CN116063789A - Heterophasic polypropylene composition, and preparation method and application thereof - Google Patents

Heterophasic polypropylene composition, and preparation method and application thereof Download PDF

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Publication number
CN116063789A
CN116063789A CN202111285548.1A CN202111285548A CN116063789A CN 116063789 A CN116063789 A CN 116063789A CN 202111285548 A CN202111285548 A CN 202111285548A CN 116063789 A CN116063789 A CN 116063789A
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polypropylene composition
component
composition according
heterophasic polypropylene
ethylene
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刘宣伯
罗春霞
任敏巧
张龙贵
张韬毅
宋文波
邹发生
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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    • 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
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F110/04—Monomers containing three or four carbon atoms
    • C08F110/06—Propene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers

Abstract

The invention belongs to the technical field of polymers, and discloses a multiphase polypropylene composition, a preparation method and application thereof, wherein the polypropylene composition comprises the following components: component a: the isotactic pentad fraction of the high-isotacticity high-crystallization homo-polypropylene is above 98%, and the melt index of the high-isotacticity high-crystallization homo-polypropylene under the conditions of 230 ℃ and 2.16kg load is 200-300g/10min; component b: copolymers of ethylene and propylene, which are xylene soluble at room temperature, contain 25-32% by weight of ethylene comonomer and have a weight average molecular weight of 450-700kg/mol. The polypropylene composition has high fluidity and good rigidity-toughness balance property.

Description

Heterophasic polypropylene composition, and preparation method and application thereof
Technical Field
The invention belongs to the technical field of polymers, and particularly relates to a heterophasic polypropylene composition, a preparation method of the heterophasic polypropylene composition and application of the heterophasic polypropylene composition in injection molding products.
Background
The high-flow impact polypropylene resin is a resin material with excellent comprehensive properties, and is widely applied to various fields, especially injection molding products.
Impact polypropylene resins are a class of multicomponent materials whose properties are determined by the characteristics of the components themselves and their synergy. The prior art generally increases impact strength by increasing the rubber content, i.e. the room temperature xylene solubles (XCS), but an increase in XCS results in a decrease in stiffness. The flowability of a material is directly related to the molecular weight, and can be increased by decreasing the molecular weight of the material. The overall flowability of the material meets the rule of addition of the flowability of each component, so that the molecular weight of one or both components needs to be reduced to further improve the overall flowability of the material. If the molecular weight of the matrix PP is reduced to a certain degree, the problem of mechanical property reduction is brought; similar problems are also caused when the molecular weight of the rubber phase is reduced to a certain extent, so that in practical cases, the balance between fluidity and mechanical properties is often considered. The phase morphology of the rubber phase, i.e. the influence of the shape and size of the dispersed phase particles on the material properties is also obvious, and in general, the morphology of the rubber phase can be regulated by adjusting the composition of the rubber phase, i.e. the kind and content of the comonomer and the viscosity ratio of the rubber phase/matrix phase; the stiffness and toughness can also be adjusted by changing the matrix phase composition, for example, when the matrix is used or contains a certain amount of copolymerized polypropylene, the impact strength can be improved, but this can simultaneously reduce the heat resistance and the stiffness of the material.
Patent document CN104781336B discloses a polypropylene composition comprising a polypropylene homopolymer matrix phase and an ethylene propylene copolymer rubber phase, XCS in an amount of 4-14% by weight and having a Melt Flow Rate (MFR) of 4-8g/10min, which patent document is low, which ensures that the stiffness of the material is at a high level, but in order to ensure impact strength the molecular weight of the components is increased, so that the flowability of the product is not high. Patent document CN105452365B discloses a polyolefin composition comprising two heterophasic propylene copolymers, wherein in one of the heterophasic copolymers the polypropylene homopolymer has an MFR of 10-400g/10min and an xcs intrinsic viscosity of 3.7-9.0dL/g. In this patent document, to achieve a more balanced performance, two different XCS components and a matrix resin have to be added, wherein XCS has different intrinsic viscosity.
Disclosure of Invention
The invention aims to provide a multiphase polypropylene composition, a preparation method and application thereof, and the multiphase polypropylene composition has high fluidity and better rigidity-toughness balance characteristic.
In a first aspect the present invention provides a heterophasic polypropylene composition comprising the following components:
component a: the isotactic pentad fraction of the high-isotacticity high-crystallization homo-polypropylene is above 98%, and the melt index of the high-isotacticity high-crystallization homo-polypropylene under the conditions of 230 ℃ and 2.16kg load is 200-300g/10min;
component b: copolymers of ethylene and propylene, which are xylene soluble at room temperature, contain 25-32% by weight of ethylene comonomer and have a weight average molecular weight of 450-700kg/mol.
The second aspect of the present invention provides a process for preparing the heterophasic polypropylene composition described above, comprising: is prepared by multistage continuous polymerization in the presence of a Ziegler-Natta catalyst system; or from a mechanical blend of component a and component b.
In a third aspect the present invention provides the use of the heterophasic polypropylene composition as described above in injection molded articles.
The multiphase polypropylene composition has high fluidity and good rigidity-toughness balance characteristic, and the components are simple and easy to obtain, so that the multiphase polypropylene composition can be widely used for injection molding products.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
FIG. 1 is a graph of Dynamic Mechanical Analysis (DMA) loss factor versus temperature for polypropylene compositions of example 1 and comparative example 1.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the polypropylene composition of example 1.
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of the polypropylene composition of comparative example 1.
FIG. 4 is a Differential Scanning Calorimetry (DSC) temperature rise profile of the polypropylene compositions of example 1 and comparative example 2.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
According to a first aspect of the present invention there is provided a heterophasic polypropylene composition comprising the following components:
component a: the isotactic pentad fraction of the high-isotacticity high-crystallization homo-polypropylene is above 98%, and the melt index of the high-isotacticity high-crystallization homo-polypropylene under the conditions of 230 ℃ and 2.16kg load is 200-300g/10min;
component b: copolymers of ethylene and propylene, which are xylene soluble at room temperature, contain 25-32% by weight of ethylene comonomer and have a weight average molecular weight of 450-700kg/mol.
In the present invention, the content of component a is 70 to 80% by weight and the content of component b is 20 to 30% by weight based on the total weight of the polypropylene composition.
According to the invention, component a is the matrix and component b is the rubber dispersed phase, component b being spherically dispersed in component a, the average diameter of the spherical component b being less than 1 μm.
In the invention, the half-peak width of the transition peak of the component b exceeds 20 ℃ in the dynamic mechanical analysis loss factor-temperature curve of the polypropylene composition.
According to the present invention, the polypropylene composition has a cold crystallization peak on the differential scanning calorimetry heating curve.
According to a second aspect of the present invention, there is provided a process for the preparation of the heterophasic polypropylene composition as described above, comprising: is prepared by multistage continuous polymerization in the presence of a Ziegler-Natta catalyst system; or from a mechanical blend of component a and component b.
In the present invention, the multistage continuous polymerization reaction comprises: the homo-polypropylene is polymerized in one or more reactors and the copolymer of ethylene and propylene is prepared in another one or more reactors. The mass comprising the Ziegler-Natta catalytic system flows between the different reactors until a composition comprising component a and component b is obtained. The Ziegler-Natta catalyst system used for the polymerization may be chosen with reference to the prior art. The polymerization process can be carried out by methods conventional in the art, such as prepolymerization, liquid phase polymerization, gas phase polymerization, specific parameters being conventionally selected with reference to the prior art.
According to the invention, mechanical blending may be achieved by extrusion pelletization, and the melt blending temperature of the components during pelletization may be the blending temperature used in usual polypropylene processing, and should be selected within a range that ensures complete melting of the polypropylene matrix without decomposition thereof, typically 180-240 ℃.
In a third aspect the present invention provides the use of the heterophasic polypropylene composition as described above in injection molded articles.
In the preparation of injection-molded articles, conventional additives such as antioxidants, nucleating agents, lubricants and the like are required to be added, and the respective additives can be specifically selected according to the needs, and the conventional amounts are also used.
The substances and parameters not defined in the present invention can be selected according to the prior art, and are conventional in the art.
The invention will be further illustrated with reference to the following examples. But are not limited by these examples.
In the following examples and comparative examples, the data were obtained as follows:
1. average diameter of dispersed phase rubber particles (average diameter of spherical component b):
the weight average value is calculated according to the following calculation formula:
Figure BDA0003332563850000041
wherein d w Represents the weight average diameter, d, of the dispersed phase particles i Represents the diameter of the ith particle, i is the particle number, n i Is of diameter d i And N is the number of particles.
2. Room temperature xylene solubles (XCS) content (content of component b): measured according to ASTM D5492-98.
3. Melt index (MFR): measured according to ISO1133 at 230℃under a load of 2.16 kg.
4. Weight average molecular weight: the molecular weight of the sample was measured by using a PL-GPC 220 gel permeation chromatograph manufactured by UK Polymer Laboratories company, the chromatographic column was 3 tandem Plgel 10 μm MIXED-B columns, the solvent and mobile phase were 1,2, 4-trichlorobenzene (containing 0.3g/1000mL antioxidant 2, 6-dibutyl-p-cresol), the column temperature was 150℃and the flow rate was 1.0mL/min, and the universal calibration was performed by using a PL company EasiCal PS-1 narrow distribution polystyrene standard.
5. The isotactic pentad fraction (mmmm) and the ethylene comonomer content (C2 inXCS) in XCS were measured by nuclear magnetic resonance, using a Bruker company AVANCEIII MHz nuclear magnetic resonance spectrometer, 10mm probe, with deuterated orthodichlorobenzene as the solvent. About 200mg of sample per 2.5mL of solvent, the sample tube was heated in an oil bath at 130-140℃until the sample dissolved to form a homogeneous solution. The test conditions were: the probe temperature was 125 ℃,90 ° pulse, sampling time AQ was 5 seconds, and delay time D1 was 10 seconds.
6. The morphology of the sample was observed with a Hitachi S-4800-model scanning electron microscope.
7. Flexural modulus of the material was measured according to GB/T9341 and Charpy simply supported beam notched impact strength was measured according to GB/T1043.1-2008.
Each of the above tests was performed at ambient conditions, unless otherwise indicated.
Examples 1-3 illustrate heterophasic polypropylene compositions of the invention and methods of making the same.
Example 1
Into a 300mL glass reaction flask, 90mL TiCl was introduced 4 Cooling to-20deg.C, adding 37mmol of magnesium halide carrier (prepared according to the method disclosed in example 1 of CN 1330086A) calculated as magnesium element, heating to 110deg.C, adding 0.3mmol of tributyl phosphate and 7.3mmol of 2-isopropyl-1, 3-dimethylpropane during heating, maintaining at 110deg.C for 30min, filtering to remove liquid, and using TiCl 4 Washing for 2 times, washing with hexane for 5 times, and vacuum drying to obtain the catalyst component CAT-A for olefin polymerization.
The weight content of phosphorus in the catalyst component for olefin polymerization, calculated as phosphorus element, was 0.11%, as measured by X-ray fluorescence spectrometry.
The polymerization was carried out on a set of polypropylene pilot plants.
The polymerization method comprises the following steps:
prepolymerization: the main catalyst CAT-A, the cocatalyst Triethylaluminum (TEAL) and the external electron donor dipiperidinyldimethylsilane are continuously added into a prepolymerization reactor after the pre-contact reaction is carried out at 10 ℃ for 20min, the triethylaluminum flow is 6g/hr, the dipiperidinyldimethylsilane flow is 1.0g/hr, and the main catalyst flow is 0.36g/hr. The prepolymerization is carried out in a liquid phase bulk environment of propylene at a temperature of 15℃and a residence time of about 4min.
The catalyst after prepolymerization continuously enters a loop reactor (liquid phase reactor), propylene homopolymerization reaction is completed in the loop reactor, the temperature of the loop polymerization reaction is 70 ℃, the reaction pressure is 4.0MPa, hydrogen is added into the feed of the loop reactor, and the concentration of the hydrogen detected by on-line chromatography is 0.95mol percent.
After the loop reactor is reacted, the obtained material enters a fluidized bed gas phase reactor to carry out copolymerization reaction of ethylene and propylene. The gas phase reaction temperature was 75 ℃, the reaction pressure was 0.65MPa, wherein the molar ratio of ethylene/(propylene+ethylene) =0.27, a certain amount of hydrogen was added to the gas phase reactor feed, and the hydrogen concentration in the recycle gas of the gas phase reactor was 0.44mol% as measured by on-line chromatography.
The specific process conditions are shown in table 1.
The polymer obtained by the reaction is subjected to degassing and wet nitrogen deactivation treatment to obtain the polypropylene composition.
The powder obtained by polymerization was added with 0.1 wt% of IRGAFOS 168 additive, 0.1 wt% of IRGANOX1010 additive, 0.05 wt% of calcium stearate and 0.25 wt% of VP101B nucleating agent, and pelletized by a twin-screw extruder. The injection molding machine prepares injection molded samples conforming to the GB standard and determines their physical properties. The measurement results are shown in Table 2.
Example 2
The main catalyst, cocatalyst, external donor, pre-complexation and polymerization process conditions used in example 2 were the same as in example 1. The difference from example 1 is that: the hydrogen concentration in the loop reactor was 0.80mol%; the reaction pressure in the gas phase fluidized bed reactor was 0.63MPa, the molar ratio of ethylene/(propylene+ethylene) was=0.29, and the hydrogen concentration in the recycle gas of the gas phase reactor was 0.33mol% as measured by on-line chromatography. Specific process conditions are shown in Table 1, and measured physical properties are shown in Table 2.
Example 3
The procatalyst, cocatalyst, external donor, pre-complexation and polymerization process conditions used in example 3 were the same as in example 1. The difference from example 1 is that: the hydrogen concentration in the loop reactor was 0.70mol%; the reaction pressure in the gas phase fluidized bed reactor was 0.62MPa, the ethylene/(propylene+ethylene) molar ratio=0.33, and the hydrogen concentration in the recycle gas of the gas phase reactor was 0.25mol% as measured by on-line chromatography. Specific process conditions are shown in Table 1, and measured physical properties are shown in Table 2.
Comparative example 1
The procatalyst, cocatalyst, pre-complexation and polymerization process conditions used in comparative example 1 were the same as in example 1. The difference from example 1 is that: the external electron donor is cyclohexyl methyl dimethoxy silane; the hydrogen concentration in the loop reactor was 0.45mol%; the reaction pressure in the gas phase fluidized bed reactor was 0.61MPa, the molar ratio of ethylene/(propylene+ethylene) was=0.52, and the hydrogen concentration in the recycle gas of the gas phase reactor was 0.55mol% as measured by on-line chromatography. Specific process conditions are shown in Table 1, and measured physical properties are shown in Table 2.
Comparative example 2
The procatalyst, cocatalyst, pre-complexation and polymerization process conditions used in comparative example 2 were the same as in example 1. The difference from example 1 is that: the external electron donor is dicyclopentyl dimethoxy silane; the hydrogen concentration in the loop reactor was 0.50mol%; the reaction pressure in the gas phase fluidized bed reactor was 0.62MPa, the molar ratio of ethylene/(propylene+ethylene) =0.34, and the hydrogen concentration in the recycle gas of the gas phase reactor was 0.67mol% as measured by on-line chromatography. Specific process conditions are shown in Table 1, and measured physical properties are shown in Table 2.
TABLE 1
Figure BDA0003332563850000081
TABLE 2
Figure BDA0003332563850000082
As can be seen from tables 1 and 2, the polypropylene composition of the present invention has high fluidity and excellent balance between rigidity and toughness. In example 1, compared with comparative example 1, XCS was similar, the melt index was higher, the impact strength was significantly improved, and the decrease in rigidity was relatively small, whereas in example 1, compared with comparative example 2, XCS was similar, the melt index was higher, the rigidity was unchanged, and the impact strength was improved. In examples 2 and 3, the melt fingers were lowered and the rigidity was lowered as compared with example 1, but the impact strength was significantly improved, and the properties were significantly improved as compared with comparative examples, and the balance of rigidity and toughness and the flowability were better.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.

Claims (9)

1. A heterophasic polypropylene composition, characterized in that the polypropylene composition comprises the following components:
component a: the isotactic pentad fraction of the high-isotacticity high-crystallization homo-polypropylene is above 98%, and the melt index of the high-isotacticity high-crystallization homo-polypropylene under the conditions of 230 ℃ and 2.16kg load is 200-300g/10min;
component b: copolymers of ethylene and propylene, which are xylene soluble at room temperature, contain 25-32% by weight of ethylene comonomer and have a weight average molecular weight of 450-700kg/mol.
2. Heterophasic polypropylene composition according to claim 1, wherein component a is present in an amount of from 70 to 80 wt% and component b is present in an amount of from 20 to 30 wt%, based on the total weight of the polypropylene composition.
3. Heterophasic polypropylene composition according to claim 1, wherein component b is spherically dispersed in component a, the average diameter of the spherical component b being below 1 μm.
4. Heterophasic polypropylene composition according to claim 1, wherein the transition peak half-width of component b in the dynamic mechanical analysis loss factor-temperature curve of the polypropylene composition exceeds 20 ℃.
5. The heterophasic polypropylene composition according to claim 1, wherein the polypropylene composition has a cold crystallization peak on the differential scanning calorimetry heating profile.
6. A process for the preparation of a heterophasic polypropylene composition according to any of claims 1 to 5, wherein the process comprises: is prepared by multistage continuous polymerization in the presence of a Ziegler-Natta catalyst system; or from a mechanical blend of component a and component b.
7. The method for preparing a heterophasic polypropylene composition according to claim 6, wherein the multistage continuous polymerization comprises: the homo-polypropylene is polymerized in one or more reactors and the copolymer of ethylene and propylene is prepared in another one or more reactors.
8. The process for preparing a heterophasic polypropylene composition according to claim 6, wherein the mechanical blending comprises extrusion pelletization, the melt blending temperature of the components during pelletization being 180-240 ℃.
9. Use of the heterophasic polypropylene composition according to any of claims 1 to 5 in injection molded articles.
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CN102203178A (en) * 2008-10-29 2011-09-28 北欧化工公司 Tough composition for food applications
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CN104558811A (en) * 2013-10-10 2015-04-29 中国石油化工股份有限公司 Polypropylene composition, and preparation method and application thereof
CN105330957A (en) * 2014-08-12 2016-02-17 中国石油化工股份有限公司 Polypropylene composition and preparation method thereof
CN106674722A (en) * 2015-11-06 2017-05-17 中国石油化工股份有限公司 Polypropylene blow-molding membrane and preparation method thereof
CN106715632A (en) * 2014-08-21 2017-05-24 陶氏环球技术有限责任公司 Hot melt adhesive composition including a crystalline block composite
CN109422958A (en) * 2017-09-05 2019-03-05 中国石油化工股份有限公司 A kind of high flowing high-rigidity high-ductility polyolefin composition and preparation method thereof
CN109422959A (en) * 2017-09-05 2019-03-05 中国石油化工股份有限公司 A kind of impact polypropylene composition and preparation method thereof

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101511929A (en) * 2006-08-15 2009-08-19 埃克森美孚化学专利公司 Plasticized hetero-phase polyolefin blends
CN102203178A (en) * 2008-10-29 2011-09-28 北欧化工公司 Tough composition for food applications
EP2338656A1 (en) * 2009-12-23 2011-06-29 Borealis AG Heterophasic polypropylene with improved balance between stiffness and transparency
CN104448537A (en) * 2013-09-18 2015-03-25 中国石油化工股份有限公司 Polypropylene composition and preparation method thereof and products made from polypropylene composition
CN104558811A (en) * 2013-10-10 2015-04-29 中国石油化工股份有限公司 Polypropylene composition, and preparation method and application thereof
CN105330957A (en) * 2014-08-12 2016-02-17 中国石油化工股份有限公司 Polypropylene composition and preparation method thereof
CN106715632A (en) * 2014-08-21 2017-05-24 陶氏环球技术有限责任公司 Hot melt adhesive composition including a crystalline block composite
CN106674722A (en) * 2015-11-06 2017-05-17 中国石油化工股份有限公司 Polypropylene blow-molding membrane and preparation method thereof
CN109422958A (en) * 2017-09-05 2019-03-05 中国石油化工股份有限公司 A kind of high flowing high-rigidity high-ductility polyolefin composition and preparation method thereof
CN109422959A (en) * 2017-09-05 2019-03-05 中国石油化工股份有限公司 A kind of impact polypropylene composition and preparation method thereof

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