.2 part of 1010,0.15 parts of 168,0.3 parts of UV-326,0.1 part of calcium stearate, in high-speed mixer, mix, through the twin screw extruder melt blending, extrude, granulation.Performance sees Table 1.
Embodiment 1:100 part melt flow rate (MFR) is the crushing-resistant copolymerization polypropylene of 20g/10min, adds 18 parts of EPDM, 14 parts of n-CaCO
3Master batch (n-CaCO
3Content 60wt%), 0.2 part 1010,0.15 parts 168,0.3UV-326 part, 0.1 part of calcium stearate, through the twin screw extruder melt blending, extrude, granulation.Performance sees Table 1.
Embodiment 2:100 part melt flow rate (MFR) is that the crushing-resistant copolymerization polypropylene of 15g/10min adds 15 parts of EPDM, 10 parts of n-CaCO
3Master batch, 0.2 part of 1010,0.15 parts of 168,0.3 parts of UV-326,0.1 part of calcium stearate, through the twin screw extruder melting mixing, extrude, granulation.Performance sees Table 1.
Embodiment 3:100 part melt flow rate (MFR) is that the crushing-resistant copolymerization polypropylene powder of 3g/10min adds 6 parts of n-CaCO3 powders, 1 part of SBS, 0.2 part of 1010,0.15 parts of 168,0.3 parts of 622,0.1 parts of calcium stearate, melt blending in Banbury mixer is extruded, pelletizing.Performance sees Table 1.
Embodiment 4:100 part melt flow rate (MFR) is that the crushing-resistant copolymerization polypropylene of 55g/10min adds 8 parts of POE, 8 parts of EPR, 3 parts of n-CaCO
3, 8 parts of talcum powder, 6 parts of maleic anhydride inoculated polypropylenes, 0.2 part of 1010,0.15 parts of 168,0.3 parts of UV-326,0.1 part of calcium stearate, through the twin screw extruder melt blending, extrude, granulation.Performance sees Table 1.
Embodiment 5:100 part melt flow rate (MFR) is in the crushing-resistant copolymerization polypropylene of 30g/10min, adds 15 parts of EPDM, 14 parts of n-CaCO
3, 0.2 part of amine hydroxybenzene, 0.2 part of 1010,0.15 parts of 168,0.3 parts of UV-327,0.1 part of calcium stearate, through the twin screw extruder melt blending, extrude, granulation.Performance sees Table 1.
Embodiment 6:100 part melt flow rate (MFR) is in the homo-polypropylene of 2.5g/10min, adds 15 parts of SBS, 2 parts of n-CaCO
3, 0.2 part of amine hydroxybenzene, 0.2 part of 1010,0.15 parts of 168,0.1 parts of calcium stearate, through the twin screw extruder melt blending, extrude, granulation.Performance sees Table 1.
Table 1
Comparative Examples 2:100 part melt flow rate (MFR) is that the Co-polypropylene of 10g/10min adds 10 parts of POE, 0.2 part of 1010,0.15 parts of 168,0.1 parts of calcium stearate, through the twin screw extruder melt blending, extrude, granulation.Performance sees Table 2.
Embodiment 7:100 part melt flow rate (MFR) is that the Co-polypropylene of 10g/10min adds 10 parts of POE, 10 parts of n-CaCO
3, 0.2 part of 1010,0.15 parts of 168,0.15 parts of DLTP, 0.1 part of calcium stearate, through the twin screw extruder melt blending, extrude, granulation.Performance sees Table 2.
Embodiment 8:40 part melt flow rate (MFR) is that crushing-resistant copolymerization polypropylene and 60 parts of melt flow rate (MFR)s of 10g/10min are in the 10g/10min homo-polypropylene, adds 15 parts of POE, 10 parts of n-CaCO
3, 0.2 part of 1010,0.15 parts of 168,0.15 parts of PS802FL, 0.1 part of calcium stearate, through the twin screw extruder melt blending, extrude, granulation.Performance sees Table 2.
Table 2
The testing method of every performance is in the table: melt flow rate (MFR) adopts the GB/T3682 standard method; Modulus in flexure adopts the GB/T9341 standard method; Tensile yield strength and elongation at break adopt the GB/T1040 standard method; The simply supported beam notched Izod impact strength adopts GB/T 1043 standard methods.
By the result of table 1 and table 2 as can be seen, polypropene composition of the present invention has good fluidity and rigidity and tough sexual balance, especially has good low-temperature impact resistance, can be used for the injection moulding of automobile component such as collision bumper, splash pan, accumulator housing, also can be used for the injection-molded item that other has higher requirements to low-temperature impact performance.
Claims (15)
1. nanometer calcium carbonate polypropylene composite material is characterized in that described matrix material comprises following component:
(A) 100 parts of acrylic resins (by weight)
(B) 1～15 part of nano-calcium carbonate (by weight)
(C) 1～20 part on elastomerics (by weight)
(D) 0.1～1 part of stablizer (by weight)
2. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that described acrylic resin (A) is the acrylic resin of 1～60g/10min for the melt flow rate (MFR) of suitability for industrialized production (MFR).
3. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that described acrylic resin (A) is ethylene-propylene copolymer segmented copolymer and/or homo-polypropylene.
4. nanometer calcium carbonate polypropylene composite material according to claim 3 is characterized in that in the described ethylene-propylene copolymer segmented copolymer, ethylene content is 5～30mol%.
5. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that described sodium rice lime carbonate (B) is the active nano-calcium carbonate powder of surface through coupling agent treatment.
6. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that described sodium rice lime carbonate (B) is for being the n-CaCO3 master batch of carrier with the polypropylene.
7. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that described sodium rice lime carbonate (B) is that median size is the light calcium carbonate of 20～100nm.
8. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that described elastomerics (C) mixes for one or more of ethylene propylene rubber (EPR), terpolymer EP rubber (EPDM), ethylene-octene copolymerization thermoplastic elastomer (POE), styrene butadiene block copolymerization thermoplastic elastomer (SBS).
9. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that described stablizer (D) is made up of oxidation inhibitor, photostabilizer and halogen-absorber.
10. nanometer calcium carbonate polypropylene composite material according to claim 9 is characterized in that described oxidation inhibitor is 1010,7910,168,264 and composition thereof.
11. nanometer calcium carbonate polypropylene composite material according to claim 9 is characterized in that described photostabilizer is UV light absorber and hindered amine light stabilizer.
12. nanometer calcium carbonate polypropylene composite material according to claim 9 is characterized in that described halogen-absorber is calcium stearate and/or Zinic stearas.
13. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that the method for this composite material by adopting Banbury mixer or twin screw extruder melt blending is prepared from.
14. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that polyolefine that described matrix material adds the small amount of polar group as compatilizer, preferred maleic anhydride, acrylic acid-grafted polypropylene.
15. nanometer calcium carbonate polypropylene composite material according to claim 1 is characterized in that described matrix material adds a little auxiliary, a kind of in preferred amine hydroxybenzene, erucicamide, the ethylene bis stearic acid amide (EBS).
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