CN102108175A - Low-gloss high-rigidity polypropylene compound material and preparation method thereof - Google Patents
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Abstract
The invention relates to a low-gloss high-rigidity polypropylene compound material and a preparation method thereof. The low-gloss high-rigidity polypropylene compound material is prepared from the following raw materials by weight percent: 55-91% of polypropylene, 0-25% of inorganic filling material, 0-10% of flexibilizer, 1-5% of nano montmorillonite, 2-4% of maleic anhydride grafted polypropylene (PP-G-MAG), 0.1-1% of antioxidant and 0-1% of other auxiliary agents. The preparation method comprises the following materials: mixing the polypropylene, the inorganic filling material, the flexibilizer, the nano montmorillonite, the PP-G-MAG, the antioxidant and the auxiliary agents in a high-speed agitator after weighing the raw materials in weight proportion; putting the mixture in a twin-screw extruder, and carrying out melt extrusion; and after extrusion, cooling, drying and pelletizing so that a finished product is obtained. The low-gloss high-rigidity polypropylene compound material has the advantages of low gloss, good impact toughness and good rigidity.
Description
Technical field
The present invention relates to the high strong and unyielding property polypropylene composite material of a kind of low gloss and form and preparation method thereof, more particularly by adding the glossiness of nano imvite reduction polypropylene composite material, material has higher impelling strength and rigidity simultaneously.Belong to polymer modification and processing technique field.
Background technology
Polypropylene (PP) has good processing properties and physics, mechanics, chemical property and electrical insulation capability because of it, and light weight, inexpensive is a kind of widely used general-purpose plastics, thereby is widely used in automotive industry in particular on the automotive interior material simultaneously.Along with the development of automobile industry, people are also more and more higher to the requirement that the driving indoor comfort reaches.If the glossiness of cab inside gadget is higher, just has stronger light reflection, thereby influence the comfortableness of navigating mate.Therefore, be used for automotive upholstery and need lower glossiness.
By on injection-moulding device, using suitable surface tissue or spraying sub-gloss varnish at product surface, product also can obtain low gloss, but its production cost is higher, and can not satisfy the requirement of use sometimes, and along with the prolongation of production time may need to handle again.The glossiness of polypropylene material own is higher, can not directly satisfy the requirement of automotive interior material, needs carry out the delustring modification to it.
In general in polypropylene, add common inorganic materials such as talcum powder, silicon-dioxide etc. and can it reduce glossiness, but extinction effect is unsatisfactory.Chinese patent CN 101121799A discloses a kind of polymer materials of being made up of polypropylene, polyethylene, peroxide cross-linking agent, mineral filler etc., effect by peroxide cross-linking agent in the melt blending process, it is crosslinked that the small PE particle that is dispersed in the PP matrix is produced, and forms small gel and be evenly distributed in the PP matrix.Gained polypropylene blending modified material surface gloss is lower, extinction effect is better, but toughness is lower, has limited its application at automotive upholstery.
In addition, the Japanese Patent spy opens 157607/1995 and discloses and comprise propene polymer, partial cross-linked thermoplastic elastomer and the polyolefin compositions of ethylene-propylene-conjugated diolefine ter-polymers, and comprise the composition (the Japanese Patent spy opens 192509/1994) of modified olefin resin and jelling agent, yet, for these compositions, though reached low-luster to a certain extent, but still not high enough, must carry out gel or crosslinking Treatment.In addition, also there is lack of homogeneity in they, is difficult to problems such as recycling.
Summary of the invention
The objective of the invention is in order to provide the high strong and unyielding property polypropylene composite material of a kind of low gloss to form and preparation method thereof.
The high strong and unyielding property polypropylene composite material of this low gloss, by following weight percent meter, it is formed and proportioning is:
Polypropylene 55～91
Mineral filler 0～25
Toughner POE 0～10
Nano imvite 1～5
PP-g-MAH 2～4
Oxidation inhibitor 0.1～1
Other auxiliary agents 0～1.
In the polypropylene composite material system that the present invention was suitable for:
Described polypropylene is that melt flow rate (MFR) is that (test condition: 230 ℃ * 2.16kg) block copolymerization propylene, the content of its comonomer ethene is between 4～10mol% for 5～45g/10min.
Described mineral filler is talcum powder, lime carbonate or their composition, and its particle size range is 1～10 micron.
Described toughner POE is linear ethylene-octene copolymer, and density is 0.86～0.90g/cm
3, melting index is 0.5～5g/10min (test condition: 190 ℃ * 2.16kg).
The percentage of grafting of described PP-g-MAH is 0.5～1.2%, and melting index is 5～30g/10min (test condition: 230 ℃ * 2.16kg).
Described oxidation inhibitor comprises primary antioxidant and auxiliary anti-oxidant, primary antioxidant can select for use hindered phenol or thioesters kind antioxidant as 3114,1010, DSTP wherein one or more; Auxiliary anti-oxidant can select for use the phosphorite kind antioxidant as 618,168 etc.; Other auxiliary agents of the present invention are pigment toners.
Described nano imvite is aluminum laminate (magnesium) silicate clay mineral, is the rice white powder, and smectite content reaches 96-98%, and average wafer row thickness is less than 20 nanometers, directly/and thickness rate reaches 200.
The preparation method of this polypropylene composite material, its step is as follows:
(1) takes by weighing raw material by above-mentioned weight proportion;
(2) polypropylene, mineral filler, toughner, nano imvite, PP-g-MAH, oxidation inhibitor or other additives were done in super mixer mixed 5～15 minutes;
(3) raw materials mixed is placed dual-screw-stem machine, through melt extruding, granulation, its technology is: 190～200 ℃ in a district, 200～210 ℃ in two districts, 210～220 ℃ in three districts, 205～215 ℃ in four districts; The residence time of whole extrusion is 1～2 minute, and pressure is 12～18MPa.
The present invention adds nano imvite, toughner in the basic components of polypropylene composite material, thereby prepares low gloss, high flexible polypropylene composite material just.
Advantage of the present invention is:
1, the present invention uses the proper amount of nano polynite in composite system, makes polypropylene compound material prepared have low-luster.
2, polypropylene compound material prepared of the present invention is when guaranteeing the material low gloss, and material has high rigidity, high tenacity.
3, the method preparation technology who improves polypropylene composite material low gloss performance of the present invention's proposition is simple, production cost is low.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
In embodiment and Comparative Examples composite-material formula, polypropylene is the block copolymerization propylene of Shanghai petrochemical iy produced, and commodity are called M2600R.The particle size range of described talcum powder, lime carbonate or their composition is 1～10 micron.Described toughner POE is linear ethylene-octene copolymer that E.I.Du Pont Company produces, and commodity are called 8180, and its density is 0.88～0.90g/cm
3, melting index is a 0.5g/10min (test condition: 190 ℃ * 2.16kg).Described nano imvite is aluminum laminate (magnesium) silicate clay mineral, is the rice white powder, and smectite content reaches 96-98%, and average wafer row thickness is less than 20 nanometers, directly/and thickness rate reaches 200.Described PP-g-MAH is the OREVAC CA100 that ARKEMA company produces, and its percentage of grafting is 1.0%, and melting index is a 18g/10min (test condition: 230 ℃ * 2.16kg).Described primary antioxidant is the DSTP that Britain ICE company produces, and trade names are Negonox DSTP, and chemical name is the thio-2 acid octadecyl ester, and Ciba company produce 3114, trade names are Irganox 3114, and chemical name is 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid.Auxiliary anti-oxidant is 168 of Ciba company product, and trade names are Irgafos 168, and chemical name is three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester.
Resin and various additive do to mix in super mixer 3～5 minutes, again in twin screw extruder through melt extruding, granulation, its technology is: 190～200 ℃ in a district, 200～210 ℃ in two districts, 210～220 ℃ in three districts, 205～215 ℃ in four districts; The whole extrusion residence time is 1～2 minute, and pressure is 12～18Mpa.
Performance evaluation mode and implementation standard:
With the particulate material for preparing as stated above, drying is 2～3 hours in 90～100 ℃ convection oven, and then the particulate material that drying is good carries out the injection molding sample preparation on injection moulding machine.
Glossiness test: try with 60 ° of angular measurements of vancometer by standard GB8807.
Melt flow rate (MFR) (MFR) is measured: undertaken by the ISO1183 standard, probe temperature is 230 ℃, load 2.16kg;
The tensile property test: undertaken by ISO 527-2 standard, specimen size is 170 * 10 * 4mm, and draw speed is 50mm/min;
The bending property test: undertaken by ISO 178 standards, specimen size is 80 * 10 * 4mm, and rate of bending is 2mm/min, and span is 64mm, and modulus in flexure is undertaken by tangential direction;
The simple beam impact strength test: undertaken by ISO 179 standards, specimen size is 80 * 6 * 4mm, and notch depth is 1/3rd of a sample thickness;
Comprehensive mechanical performance is passed judgment on by the numerical value of notched Izod impact strength, tensile strength, flexural strength and the modulus in flexure of test gained.
Example formulations and every The performance test results be each table as follows:
Table 1 embodiment 1-6 and Comparative Examples 1-3 material prescription table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 | |
| M2600R, weight % | 59.4 | 57.4 | 55.4 | 57.4 | 70.4 | 90.4 | 60.4 | 75.4 | 95.4 |
| Talcum powder, weight % | 25 | 25 | 25 | 25 | 15 | - | 25 | 15 | - |
| POE, weight % | 10 | 10 | 10 | 10 | 5 | - | 10 | 5 | - |
| PP-g-MAH, weight % | 4 | 4 | 4 | 2 | 4 | 4 | 4 | 4 | 4 |
| Nano imvite, weight % | 1 | 3 | 5 | 5 | 5 | 5 | - | - | - |
| 3114, weight % | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| DSTP, weight % | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| 168, weight % | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Black toner, weight % | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
The test result of each prescription is as follows:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 | |
| Melting index (g/10min) | 17.2 | 17.5 | 17.6 | 17.7 | 21.1 | 27.4 | 17.0 | 21.8 | 26 |
| Density (g/cm 3) | 1.081 | 1.083 | 1.090 | 1.090 | 1.041 | 0.939 | 1.079 | 1.010 | 0.905 |
| Notched Izod impact strength (kJ/m 2) | 21.8 | 21.0 | 20.2 | 20.8 | 19.6 | 7.8 | 22.0 | 23.1 | 8.2 |
| Tensile strength | 18.3 | 18.8 | 19.4 | 18.2 | 25.8 | 24.8 | 18.1 | 22.4 | 23.1 |
| ?(MPa) | |||||||||
| Modulus in flexure (MPa) | 1552 | 1590 | 1670 | 1564 | 1937 | 1320 | 1541 | 1780 | 1263 |
| Glossiness (dermatoglyph face) | 2.2 | 1.8 | 1.7 | 1.9 | 2.4 | 3.4 | 2.6 | 2.9 | 5.2 |
Contrast from embodiment 1,2,3,4 and Comparative Examples 1, the contrast of the contrast of embodiment 5 and Comparative Examples 2 and embodiment 6 and Comparative Examples 3 as can be seen, after adding nano imvite and PP-g-MAH, the glossiness of PP matrix material obviously reduces, and increase along with nano imvite and PP-g-MAH content, the glossiness of matrix material also constantly reduces, and glossiness can reach 1.7, and material has good toughness and rigidity simultaneously.
Claims (10)
1. the high strong and unyielding property polypropylene composite material of a low gloss, it is characterized in that: by weight percentage, it is formed and proportioning is:
Polypropylene 55～91
Mineral filler 0～25
Toughner POE 0～10
Nano imvite 1～5
PP-g-MAH 2～4
Oxidation inhibitor 0.1～1
Other auxiliary agents 0～1.
2. the high strong and unyielding property polypropylene composite material of low gloss according to claim 1, it is characterized in that: under the test condition of 230 ℃ * 2.16kg, polypropylene is that melt flow rate (MFR) is the block copolymerization propylene of 5～45g/10min, and the content of its comonomer ethene is between 4～10mol%.
3. the high strong and unyielding property polypropylene composite material of low gloss according to claim 1 is characterized in that: described mineral filler be in talcum powder and the lime carbonate one or both, its particle size range is 1～10 micron.
4. the high strong and unyielding property polypropylene composite material of low gloss according to claim 1, it is characterized in that: described toughner POE is linear ethylene-octene copolymer, density is 0.86～0.90g/cm
3, under the test condition of 190 ℃ * 2.16kg, melting index is 0.5～5g/10min.
5. the high strong and unyielding property polypropylene composite material of low gloss according to claim 1, it is characterized in that: the percentage of grafting of described PP-g-MAH is 0.5～1.2%, (under the test condition of 230 ℃ * 2.16kg, melting index is 5～30g/10min.
6. the high strong and unyielding property polypropylene composite material of low gloss according to claim 1, it is characterized in that: described oxidation inhibitor comprises primary antioxidant and auxiliary anti-oxidant, primary antioxidant is hindered phenol or thioesters kind antioxidant; Auxiliary anti-oxidant is the phosphorite kind antioxidant.
7. the high strong and unyielding property polypropylene composite material of low gloss according to claim 6 is characterized in that: described primary antioxidant 3114,1010, DSTP wherein one or more; Described auxiliary anti-oxidant is 618 or 168.
8. the high strong and unyielding property polypropylene composite material of low gloss according to claim 1, it is characterized in that: described nano imvite is aluminum laminate/magnesium silicate clay mineral, is the rice white powder, and smectite content reaches 96-98%, average wafer row thickness is less than 20 nanometers, directly/and thickness rate reaches 200.
9. the high strong and unyielding property polypropylene composite material of low gloss according to claim 1, it is characterized in that: described other auxiliary agents are the pigment toner.
10. method for preparing the described polypropylene composite material of claim 1, its step is as follows:
(1) takes by weighing raw material by above-mentioned weight proportion;
(2) polypropylene, mineral filler, toughner, nano imvite, PP-g-MAH, oxidation inhibitor or other additives were done in super mixer mixed 5～15 minutes;
(3) raw materials mixed is placed dual-screw-stem machine, through melt extruding, granulation, its technology is: 190～200 ℃ in a district, 200～210 ℃ in two districts, 210～220 ℃ in three districts, 205～215 ℃ in four districts; The residence time of whole extrusion is 1～2 minute, and pressure is 12～18MPa.
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| CN103113680A (en) * | 2013-02-20 | 2013-05-22 | 合肥杰事杰新材料股份有限公司 | Low-gloss polyolefin elastomer composite material and preparation method thereof |
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| WO2021130121A1 (en) | 2019-12-24 | 2021-07-01 | Sabic Global Technologies B.V. | Heterophasic propylene copolymer composition with low gloss |
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| CN102532704A (en) * | 2011-12-21 | 2012-07-04 | 上海普利特复合材料股份有限公司 | Liquid crystalline polymer reinforced polypropylene composite material and preparation method thereof |
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| CN102827424A (en) * | 2012-09-27 | 2012-12-19 | 马宁 | Polypropylene (PP) elastomer composition with high impact resistance and preparation method thereof |
| CN103113680A (en) * | 2013-02-20 | 2013-05-22 | 合肥杰事杰新材料股份有限公司 | Low-gloss polyolefin elastomer composite material and preparation method thereof |
| CN105542318A (en) * | 2015-12-30 | 2016-05-04 | 上海普利特复合材料股份有限公司 | Low-after-shrinkage modified polypropylene composite material and preparation method thereof |
| CN109735006A (en) * | 2018-12-27 | 2019-05-10 | 浙江普利特新材料有限公司 | A kind of low gloss, high-performance are thinning PP composite material and preparation method thereof |
| CN111019242A (en) * | 2019-12-23 | 2020-04-17 | 广东金发科技有限公司 | Impact-resistant, heat-resistant and flame-retardant MPP power pipe material and preparation method thereof |
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| CN114148062B (en) * | 2021-10-19 | 2023-01-17 | 安徽金田高新材料股份有限公司 | BOPP extinction transfer film and preparation method thereof |
| CN114539669A (en) * | 2022-03-08 | 2022-05-27 | 哈尔滨理工大学 | Nano modified blended polypropylene, preparation method and high-voltage cable |
| CN114672035A (en) * | 2022-03-18 | 2022-06-28 | 湖南工业大学 | Hyperbranched polymer delustering agent and preparation method and application thereof |
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Address after: 201703 12th Floor, Lane 1, 2855, Shanghai Qingping Highway, Zhaoxiang Town, Qingpu District, Shanghai Patentee after: Shanghai Pret Compound Material Co., Ltd. Address before: 200081 2nd Floor, 421 Lane, Siping Road, Hongkou District, Shanghai Patentee before: Shanghai Pret Compound Material Co., Ltd. |