CN114031846A - Polypropylene composition with low plastic deformation and high elastic recovery, and preparation method and application thereof - Google Patents

Polypropylene composition with low plastic deformation and high elastic recovery, and preparation method and application thereof Download PDF

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CN114031846A
CN114031846A CN202111335457.4A CN202111335457A CN114031846A CN 114031846 A CN114031846 A CN 114031846A CN 202111335457 A CN202111335457 A CN 202111335457A CN 114031846 A CN114031846 A CN 114031846A
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polypropylene composition
parts
poe
uhmwpe
plastic deformation
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CN114031846B (en
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丁明笃
陈平绪
叶南飚
杨霄云
陆湛泉
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Kingfa Science and Technology Co Ltd
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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
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/24—Crystallisation aids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/06—Properties of polyethylene
    • C08L2207/068—Ultra high molecular weight polyethylene
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

Abstract

The invention discloses a polypropylene composition with low plastic deformation and high elastic recovery, a preparation method and application thereof. The polypropylene composition comprises the following components in parts by weight: 70-80 parts of PP, 5-10 parts of POE, 5-10 parts of UHMWPE, 1-2 parts of sorbitol nucleating agent and 0-5 parts of other auxiliary agents; the content of octene in POE is more than or equal to 20%, and the number average molecular weight of UHMWPE is more than or equal to 100 ten thousand. POE forms a sea-island structure with large particle size in the PP matrix, limits the movement of PP molecular chains and provides potential energy for the resilience of subsequent materials; the UHMWPE promotes entanglement of internal molecular segments within the polypropylene composition; the sorbitol nucleating agent provides more heterogeneous nucleation points for PP, and effectively improves the elastic recovery capability of the material. Through the synergistic effect of POE, UHMWPE, sorbitol nucleating agent and PP, the polypropylene composition has extremely low plastic deformation and excellent elastic recovery performance.

Description

Polypropylene composition with low plastic deformation and high elastic recovery, and preparation method and application thereof
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polypropylene composition with low plastic deformation and high elastic recovery, and a preparation method and application thereof.
Background
The polypropylene material is widely applied to the aspects of automobile industry, household appliances, sports equipment and the like. For components such as an electric appliance switch and the like, the switch operation is performed for a long time, and the materials are required to have excellent elastic recovery performance (also called resilience) in the opening and closing process so as to avoid the hidden danger of using the household appliance in the opening process; meanwhile, the low plastic deformation is required to be ensured in the long-term repeated opening and closing process.
At present, the following two methods are mainly used for improving the elastic recovery performance of polypropylene materials: (1) inorganic fillers such as mineral fillers and glass fibers are filled in the high-modulus polypropylene material, so that the material can quickly rebound after deformation; however, the method is only suitable for the condition of low deformation amount, and the rebound performance is poor for the use scene with large deformation amount; (2) adding an elastomer into a polypropylene material for toughening, so that after the material is impacted by external force, the impact of the external force is buffered by a larger deformation amount, and the material gradually returns to a state close to the state before deformation; however, the material deformed by the method can not completely recover the initial state, and after long-term repeated deformation, the plastic deformation is increased, and the plastic deformation part is converted into permanent deformation, so that the rebound performance is attenuated.
Therefore, it is desired to develop a polypropylene composition having both low plastic deformation and high elastic recovery.
Disclosure of Invention
The invention provides a polypropylene composition with low plastic deformation and high elastic recovery for overcoming the defects of high plastic deformation and poor elastic recovery in the prior art, POE forms a sea-island structure with large particle size in a PP matrix, limits the movement of PP molecular chains, avoids plastic deformation caused by slippage of amorphous region molecular chain segments, and provides potential energy for the recovery of subsequent materials; the UHMWPE promotes entanglement of the sub-segments within the polypropylene composition, so that the material is still under elastic deformation in case of large deformation quantities; the sorbitol nucleating agent provides more heterogeneous nucleation points for PP, simultaneously avoids forming imperfect lamella, and effectively improves the elastic recovery capability of the material. Through the synergistic effect of POE, UHMWPE, sorbitol nucleating agent and PP, the polypropylene composition disclosed by the invention has extremely low plastic deformation and excellent elastic recovery performance.
Another object of the present invention is to provide a process for preparing the polypropylene composition having low plastic deformation and high elastic recovery.
The invention also aims to provide the application of the polypropylene composition with low plastic deformation and high elastic recovery in preparing automobile parts, household appliance switches and sports equipment parts.
In order to solve the technical problems, the invention adopts the technical scheme that:
a polypropylene composition with low plastic deformation and high elastic recovery comprises the following components in parts by weight:
70-80 Parts of Polypropylene (PP),
5-10 parts of ethylene-octene copolymer (POE),
5-10 parts of ultrahigh molecular weight polyethylene (UHMWPE),
1-2 parts of a sorbitol nucleating agent,
0-5 parts of other auxiliary agents;
the content of octene in POE is more than or equal to 20 wt.%, and the number average molecular weight of UHMWPE is more than or equal to 100 ten thousand.
In the polypropylene composition system, the viscosity difference between the PP and the POE is utilized, so that the POE exists in a large-size island phase in a continuous phase of the polypropylene, and the existence of the POE island phase can provide good steric hindrance, thereby limiting the movement of a PP molecular chain and effectively avoiding plastic deformation caused by slippage of a molecular chain segment in an amorphous region. Meanwhile, the POE sea island phase also serves as an energy storage area, and potential energy is provided for resilience of subsequent materials in the material deformation process.
The UHMWPE can promote the entanglement of partial molecular chain segments in the polypropylene composition, increase the topological entanglement and the secondary entanglement density, and provide a natural barrier for the disentanglement of the molecular chain segments in the deformation process, so that the material is still in the elastic deformation category under the condition of larger deformation amount. In addition, the inventor researches and discovers that UHMWPE and POE have a synergistic toughening effect in the polypropylene system of the invention, and can provide more excellent resilience and lower plastic deformation for the material.
The sorbitol nucleating agent has better grain refining effect in polypropylene compared with other nucleating agents. During processing of the polypropylene composition, a three-dimensional network structure is formed in the PP system, which provides more support points for heterogeneous nucleation of PP, and simultaneously does not promote longitudinal elongation of the crystal nucleus. Thus avoiding imperfect platelet formation during the rapid growth of the crystal nucleus. The inventor researches and discovers that the sliding of the lamella and the structural damage and recombination of the crystal region are important reasons for promoting the material to enter a yield state, and the elastic recovery capability of the material can be effectively improved by reducing imperfect lamella and improving the crystal perfection degree of the crystal region.
Preferably, the melt flow rate of the PP at 230 ℃ and 2.16kg is 10-50 g/10 min.
More preferably, the melt flow rate of the PP at 230 ℃ and 2.16kg is 20-30 g/10 min.
Preferably, the melt flow rate of the POE at 190 ℃ and 2.16kg is 0.5-3 g/10 min.
More preferably, the melt flow rate of the POE at 190 ℃ and 2.16kg is 1-2 g/10 min.
The melt flow rates of PP and POE are determined according to the ISO 1133-1:2011 standard method.
Preferably, the PP is one or more of homo-polypropylene, block co-polypropylene or random co-polypropylene.
Preferably, the content of octenes in the POE is 22-25 wt.%.
The more the content of octene is, the more the soft molecular chain in POE is, and the more energy can be absorbed as an elastomer; however, when the content of octene is too high, the ethylene content in POE is relatively reduced, which results in the decrease of crystallinity, so that the physical crosslinking point is reduced, and POE is easily over-soft and has insufficient elasticity.
Preferably, the number average molecular weight of the UHMWPE is more than or equal to 150 ten thousand.
More preferably, the UHMWPE has a number average molecular weight of 150-200 ten thousand.
The number average molecular weight of UHMWPE is measured by high temperature gel permeation chromatography, and the test standard is SN/T3002-.
Preferably, the nucleating agent is one or more of unsubstituted dibenzylidene sorbitol (DBS), (1,3,2, 4-bis (p-methyldibenzylidene) sorbitol (MDBS), (1,3,2,4) -bis (3, 4-dimethyl) benzylidene sorbitol (DMDBS), or a condensate of n-propylbenzaldehyde-n-propylsorbitol.
More preferably, the nucleating agent is DMDBS.
The inventors have found that DMDBS as a nucleating agent in the polypropylene composition of the present invention can provide a material with better resilience and lower plastic deformation.
Preferably, the other auxiliary agent is 1-3 parts of antioxidant and/or 1-3 parts of processing aid.
Preferably, the antioxidant is one or more of a phenol antioxidant, a phosphite antioxidant, a divalent sulfur antioxidant or a hindered amine antioxidant.
Optionally, the phenolic antioxidant is one or more of antioxidant 264, antioxidant 1010, antioxidant 1076, antioxidant SP, antioxidant 2246, antioxidant CA, antioxidant 330, Irganox1890 or antioxidant 3114.
Optionally, the phosphite antioxidant is one or more of an antioxidant TNP, an antioxidant ODP, an antioxidant 168, Irganox1093 and Irganox 1222.
Optionally, the divalent sulfur antioxidant is one or more of dilaurate thiodipropionate (DLTP) and distearate thiodipropionate (DSTP).
Optionally, the hindered amine antioxidant is one or more of LS-744, LS-770, GW-540 or Flamstab NOR 116.
Preferably, the processing aid is one or more of a low molecular weight lipid processing aid, a metal soap processing aid, a stearic acid complex ester processing aid or an amide processing aid.
Optionally, the low molecular lipid processing aid is one or more of paraffin wax, liquid paraffin wax or low molecular polyolefin wax.
Optionally, the metal soap processing aid is one or more of calcium stearate, magnesium stearate, zinc stearate or barium stearate.
Optionally, the stearic acid composite ester processing aid is one or more of ethylene glycol stearate, glyceryl stearate or pentaerythritol stearate.
Optionally, the amide processing aid is one or more of erucamide, methylene bis stearamide or N, N-ethylene bis stearamide.
Preferably, the polypropylene composition consists of the following components in parts by weight:
73-76 parts of PP, 7-9 parts of POE, 7-9 parts of UHMWPE, 1.2-1.5 parts of sorbitol nucleating agent, 1-2 parts of antioxidant and 1-2 parts of processing aid.
The invention also provides a preparation method of the polypropylene composition, which comprises the following steps:
PP, POE, UHMWPE, sorbitol nucleating agent and other auxiliary agents are mixed and then added into an extruder, and the polypropylene composition is obtained through melt mixing, extrusion and granulation.
Preferably, the extruder is a twin screw extruder.
Preferably, the temperature of a plasticizing section of the double-screw extruder is 190-210 ℃, the temperature of a die head is 200-220 ℃, and the traction speed is 100-200 mm/s.
The invention also protects the application of the polypropylene composition with low plastic deformation and high elastic recovery in the preparation of automobile parts, household appliance switches and parts in the field of sports equipment.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a polypropylene composition with low plastic deformation and high elastic recovery. POE forms a sea-island structure with large particle size in a PP matrix, limits the movement of PP molecular chains, avoids plastic deformation caused by slippage of amorphous region molecular chain segments, and provides potential energy for the rebound of subsequent materials; the UHMWPE promotes entanglement of the sub-segments within the polypropylene composition, so that the material is still under elastic deformation in case of large deformation quantities; the sorbitol nucleating agent provides more heterogeneous nucleation points for PP, simultaneously avoids forming imperfect lamella, and effectively improves the elastic recovery capability of the material. Through the synergistic effect of POE, UHMWPE, sorbitol nucleating agent and PP, the polypropylene composition disclosed by the invention has extremely low plastic deformation and excellent elastic recovery performance.
Drawings
FIG. 1 is an SEM photograph of the polypropylene composition obtained in example 1.
FIG. 2 is a schematic diagram of the elastic property test of the polypropylene composition.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The starting materials in the examples and comparative examples are commercially available as follows:
Figure BDA0003350341040000051
Figure BDA0003350341040000061
reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Examples 1 to 15
Examples 1 to 15 respectively provide a polypropylene composition, the component contents of which are shown in table 1, and the preparation method is as follows:
mixing the components according to the table 1, adding the mixture into a double-screw extruder, and performing melt mixing and extrusion granulation to obtain a polypropylene composition;
wherein the temperature of a plasticizing section of the double-screw extruder is 190-210 ℃, the temperature of a die head is 200-220 ℃, and the traction speed is 100-200 mm/s.
TABLE 1 component content (parts by weight) of the polypropylene compositions of examples 1 to 15
Figure BDA0003350341040000062
Figure BDA0003350341040000063
Figure BDA0003350341040000071
Comparative examples 1 to 7
Comparative examples 1 to 7 respectively provide a polypropylene composition, the component contents of which are shown in table 2, and the preparation method is as follows:
mixing the components according to the table 2, adding the mixture into a double-screw extruder, and performing melt mixing and extrusion granulation to obtain a polypropylene composition;
wherein the temperature of a plasticizing section of the double-screw extruder is 190-210 ℃, the temperature of a die head is 200-220 ℃, and the traction speed is 100-200 mm/s.
TABLE 2 component content (parts by weight) of the polypropylene compositions of comparative examples 1 to 7
Figure BDA0003350341040000072
Performance testing
The polypropylene compositions prepared in the above examples and comparative examples were tested for their properties by the following specific methods:
the polypropylene composition is injection molded into a rectangular sample strip with the length of 100mm, the width of 10mm and the thickness of 4 mm;
the sample strip is horizontally placed as shown in FIG. 2, an external force F is applied to the end of the sample strip away from the table top, the sample strip is pressed downward, and the deformation is performed when the end point of the sample strip is away from the table topFront H0Then, the external force is released, the height of the tail end of the sample strip from the tail end point when the external force is not applied is recorded as H after the sample strip is rebounded and stabilized1Degree of rebound S of the material1＝(H0-H1)/H0100%, the degree of springback S represents the elastic recovery of the material, and (100% -S)1) It represents the plastic deformation of the material. According to the operation, after n times of continuous deformation, recording the maximum height H which can be recovered by the endpoint of the sample stripnAt this time, the degree of springback S of the materialn＝(H0-Hn)/H0100% and (100% -S)n) Representing the plastic deformation of the material after n times of deformation; according to this method, the degree of springback (denoted as S, respectively) of the specimen at the 1 st, 10 th and 100 th deformations is detected and recorded1、S10、S100) And plastic deformation values (100% -S, respectively)1、100％-S10、100％-S100In units of%);
SEM atlas: field emission scanning electron microscope Pharos (femtoscope electron microscope), acceleration voltage: 15.0kV, WD: 6.4 mm.
The SEM spectrum of example 1 is shown in FIG. 1, and the test results of examples 1-15 and comparative examples 1-7 are shown in tables 3 and 4.
As can be seen from FIG. 1, in the polypropylene composition of the present invention, POE exists in the continuous phase of polypropylene as a large-sized sea-island phase.
TABLE 3 test results of examples 1 to 15
Figure BDA0003350341040000081
According to the test results in Table 3, the polypropylene compositions obtained in the examples of the present invention have excellent resilience properties satisfying the condition of S1≥96％，S10≥94％，S100Not less than 88 percent, and after 100 times of deformation, the plastic deformation value is not more than 12 percent.
From the examples 1 to 8, it can be seen that the polypropylene composition has excellent resilience and low plastic deformation when the melt flow rate of PP is 10 to 50g/10min at 230 ℃ and 2.16kg and the melt flow rate of POE is 0.5 to 3g/10min at 190 ℃ and 2.16 kg; when the conditions that the melt flow rate of PP at 230 ℃ and 2.16kg is 20-30 g/10min, the melt flow rate of POE at 190 ℃ and 2.16kg is 1-2 g/10min and the content of octene in POE is 22-25% are met, the rebound resilience and the deformation value of the polypropylene composition are relatively better.
From examples 1, 11 and 12, conventional sorbitol nucleating agents all can provide more pivot points for heterogeneous nucleation of PP and avoid formation of imperfect platelets, thereby improving the elastic recovery capability of the polypropylene composition, wherein DMDBS can be used as the nucleating agent, so that the material has better rebound resilience and lower plastic deformation.
From examples 14 to 15, the polypropylene composition had the following components: 73-76 parts of PP, 7-9 parts of POE, 7-9 parts of UHMWPE, 1.2-1.5 parts of sorbitol nucleating agent, 1-2 parts of antioxidant and 1-2 parts of processing aid, the polypropylene composition has higher elastic recovery degree and lower plastic deformation value, and particularly after multiple times of deformation, the plastic deformation value of the polypropylene composition in the example 15 is only 7% at the 100 th time.
TABLE 4 test results for comparative examples 1 to 7
1 2 3 4 5 6 7
S1 92 95 95 90 92 91 93
100％-S1 8 5 5 10 8 9 7
S10 80 86 88 78 82 80 84
100％-S10 20 14 12 22 18 20 16
S100 60 75 79 63 70 68 72
100％-S100 40 25 21 37 30 32 28
From the test results of table 4, it can be seen from comparative examples 1, 4 and 6 that the polypropylene composition has poor resilience and high plastic deformation value in the absence of any of POE, UHMWPE or sorbitol-based nucleating agent, and the plastic deformation value has reached 8% or more at the first deformation.
From comparative examples 2 and 3, when POE was replaced with another elastomer such as EPDM or the content of octene was too low, the degree of improvement of the rebound property for the polypropylene composition was poor, and S was10080% or less, much lower than S in the examples of the present invention100≥88％。
Compared with the comparative example 5, the UHMWPE is replaced by the conventional linear low-density polyethylene, the entanglement effect of the polypropylene molecular chain segment cannot be improved, and the rebound performance of the UHMWPE on the polypropylene material is difficult to achieve to be equivalent to that of the UHMWPE. From comparative example 7, when the sorbitol-based nucleating agent was replaced with another nucleating agent, the polypropylene composition could not combine excellent resilience and plastic deformation values.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (10)

1. The polypropylene composition with low plastic deformation and high elastic recovery is characterized by comprising the following components in parts by weight:
70-80 parts of PP, 5-10 parts of POE, 5-10 parts of UHMWPE, 1-2 parts of sorbitol nucleating agent and 0-5 parts of other auxiliary agents;
the content of octene in POE is more than or equal to 20 wt.%, and the number average molecular weight of UHMWPE is more than or equal to 100 ten thousand.
2. The polypropylene composition according to claim 1, wherein the PP has a melt flow rate of 10 to 50g/10min at 230 ℃ under 2.16 kg.
3. The polypropylene composition of claim 1, wherein the POE has a melt flow rate of 0.5-3 g/10min at 190 ℃ under 2.16 kg.
4. The polypropylene composition according to any one of claims 1 to 3, wherein the melt flow rate of the PP at 230 ℃ and 2.16kg is 20 to 30g/10min, and the melt flow rate of the POE at 190 ℃ and 2.16kg is 1 to 2g/10 min.
5. The polypropylene composition of claim 1, wherein the POE has an octene content of 22-25%.
6. The polypropylene composition according to claim 1, wherein the UHMWPE has a number average molecular weight of 150 to 200 ten thousand.
7. The polypropylene composition according to claim 1, wherein the nucleating agent is one or more of unsubstituted dibenzylidene sorbitol, (1,3,2, 4-bis (p-methyldibenzylidene) sorbitol, (1,3,2,4) -bis (3, 4-dimethyl) benzylidene sorbitol, or a condensate of n-propylbenzaldehyde-n-propylsorbitol.
8. A process for the preparation of a polypropylene composition according to any one of claims 1 to 7, comprising the steps of:
PP, POE, UHMWPE, sorbitol nucleating agent and other auxiliary agents are mixed and then added into an extruder, and the polypropylene composition is obtained through melt mixing, extrusion and granulation.
9. The preparation method according to claim 8, wherein the extruder is a twin-screw extruder, the temperature of a plasticizing section of the twin-screw extruder is 190-210 ℃, the temperature of a die head is 200-220 ℃, and the drawing speed is 100-200 mm/s.
10. Use of the polypropylene composition according to any one of claims 1 to 7 for the manufacture of automotive parts, household appliance switches, parts for sports equipment.
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