CN111635588A - Low-temperature ultrahigh-toughness polypropylene blending composite material and preparation method thereof - Google Patents
Low-temperature ultrahigh-toughness polypropylene blending composite material and preparation method thereof Download PDFInfo
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- CN111635588A CN111635588A CN202010482756.XA CN202010482756A CN111635588A CN 111635588 A CN111635588 A CN 111635588A CN 202010482756 A CN202010482756 A CN 202010482756A CN 111635588 A CN111635588 A CN 111635588A
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- 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
- C08L2205/242—Beta spherulite nucleating agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The description discloses a low-temperature ultrahigh-toughness polypropylene blending composite material and a preparation method thereof, belonging to the field of polymer processing modification, wherein the blending composite material is prepared from the following raw materials in parts by weight: 70-90 parts of polypropylene, 10-30 parts of ethylene-octene segmented copolymer, 0.1 part of beta nucleating agent and 0.05-2 parts of carbon nano tube. The preparation method comprises the steps of premixing the carbon nano tube, the beta nucleating agent, the ethylene-octene segmented copolymer and the polypropylene, then carrying out melt blending granulation on the premix through an extruder, and then preparing the polypropylene blending composite material product by adopting an injection molding machine. The carbon nano tube, the beta nucleating agent and the ethylene-octene segmented copolymer are added simultaneously to generate a low-temperature synergistic toughening effect on the polypropylene, so that the polypropylene blending composite material shows excellent low-temperature toughness.
Description
Technical Field
The invention relates to a polypropylene blending composite material and a preparation method thereof, in particular to a low-temperature ultrahigh-toughness polypropylene blending composite material and a preparation method thereof, belonging to the field of polymer processing modification.
Background
As one of five general-purpose plastics, polypropylene has a series of advantages of excellent comprehensive performance, easy processing, low production cost and the like, and is widely applied to the fields of automobiles, household appliances, electronics, food packaging and the like. However, polypropylene has a significant disadvantage of poor toughness, especially low temperature toughness, which greatly limits its application expansion.
Researchers began to research the toughening modification of polypropylene from the last 70 th century and developed a series of polypropylene toughening modification methods. The introduction of elastomers into polypropylene is the most common and efficient method for improving the room temperature toughness of polypropylene, but the low temperature toughening effect of polypropylene is not obvious. This is mainly due to the time-temperature equivalent principle, the glass transition temperature of the elastomer and polypropylene subjected to the instantaneous impact force rises, and brittle fracture occurs. If the elastomer with low glass transition temperature is added or the glass transition temperature of the elastomer is reduced, the polypropylene composite material can generate brittle-tough transition at low temperature, and the low-temperature toughness of the polypropylene is improved. It was found that 50 wt% EPDM was added to the polypropylene. The impact strength of the polypropylene blend at-30 ℃ was improved by 6 times compared to pure PP (Lopez-Manchado, M. A.; Biagiotti, J.; Arroyo, M. Macromol Symp. 1999, 148, 345.).
The elongation at break of the β -NA-containing polypropylene/EPR composite material is improved by 121% compared with polypropylene even at-40 ℃ (Kotek, J.; Scudla, J.; Slouf, M. J appl Polym Sci, 2007, 103, 3539.). Yang and the like prepares a polypropylene/POE/β nucleating agent blend through annealing treatment, when the POE content reaches 40 wt%, the low-temperature (-40 ℃) impact strength of the blend reaches 51 kJ/m2The low temperature toughness of polypropylene is improved to some extent synergistically by the incorporation of elastomers in combination with β nucleating agents, but the low temperature toughness of polypropylene is still not improved to a certain extentMeeting the low-temperature application requirement of polypropylene. In addition, in this case, the elastomer is generally contained in a large amount, which results in a significant decrease in rigidity, deterioration in processing fluidity, and insignificant economic benefits.
From the examined patents and documents, the patents related to the improvement of the low-temperature toughness of polypropylene are not many and the effect is not obvious. A high-low temperature toughness modified polypropylene material and a preparation method thereof (Chinese patent publication No. CN 102002189A) and a preparation method of a low-temperature toughness isotactic polypropylene product (Chinese patent publication No. CN 103265758A) have no obvious low-temperature toughening effect in the two patents; the invention discloses a low-temperature-resistant polypropylene modified pipe and a preparation method thereof (Chinese invention patent, publication No. CN 103642126A), and the invention indicates that no pipe is cracked in an impact test at-10 ℃, but quantitative data is not available; an ultra-low temperature toughness polypropylene composition and a preparation method thereof (Chinese invention patent, publication No. CN 103665570A) need to vulcanize an elastomer; the ultralow temperature high toughness modified polypropylene and its preparation process (Chinese patent publication No. CN 104744812A) needs self-synthesis of amorphous alpha-olefin as toughening agent. The processes of the two patents are complicated. The patent does not report the low-temperature ultrahigh-toughness polypropylene/ethylene-octene block copolymer/beta nucleating agent/carbon nanotube quaternary blending composite material and the preparation method thereof, which are the same as or similar to the patent.
Disclosure of Invention
The invention aims to develop a low-temperature ultrahigh-toughness polypropylene blending composite material and a preparation method thereof, wherein the blending composite material is prepared from the following raw materials in parts by weight:
70-90 parts of polypropylene
10-30 parts of ethylene-octene block copolymer
Beta nucleating agent 0.1 part
0.05-2 parts of carbon nano tube
The preparation method comprises the steps of premixing the carbon nano tube, the beta nucleating agent, the ethylene-octene segmented copolymer and the polypropylene, then carrying out melt blending granulation on the premix through an extruder, and then preparing the polypropylene blending composite material product by adopting an injection molding machine.
More specific process steps and conditions are as follows:
(1) premixing carbon nano tubes, a beta nucleating agent, an ethylene-octene block copolymer and polypropylene: stirring the carbon nano tube, the beta nucleating agent, the ethylene-octene segmented copolymer and the polypropylene at normal temperature according to the weight part ratio, and carrying out physical premixing;
(2) extruding and granulating the carbon nano tube/beta nucleating agent/ethylene-octene segmented copolymer/polypropylene premix: and (3) melting and mixing the premix in the step (1) by using an industrial conventional double-screw extruder, and extruding and granulating. The adopted extrusion process conditions are as follows: the temperature of a feeding section (1-2 sections) is 160-200 ℃, the temperature of a shearing and blending section (3-8 sections) is 180-210 ℃, the temperature of an extruding section (9-10 sections) is 180-200 ℃, the rotating speed of a screw is 80-100 rpm, extruded strips are cooled in cold water at the temperature lower than 30 ℃, and then granulated by a granulator, wherein the length of granules is 3-6 mm;
(3) injection molding of the carbon nanotube/beta nucleating agent/ethylene-octene block copolymer/polypropylene blend: drying the granulated blend granules in a vacuum oven at 80 ℃ until the moisture content is less than 0.01 percent by weight, and selecting an industrial screw type injection molding machine to form a product, thereby obtaining the low-temperature ultrahigh-toughness polypropylene/ethylene-octene segmented copolymer blend composite material. The adopted injection molding process conditions are as follows: the temperature of a charging barrel and a nozzle of the injection molding machine is 180-220 ℃, the injection pressure is 60-80 MPa, the pressure maintaining time is 15-20 s, and the cooling time is 15-60 s.
Wherein:
the polypropylene is any isotactic polypropylene which is commercially available.
The ethylene-octene block copolymer is any commercially available ethylene-octene block copolymer with a glass transition temperature of less than-45 ℃.
The beta nucleating agent is not particularly limited and may be any commercially available beta nucleating agent.
The carbon nanotubes may be any commercially available carbon nanotubes.
Based on the problem of insufficient improvement of the low-temperature toughness of the polypropylene in the prior art, the ethylene-octene block copolymer, the carbon nano tube and the beta nucleating agent are simultaneously added into the polypropylene matrix. The polypropylene blending composite material forms a similar bicontinuous phase structure and a bicontinuous phase structure, which is beneficial to the superposition of stress fields; CNTs are selectively distributed at the phase interface of polypropylene and an ethylene-octene block copolymer; the beta nucleating agent induces the polypropylene to form self-toughened beta crystals and improves the compatibility of the polypropylene and the ethylene-octene block copolymer; the mobility of the amorphous zone subchain of the blended composite material is obviously improved. The synergistic effect of the factors greatly improves the low-temperature toughness of the polypropylene, and exceeds the linear sum of the toughness improvement range when the three are independently introduced.
In addition, the invention also has the following advantages:
1) the room temperature impact toughness of the polypropylene composite material reaches a super toughness level. The impact strength at 20 ℃ is as high as 69.1kJ/m2Being of pure polypropylene (3.1 kJ/m)2) 22.3 times.
2) The carbon nano tube, the beta nucleating agent, the ethylene-octene block copolymer and the polypropylene used in the method are all commercial products and have low price.
3) The addition amounts of the carbon nano tube and the beta nucleating agent are less, the processing performance of the material is not influenced, and the processing technology is not required to be changed.
4) The preparation method is simple in operation process, low in production cost and suitable for large-scale industrial production, and the polypropylene composite material is prepared by using an industrial conventional double-screw extruder and an injection molding machine.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following examples are given to illustrate the present invention and it should be noted that the following examples are given only for the purpose of further illustrating the present invention and should not be construed as limiting the scope of the present invention.
Examples 1 to 7 and comparative examples 1 to 6:
(1) premixing: the carbon nano tube, the beta nucleating agent, the ethylene-octene block copolymer with the glass transition temperature lower than-45 ℃ and the isotactic polypropylene are stirred and premixed at normal temperature according to the weight part ratio. The specific formulation is shown in table 1.
(2) Extruding and granulating the carbon nano tube/beta nucleating agent/ethylene-octene segmented copolymer/polypropylene premix: and (3) melting and mixing the premix in the step (1) by using an industrial conventional double-screw extruder, and extruding and granulating. The adopted extrusion process conditions are as follows: the temperature of a feeding section (1-2 sections) is 160 ℃, the temperature of a shearing and blending section (3-8 sections) is 180-195 ℃, the temperature of an extruding section (9-10 sections) is 190 ℃, the rotating speed of a screw is 80 rpm, and extruded material strips are granulated by a granulator after being cooled in cold water at 23 ℃. The specific process parameters are shown in Table 2.
(3) Injection molding of the carbon nanotube/beta nucleating agent/ethylene-octene block copolymer/polypropylene blended composite material: the blended pellets were dried in a vacuum oven at 80 ℃ until the moisture content was less than 0.01% by weight. Selecting an industrial screw type injection molding machine to form a product, and obtaining the low-temperature ultrahigh-toughness polypropylene/ethylene-octene segmented copolymer blending composite material product. The adopted injection molding process conditions are as follows: the temperature from a charging barrel to a nozzle of the injection molding machine is 190-210 ℃, the injection pressure is 60 MPa, the pressure maintaining pressure is 65 MPa, the pressure maintaining time is 15 s, and the cooling time is 20 s. The specific process parameters are shown in Table 3.
Performance evaluation method:
the impact test is carried out according to GB/T1843-2008, a notch sampling machine is adopted to mill a notch, an impact sample strip is prepared, and after the impact sample strip is placed for 48 hours, the impact test is carried out at 20 ℃ and low temperature (0 ℃ -20 ℃). The test method of the low-temperature impact test is to quickly carry out the impact test after a sample is placed in a low-temperature reaction bath for soaking for 2 hours. The results of the impact property tests of the examples and comparative examples are shown in Table 4.
Table 1 examples 1-7 and comparative examples 1-6 formula tables:
table 2 melt extrusion process parameters:
table 3 injection molding process parameters:
table 4 impact performance test results for examples 1-7 and comparative examples 1-6:
from the above, at-20 ℃, the impact strength of the pure polypropylene is only 2.1 kJ/m2, 0.05 part of carbon nano tube, 0.1 part of beta nucleating agent or 30 parts of ethylene-octene block copolymer are respectively added into the polypropylene, and the impact strength of the polypropylene blending composite material can respectively reach 2.2 kJ/m2, 2.1 kJ/m2 and 8.3 kJ/m2, which are respectively improved by 4.8%, 0% and 295% compared with the pure polypropylene. And 0.05 part of carbon nano tube, 0.1 part of beta nucleating agent and 30 parts of ethylene-octene block copolymer are simultaneously added into polypropylene, so that the impact strength of the polypropylene blending composite material is as high as 32.8 kJ/m2, which is 1462% higher than that of pure polypropylene. With the further increase of the CNTs content to 0.5 parts, the impact strength of the polypropylene blend composite material at-20 ℃ is more up to 52.5 kJ/m 2.
Description of the drawings: in the preparation method of the low-temperature ultrahigh-toughness polypropylene blending composite material, the process conditions of extrusion granulation of the premix and injection molding of the blend can be adjusted within a certain range according to actual conditions, and are not limited to the examples. The extrusion process conditions are as follows: the temperature of a feeding section (1-2 sections) is 160-200 ℃, the temperature of a shearing and blending section (3-8 sections) is 180-210 ℃, the temperature of an extruding section (9-10 sections) is 180-200 ℃, the rotating speed of a screw is 80-100 rpm, extruded strips are cooled in cold water at the temperature lower than 30 ℃, and then granulated by a granulator, wherein the length of granules is 3-6 mm; the injection molding process conditions are as follows: the temperature of a charging barrel and a nozzle of the injection molding machine is 180-220 ℃, the injection pressure is 60-80 MPa, the pressure maintaining time is 15-20 s, and the cooling time is 15-60 s.
Claims (4)
1. A low-temperature ultrahigh-toughness polypropylene blending composite material and a preparation method thereof are characterized in that: the material is composed of the following raw materials in parts by weight:
70-90 parts of polypropylene
10-30 parts of ethylene-octene block copolymer
Beta nucleating agent 0.1 part
0.05-2 parts of carbon nano tube
The preparation method comprises the steps of premixing the carbon nano tube, the beta nucleating agent, the ethylene-octene segmented copolymer and the polypropylene, then carrying out melt blending granulation on the premix through an extruder, and then preparing the polypropylene blending composite material product by adopting an injection molding machine.
2. The low-temperature ultra-high toughness polypropylene blend composite material and the preparation method thereof as claimed in claim 1, wherein: the polypropylene is isotactic polypropylene.
3. The low-temperature ultra-high toughness polypropylene blend composite material and the preparation method thereof as claimed in claim 1, wherein: the ethylene-octene block copolymer is an ethylene-octene block copolymer having a glass transition temperature of less than-45 ℃.
4. The low-temperature ultra-high toughness polypropylene blend composite material and the preparation method thereof as claimed in claim 1, wherein: the preparation steps are as follows:
(1) premixing carbon nano tubes, a beta nucleating agent, an ethylene-octene block copolymer and polypropylene: stirring the carbon nano tube, the beta nucleating agent, the ethylene-octene segmented copolymer and the polypropylene at normal temperature according to the weight part ratio, and carrying out physical premixing;
(2) extruding and granulating the carbon nano tube/beta nucleating agent/ethylene-octene segmented copolymer/polypropylene premix: melting and mixing the premix in the step (1) by adopting an industrial conventional double-screw extruder, and extruding and granulating; the adopted extrusion process conditions are as follows: the temperature of a feeding section (1-2 sections) is 160-200 ℃, the temperature of a shearing and blending section (3-8 sections) is 180-210 ℃, the temperature of an extruding section (9-10 sections) is 180-200 ℃, the rotating speed of a screw is 80-100 rpm, extruded strips are cooled in cold water at the temperature lower than 30 ℃, and then granulated by a granulator, wherein the length of granules is 3-6 mm;
(3) injection molding of the carbon nanotube/beta nucleating agent/ethylene-octene block copolymer/polypropylene blend: drying the granulated blend granules in a vacuum oven at 80 ℃ until the moisture content is less than 0.01 percent by weight, and selecting an industrial screw injection molding machine to form a product; the adopted injection molding process conditions are as follows: the temperature of a charging barrel and a nozzle of the injection molding machine is 180-220 ℃, the injection pressure is 60-80 MPa, the pressure maintaining time is 15-20 s, and the cooling time is 15-60 s.
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| CN202011244933.7A CN112094460A (en) | 2020-06-01 | 2020-11-10 | Low-temperature ultrahigh-toughness polypropylene blending composite material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112552605A (en) * | 2020-12-11 | 2021-03-26 | 成都金发科技新材料有限公司 | Polypropylene composite material with good dermatoglyph replication capacity and preparation method thereof |
| CN113527809A (en) * | 2021-07-28 | 2021-10-22 | 西北工业大学宁波研究院 | Polypropylene injection molded article and method for producing the same |
| CN117024873A (en) * | 2023-06-15 | 2023-11-10 | 广州力合新材料科技有限公司 | Preparation method of modified polypropylene plastic |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112809957A (en) * | 2020-12-23 | 2021-05-18 | 安徽杰蓝特新材料有限公司 | High-performance non-elastomer ternary blending composite material and preparation method thereof |
| CN113337028B (en) * | 2021-07-20 | 2023-04-28 | 福建师范大学泉港石化研究院 | Plastic wall pipe and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103265758B (en) * | 2013-06-03 | 2015-07-29 | 四川大学 | A kind of preparation method of low-temperature flexibility isotatic polypropylene goods |
| CN110343332A (en) * | 2019-07-11 | 2019-10-18 | 西北工业大学 | A kind of high-toughness polypropylene/elastic composite and preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112552605A (en) * | 2020-12-11 | 2021-03-26 | 成都金发科技新材料有限公司 | Polypropylene composite material with good dermatoglyph replication capacity and preparation method thereof |
| CN112552605B (en) * | 2020-12-11 | 2024-02-02 | 成都金发科技新材料有限公司 | Polypropylene composite material with good dermatoglyph replication capability and preparation method thereof |
| CN113527809A (en) * | 2021-07-28 | 2021-10-22 | 西北工业大学宁波研究院 | Polypropylene injection molded article and method for producing the same |
| CN117024873A (en) * | 2023-06-15 | 2023-11-10 | 广州力合新材料科技有限公司 | Preparation method of modified polypropylene plastic |
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