CN116574328B - Polypropylene composite material and preparation method thereof - Google Patents
Polypropylene composite material and preparation method thereof Download PDFInfo
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- CN116574328B CN116574328B CN202310534692.7A CN202310534692A CN116574328B CN 116574328 B CN116574328 B CN 116574328B CN 202310534692 A CN202310534692 A CN 202310534692A CN 116574328 B CN116574328 B CN 116574328B
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- polypropylene composite
- polypropylene
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- butadiene rubber
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- -1 Polypropylene Polymers 0.000 title claims abstract description 38
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 36
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 35
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 239000005062 Polybutadiene Substances 0.000 claims abstract description 13
- 229920002857 polybutadiene Polymers 0.000 claims abstract description 13
- 239000012745 toughening agent Substances 0.000 claims abstract description 11
- 239000000155 melt Substances 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 239000012760 heat stabilizer Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 2
- VTJUKNSKBAOEHE-UHFFFAOYSA-N calixarene Chemical compound COC(=O)COC1=C(CC=2C(=C(CC=3C(=C(C4)C=C(C=3)C(C)(C)C)OCC(=O)OC)C=C(C=2)C(C)(C)C)OCC(=O)OC)C=C(C(C)(C)C)C=C1CC1=C(OCC(=O)OC)C4=CC(C(C)(C)C)=C1 VTJUKNSKBAOEHE-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 150000002989 phenols Chemical class 0.000 claims description 2
- 150000008301 phosphite esters Chemical class 0.000 claims description 2
- 150000007970 thio esters Chemical class 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 11
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 2
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000006224 matting agent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 208000003464 asthenopia Diseases 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- FTQWRYSLUYAIRQ-UHFFFAOYSA-N n-[(octadecanoylamino)methyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCNC(=O)CCCCCCCCCCCCCCCCC FTQWRYSLUYAIRQ-UHFFFAOYSA-N 0.000 description 1
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 108010038132 serratiopeptidase Proteins 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a polypropylene composite material and a preparation method thereof. According to the invention, cis-butadiene rubber with proper cis-structure ratio and viscosity is selected as a toughening agent, so that the material has good toughness, the crystal size of polypropylene can be reduced, and the polypropylene is effectively prevented from crystallizing, thereby reducing the glossiness of the product; in addition, the toughening agent butadiene rubber can be uniformly dispersed through the preferable dispersing agent, and the problem that the toughness of the material cannot be improved due to the fact that the poor dispersion size is too large is avoided, so that excellent rigidity-toughness balance is obtained.
Description
Technical Field
The invention belongs to the field of modified plastics, and particularly relates to a polypropylene composite material and a preparation method thereof.
Background
In recent years, along with rapid development of new energy vehicle types, higher requirements are put forward on light weight of the whole vehicle, and polypropylene materials are widely applied to inner and outer decoration pieces of the vehicle due to the characteristics of low density, excellent performance and the like, but the polypropylene materials are always subjected to the problems of easy initiation of visual fatigue and sight obstruction of drivers and passengers due to higher self-gloss.
Patent CN105647001a discloses a low-glossiness modified polypropylene material and a preparation method thereof, the invention reduces the glossiness of the modified polypropylene material and improves the toughness of products by using maleic anhydride grafted ethylene-octene copolymer, but the invention is limited by no filling material, and the prepared composite material has limited mechanical properties and cannot be widely applied to automobile part materials; the invention discloses a modified polypropylene material for automobile interior trim with low VOC, low gloss and low shrinkage and a preparation method thereof, wherein the gloss is reduced by adding an inorganic matting agent, and the prepared modified polypropylene material for automobile interior trim has low gloss, low shrinkage and excellent mechanical property and processability, but the inorganic matting agent is wollastonite which can cause a large amount of pits on the surface of a product to cause poor appearance, and the application range is limited.
Disclosure of Invention
The invention aims to provide a polypropylene composite material and a preparation method thereof, wherein the composite material can reduce the glossiness of a product and obtain excellent rigidity-toughness balance.
The invention provides a polypropylene composite material which comprises the following components in parts by mass:
Wherein the toughening agent is butadiene rubber, and the cis structure weight ratio is more than 95%.
The melt flow index of the polypropylene resin under the condition of 230 ℃/2.16kg (test standard: ISO 1133-1:2011) is 1-120g/10min.
Preferably, the cis structure weight ratio of the butadiene rubber is 96% -99%. The cis-butadiene rubber with high cis-form (the cis-form structure weight ratio is more than 95%) has better comprehensive mechanical properties, and has wider molecular weight and easier dispersion and processing compared with the cis-butadiene rubber with low cis-form structure. The cis structure weight ratio is tested according to the method of measuring infrared spectroscopy of SHT 1727-2017 butadiene rubber microstructure.
The cis structure is that two substituents are on the same side, and the following structural formula is shown:
the filler is 1250-5000 mesh talcum powder.
The structural formula of the dispersing agent is shown in the formula (I);
Wherein n=15-50, R 1 are each independently selected from C20-C22 alkyl groups, R 2 are each independently selected from C16-C18 alkyl groups; or the dispersant is a polyester-based dispersant.
The heat stabilizer is at least one of phenols, amines, phosphite ester, compound of acryl functional group and thioester and calixarene heat stabilizer.
Preferably, the composition comprises the following components in parts by weight:
The invention provides a preparation method of a polypropylene composite material, which comprises the following steps:
Adding the components into a mixer for mixing to obtain a material; extruding and granulating the material by an extruder to obtain the polypropylene composite material.
The extrusion temperature is 120-220 ℃, and the length-diameter ratio of the extruder is 30-48:1.
The invention provides an application of a polypropylene composite material in automotive ornaments, in particular to automotive interior parts such as instrument panels, door panels, upright posts and the like.
Advantageous effects
According to the invention, the high cis-butadiene rubber is selected as the toughening agent, so that the material has good toughness, the crystal size of polypropylene can be reduced, and the polypropylene is effectively prevented from crystallizing, thereby reducing the glossiness of the product; in addition, the toughening agent butadiene rubber can be uniformly dispersed through the preferable dispersing agent, and the problem that the toughness of the material cannot be improved due to the fact that the poor dispersion size is too large is avoided, so that excellent rigidity-toughness balance is obtained.
Detailed Description
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The reagents, methods and apparatus employed in the present invention, unless otherwise specified, are all conventional in the art.
The following examples and comparative examples were prepared from the following raw materials:
Polypropylene resin 1: the melt flow index under the conditions of EP548R,230 ℃/2.16kg (test standard: ISO 1133-1:2011) is 25g/10min, sea shell in the manufacturer.
Polypropylene resin 2: the melt flow index of the PP PPB-M02D under the condition of 230 ℃/2.16kg (test standard: ISO 1133-1:2011) is 1.5g/10min, and the manufacturer flourishes.
Polypropylene resin 3: the melt flow index under the conditions of EP640V,230 ℃ C./2.16 kg (test standard: ISO 1133-1:2011) is 105g/10min, sea shell in the manufacturer.
Toughening agent 1: butadiene rubber: yanshan petrochemical BR9000, 97% cis structure, mooney viscosity 43; jinzhou petrochemical BR9100-41, mooney viscosity 41, cis-structure 98%; jinzhou petrochemical BR9100-53, mooney viscosity 53, cis structure 96%; qilu petrochemical BR9002, 99% of cis structure and 34% of Mooney viscosity; dushan mountain petrochemical LCBR P30AF with 35% cis structure and 30 Mooney viscosity;
toughening agent 2: ethylene octene copolymer: brand DF610, manufacturer Dow chemical.
Filler: talc TYT-777A of 3000 mesh, manufacturer adds source chemical industry.
Dispersant 1: the brand number Armowax W-440 is shown in the formula (I) and is manufactured by AKZO NOBEL.
Wherein in formula (I), n=45, R 1 =c20 alkyl, and R 2 =c16 alkyl.
Dispersant 2: polyester dispersant, trade mark Solplus DP310,310, manufacturer's uk road rinse.
Dispersant 3: ethylene bis stearamide, EBS, manufacturer Shanghai dasen.
Thermal stabilization aids: the antioxidant is composed of an antioxidant 1 and an antioxidant 2 (the mass ratio is 1:1), wherein the antioxidant 1 is hindered phenol antioxidant 1010 (tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester); the antioxidant 2 is phosphite antioxidant 168 (tris [2, 4-di-tert-butylphenyl ] phosphite), and the same species are used in parallel experiments.
The composite materials of each example and comparative example were prepared by the following procedure:
Putting the components into a mixer, and mixing for 1-3min to obtain a uniformly mixed state, thereby obtaining a uniformly mixed material; extruding and granulating the uniformly mixed materials through a double-screw extruder to obtain the composite material. The conditions of melt extrusion were: the temperature of the first area is 120-180 ℃, the temperature of the second area is 180-200 ℃, the temperature of the third area is 200-220 ℃, the temperature of the fourth area is 200-220 ℃, the temperature of the fifth area is 200-220 ℃, the temperature of the sixth area is 200-220 ℃, the temperature of the seventh area is 200-230 ℃, the temperature of the eighth area is 200-220 ℃, the temperature of the ninth area is 200-220 ℃, and the rotating speed of a host is 250-600r/min; the length-diameter ratio of the twin-screw extruder is (30-48): 1.
Examples and comparative examples were subjected to the following test methods or test criteria:
1. flexural modulus test, test according to standard ISO 178-2010, spline dimensions: 80 x 10 x 4, test conditions:
The bending speed is 2mm/min at 23 ℃, the higher the strength is, the better the rigidity of the material is, and the use of the material is affected if the strength is too low;
2. Cantilever notched impact strength test, test according to standard ISO 180-2019, V-notch, spline size: 80 x 10 x4, test conditions: the pendulum energy is 4J at 23 ℃, the unit KJ/m 2 is that the higher the strength is, the better the toughness of the material is, and the use of the material is affected if the strength is too low;
3. Gloss testing, according to standard ASTM-D2457, test angle 60 degrees, using a mass skin plate (skin number K4T); the lower the gloss value, the more satisfactory the low gloss material usage requirements.
Table 1 example formulation and test results thereof
Table 2 comparative example formulation and test results thereof
As can be seen from tables 1 and 2, the polypropylene composite material of the invention has the glossiness of 1.3-1.7, the rigidity and the toughness, the flexural modulus of 1345MPa or more and the notch impact strength of 22.5MPa or more. As can be seen from comparative examples 1 and 2, when the cis structure ratio of the conventional toughening agent or butadiene rubber is not satisfactory, the rigidity and toughness of the obtained material are not satisfactory. Comparative example 1 and comparative example 3 can see that the material toughness is poor when no toughening agent is added. Comparative example 1 and comparative example 4 can be seen that the material rigidity is poor when no dispersant is added. Comparative example 1 and comparative examples 5, 6 can see that when the toughening agent is added too much or the dispersing agent is added too much, the properties of the material are not satisfactory.
Claims (10)
1. A polypropylene composite material characterized by: the coating comprises the following components in parts by weight:
Wherein the toughening agent is butadiene rubber, and the cis structure weight ratio is more than 95%; the dispersing agent is a polyester dispersing agent.
2. The polypropylene composite according to claim 1, wherein: the melt flow index of the polypropylene resin under the condition of 230 ℃/2.16kg is 1-120g/10min.
3. The polypropylene composite according to claim 1, wherein: the cis structure weight ratio of the butadiene rubber is 96% -99%.
4. The polypropylene composite according to claim 1, wherein: the filler is 1250-5000 mesh talcum powder.
5. The polypropylene composite according to claim 1, wherein: the structural formula of the dispersing agent is shown in the formula (I);
Wherein n=15-50, R 1 are each independently selected from C20-C22 alkyl groups, and R 2 are each independently selected from C16-C18 alkyl groups.
6. The polypropylene composite according to claim 1, wherein: the heat stabilizer is at least one of phenols, amines, phosphite ester, compound of acryl functional group and thioester and calixarene heat stabilizer.
7. The polypropylene composite according to claim 1, wherein: the composite material comprises the following components in parts by weight:
8. a process for the preparation of a polypropylene composite as claimed in any one of claims 1 to 7, comprising the steps of:
Adding the components into a mixer for mixing to obtain a material; extruding and granulating the material by an extruder to obtain the polypropylene composite material.
9. The method of manufacturing according to claim 8, wherein: the extrusion temperature is 120-220 ℃, and the length-diameter ratio of the extruder is 30-48:1.
10. Use of a polypropylene composite according to any one of claims 1 to 7 in automotive trim.
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| CN116574328B true CN116574328B (en) | 2024-08-23 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716764A (en) * | 2022-03-30 | 2022-07-08 | 江苏金发科技新材料有限公司 | Polypropylene composite material and preparation method and application thereof |
| CN115558204A (en) * | 2022-09-27 | 2023-01-03 | 金旸（厦门）新材料科技有限公司 | Low-shrinkage high-gloss V0-grade halogen-free flame-retardant polypropylene composite material and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB943366A (en) * | 1961-01-30 | 1963-12-04 | Shell Int Research | Improved polypropylene product |
| DE1570315A1 (en) * | 1965-11-19 | 1970-01-22 | Basf Ag | Process for the production of propylene polymers by copolymerizing propylene with butadiene |
| IT1274746B (en) * | 1994-08-30 | 1997-07-24 | Enichem Elastomers | VULCANIZED POLYOLEFINIC PLASTOELASTOMERIC COMPOSITION AND PROCEDURE FOR ITS PREPARATION |
| CN104817769A (en) * | 2015-04-22 | 2015-08-05 | 重庆交通大学 | Novel bumper material and automobile bumper thereof |
| CN109575427A (en) * | 2017-09-29 | 2019-04-05 | 合肥杰事杰新材料股份有限公司 | A kind of low-luster polypropylene composite material and preparation method thereof |
| CN113185776A (en) * | 2021-05-31 | 2021-07-30 | 宁夏大学 | Polypropylene-based composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716764A (en) * | 2022-03-30 | 2022-07-08 | 江苏金发科技新材料有限公司 | Polypropylene composite material and preparation method and application thereof |
| CN115558204A (en) * | 2022-09-27 | 2023-01-03 | 金旸（厦门）新材料科技有限公司 | Low-shrinkage high-gloss V0-grade halogen-free flame-retardant polypropylene composite material and preparation method thereof |
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