CN114230928A - Low-temperature impact resistant polypropylene composition and preparation method thereof - Google Patents
Low-temperature impact resistant polypropylene composition and preparation method thereof Download PDFInfo
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- CN114230928A CN114230928A CN202210053368.9A CN202210053368A CN114230928A CN 114230928 A CN114230928 A CN 114230928A CN 202210053368 A CN202210053368 A CN 202210053368A CN 114230928 A CN114230928 A CN 114230928A
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- C—CHEMISTRY; METALLURGY
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- 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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- 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
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- C08L23/14—Copolymers of propene
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Abstract
The invention discloses a low-temperature impact resistant polypropylene composition and a preparation method thereof, belonging to the field of high polymer materials. The low-temperature impact resistant polypropylene composition does not use expensive chopped aramid fiber as a reinforcing filler, but adopts a specific toughening agent matched with the copolymerized nylon 6 as a component, so that the obtained product has good normal-temperature tensile property and excellent low-temperature impact resistance, can meet the requirements of a low-temperature-55 ℃ drop impact test, and does not have obvious cracks after the test. The invention also discloses a preparation method of the low-temperature impact resistant polypropylene composition and application of the low-temperature impact resistant polypropylene composition in preparing military material packing boxes.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a low-temperature impact resistant polypropylene composition and a preparation method thereof.
Background
Polypropylene (PP) is increasingly used in automobiles and home appliances due to its advantages of low density, easy processing, excellent electrical properties, etc. However, polypropylene materials have poor low-temperature toughness, which results in poor low-temperature impact properties of the product, and limits further application development; therefore, in the prior art, the glass fiber is usually introduced into the polypropylene material, so that the mechanical strength of the material is improved, and the long glass fiber reinforced polypropylene material is particularly used, so that the mechanical strength and the impact property of the material can be obviously improved.
However, in some extreme applications, such as military shell packing cases, the low-temperature-55 ℃ drop impact test is required to be met, the performance requirements of a pure long glass fiber reinforced polypropylene material are difficult to meet, and the tensile property and other mechanical strength of the material are reduced by increasing the content of the toughening agent in the product components, so that the system needs to be further modified to meet the excellent low-temperature impact resistance.
CN 107345026A discloses a polypropylene composite material with low-temperature impact resistance of-55 ℃ and high-temperature deformation resistance of 70 ℃, wherein a polypropylene blending modified material prepared by using long glass fiber mixed chopped aramid fiber as a reinforcing matrix and matching a toughening agent can meet the requirement of no damage in low-temperature falling of military cannonball packing cases, but the used chopped aramid fiber is expensive and has large addition amount, and is not suitable for industrial production. CN 109370062A discloses a long glass fiber reinforced polypropylene material with anti-falling ball impact and good appearance, a preparation method and application thereof, and the problems of falling ball cracking and stress whitening of the material are greatly improved by a method of compounding high impact polypropylene, polyethylene and antimony trioxide; although the cost of the raw materials used in the method is low, the main emphasis is on stress whitening and normal-temperature notch impact, the impact strength at the low temperature of-55 ℃ is difficult to achieve, and the added antimony trioxide is not favorable for material color matching, so that the application of the antimony trioxide is further limited.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide the low-temperature impact resistant polypropylene composition, the components of the product are combined and matched by nylon and a specific toughening agent, so that the low-temperature impact resistance of the product is effectively improved, the requirements of a low-temperature-55 ℃ drop impact test are met, no obvious crack appears after the test, and the polypropylene composition has good intrinsic normal-temperature tensile strength and is suitable for extreme applications such as military shell packing cases; the components of the product are low in price, and industrial production can be realized.
In order to achieve the purpose, the invention adopts the technical scheme that:
a polypropylene composition with low-temperature impact resistance comprises a component A and a component B;
the component A comprises the following components in parts by weight:
30-60 parts of polypropylene, 40-60 parts of long glass fiber, 3-7 parts of compatilizer and 0.2-2 parts of processing aid;
the component B comprises the following components in parts by weight:
35-75 parts of polypropylene, 15-25 parts of a toughening agent, 610-30 parts of copolymerized nylon and 0.2-2 parts of a processing aid; the toughening agent comprises at least one of ethylene octene copolymer (POE), maleic anhydride grafted POE, maleic anhydride grafted ethylene propylene diene monomer rubber and ethylene-ethyl acrylate copolymer;
the mass ratio of the component A to the component B is (5-7.5): (2.5-5).
The polypropylene composition adopts a form of combining the component A and the component B, the component A mainly serves as a matrix mechanical property component, the long glass fiber with low cost is used as a filling material, and the component A prepared under the condition of the mixture ratio can provide excellent tensile property and impact resistance of a final product.
The component B in the polypropylene composition is prepared by matching and combining the copolymerized nylon 6 with a good low-temperature impact resistance effect and a specific toughening agent in a synergistic manner, other additional inorganic components are not required to be introduced, the normal-temperature tensile strength of the obtained product can be improved (the tensile strength of a polypropylene material at a low temperature is generally better than that at a normal temperature, so that the normal-temperature tensile strength can represent the property of the product at the low temperature), the low-temperature impact resistance of the product can be enhanced, the requirements of a low-temperature-55 ℃ drop impact test are met, and the polypropylene composition is suitable for extreme applications such as military cannonball packing cases.
Preferably, the toughening agent is a mixture of POE and maleic anhydride grafted POE;
more preferably, the grafting rate of the maleic anhydride grafted POE in the toughening agent is 0.8-1%, and the mass ratio of the POE to the maleic anhydride grafted POE is (2-4): 1.
The inventor finds that compared with the method of using pure POE as a toughening agent, the mixture obtained by mixing and matching the maleic anhydride grafted POE with the POE can further improve the low-temperature impact resistance of the obtained product, however, if the content of the maleic anhydride grafted POE is too much (or the grafting rate of the maleic anhydride is too high), the fluidity of the product is deteriorated, the dispersibility of the toughening agent is poor, and the low-temperature impact resistance of the product is weakened, and if the content of the maleic anhydride grafted POE is lower, the low-temperature impact resistance of the product is improved to a lower extent.
Preferably, the preparation method of the copolymerized nylon 6 comprises the following steps: uniformly mixing caprolactam monomer and nylon monomer salt, putting the mixture into a high-pressure reaction kettle, pumping the interior of the high-pressure reaction kettle to a vacuum state, reacting under the protection of atmosphere, and sequentially carrying out wire drawing, grain cutting, water boiling and drying on the obtained product to obtain the copolymerized nylon 6.
Preferably, the polypropylene in the A component and the B component is a co-polypropylene.
Preferably, the melt index of the polypropylene in the component A and the component B is more than or equal to 80g/10min at 230 ℃ and under the load of 2.16kg according to ISO 1133-2011.
The inventor finds that the polypropylene copolymer has more excellent impact resistance compared with the polypropylene homopolymer, and the raw material with higher fluidity can lead to better dispersibility, higher formability and better low-temperature impact resistance of each component, while the lower fluidity can lead to reduced dispersibility of each component and reduced low-temperature impact resistance of the product.
Preferably, the long glass fibers have an average diameter of 15 to 19 μm.
Preferably, the compatilizer is at least one of maleic anhydride grafted polypropylene, acrylic acid grafted polypropylene and glycidyl acrylate grafted polypropylene;
more preferably, the grafting rate of the compatilizer is 0.7-1.2%.
The inventor finds that when the grafted polypropylene with a specific grafting ratio is used as a compatilizer, the compatibility of the polypropylene and the long glass fiber in the components can be effectively coordinated, the stability of the product is improved, and when the grafting ratio is too high, the poor dispersibility of the components is easily caused, and the low-temperature impact resistance of the final product is reduced.
Preferably, the processing aid is at least one of an antioxidant, a light stabilizer and a lubricant;
more preferably, the antioxidant is at least one of hindered phenol antioxidant and phosphite antioxidant; the light stabilizer is a hindered amine antioxidant; the lubricant is at least one of zinc stearate, calcium stearate, magnesium stearate, polyethylene wax, EVA wax, oleamide, erucamide, ethylene bis stearamide, an organic silicon lubricant and pentaerythritol stearate.
Another object of the present invention is to provide a method for preparing the polypropylene composition with low temperature impact resistance, comprising the following steps:
(1) preparation of component A: uniformly mixing the polypropylene, the compatilizer and the processing aid in the component A according to a ratio, putting the mixture into a double-screw extruder, then putting the long glass fiber subjected to pre-dispersion treatment, and performing melt extrusion granulation to obtain a component A;
(2) preparation of the component B: uniformly mixing all the components in the component B according to the proportion, and putting the mixture into a double-screw extruder for melt extrusion granulation to obtain the component B;
(3) and uniformly mixing the component A and the component B according to the proportion, melting, extruding and granulating to obtain the low-temperature impact resistant polypropylene composition.
The preparation method of the low-temperature impact resistant polypropylene composition has simple operation steps and can realize industrial mass production.
Preferably, the temperature of the twin-screw extruder in the step (1) during melting, extruding and granulating is 210-250 ℃, the component A enters a soaking die head in the twin-screw extruder, and the temperature of the soaking die head is 270-320 ℃.
Preferably, the temperature of the twin-screw extruder in the step (2) during melt extrusion granulation is 210-250 ℃.
Preferably, the temperature of the twin-screw extruder in the step (3) during melt extrusion granulation is 210-250 ℃.
It is a further object of the present invention to provide the use of said low temperature impact resistant polypropylene composition for the preparation of packaging boxes for military materials.
The low-temperature impact resistant polypropylene composition has the advantages of low raw material cost, simple preparation process, good conventional tensile strength and excellent low-temperature impact resistance, and is particularly suitable for preparing military material packing boxes with special requirements on extreme low-temperature impact resistance.
The invention has the beneficial effects that the low-temperature impact resistant polypropylene composition is prepared by using the specific toughening agent matched with the copolymerized nylon 6 as a component instead of using expensive chopped aramid fiber as a reinforcing filler, so that the obtained product has good normal-temperature tensile property and excellent low-temperature impact resistance, can meet the requirements of a low-temperature-55 ℃ drop impact test, and does not have obvious cracks after the test. The invention also provides a preparation method of the low-temperature impact resistant polypropylene composition and application of the low-temperature impact resistant polypropylene composition in preparing military material packing boxes.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples and comparative examples, which are intended to be understood in detail, but not intended to limit the invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention. The experimental reagents and instruments designed for the practice of the present invention and the comparative examples are common reagents and instruments unless otherwise specified.
Example 1
In one embodiment of the polypropylene composition with low temperature impact resistance of the present invention, the preparation method of the polypropylene composition comprises the following steps:
(1) preparation of component A: uniformly mixing the polypropylene, the compatilizer and the processing aid in the component A in a high mixing machine according to a ratio, putting the mixture into a double-screw extruder, enabling the components to pass through an infiltration die head in a molten state, then putting long glass fibers subjected to pre-dispersion treatment into the double-screw extruder, enabling the long glass fibers to enter the infiltration die head, and performing melt extrusion granulation on the components in an infiltration die head to obtain the component A; the temperature of the double-screw extruder is 210-250 ℃, and the temperature of the infiltration die head is 270-320 DEG C
(2) Preparation of the component B: uniformly mixing all the components in the component B in a high-speed mixer according to the proportion, putting the mixture into a double-screw extruder, and performing melt extrusion granulation to obtain the component B; the temperature of the double-screw extruder is 210-250 ℃;
(3) uniformly mixing the component A and the component B according to the ratio of 6:4, and performing melt extrusion granulation to obtain the low-temperature impact resistant polypropylene composition; the temperature of the double-screw extruder is 210-250 ℃.
Wherein the ratio of the component A and the component B is shown in Table 1.
Examples 2 to 18
Examples 2 to 18 differ from example 1 only in the ratio of the components, as shown in table 1.
TABLE 1
Wherein the polypropylene 1 is an EP640V product produced by Zhonghai Shell company, and has a melt index of 100g/10min at 230 ℃ under a load of 2.16 kg;
the long glass fiber is a product model SE4805-2400 produced by OC company, and the average diameter of the long glass fiber is 17 mu m;
the compatilizer is a CA100 product produced by Achima, maleic anhydride grafted polypropylene, and the grafting rate of the compatilizer is 0.8%;
the POE is a POE 8137 product produced by the Dow chemical company;
the maleic anhydride grafted ethylene propylene diene monomer rubber is a KT-7 product generated by Konton company;
the ethylene-ethyl acrylate copolymer is AMPLIFY EA101 product produced by the Dow chemical company;
the maleic anhydride grafted POE1 is a KT-916K product produced by Shenyang Ketong company, and the grafting rate is 0.9%;
the copolymerized nylon 6 is self-made;
the preparation method of the copolymerized nylon 6 comprises the following steps: preparing a mixed material of caprolactam monomer and required nylon monomer salt (PA610 salt), adding the mixed material into a high-pressure reaction kettle, vacuumizing the high-pressure reaction kettle, reacting under the protection of nitrogen, controlling the relative viscosity of the obtained product to be 2.5, and sequentially carrying out wire drawing, grain cutting, water boiling and drying on the obtained product to obtain the nylon 6 copolymer.
The antioxidant is a commercially available antioxidant; the light stabilizer is a commercial light stabilizer; the lubricant is a commercially available lubricant; the toner is a commercially available toner.
The maleic anhydride grafted POE2 is a KT series experimental material product produced by Shenyang Ketong company, and the grafting rate is 1.1%.
The maleic anhydride grafted POE3 was an N406 product from Netsuka corporation, and its grafting ratio was 0.5%.
The polypropylene 2 is a product of EP548R model manufactured by Zhonghai Shell company, and has a melt index of 28g/10min at 230 ℃ under a load of 2.16 kg;
the polypropylene 3 is M60T model homopolymerized polypropylene produced by Zhenhai refining, and has a melt index of 60g/10min at 230 ℃ under the load of 2.16 kg;
comparative examples 1 to 9
Comparative examples 1 to 9 differ from example 1 only in the component ratio, as shown in table 2.
TABLE 2
The maleic anhydride grafted ethylene terpolymer is an Elvaloy resins PTW product produced by DuPont.
The copolymerized nylon 66 is a nylon EP-158 product produced by Huafeng company.
Except for the specific description above, the commercial raw materials used in each of the various proportions were the same species as used in the examples.
Effect example 1
In order to verify the low temperature impact resistant polypropylene composition, each product is subjected to injection molding to form an experimental square plate with 100 x 3mm, and a normal temperature (25 ℃) tensile strength test, a-55 ℃ low temperature impact strength test and a low temperature ball drop impact test are respectively carried out, specifically as follows:
(1) and (3) testing the normal-temperature tensile strength: the test of the experimental square plate is carried out according to ISO 527-;
(2) -55 ℃ pendulum low temperature impact strength test: the experimental square plate is tested according to ISO 179-2010 standard, and the impact pendulum capacity is 5.5J;
(3) and (3) low-temperature ball drop impact test: the experimental square plate is placed in an environment with the temperature of-55 ℃, 500g of pure metal iron balls are placed at the height of 500mm right above the experimental square plate, and the surface fracture condition of the experimental square plate is observed after the iron balls freely fall and fall on the experimental square plate.
The surface fracture was judged according to the following criteria:
no crack: the surface of the sample is free from any crack cracks;
slight cracking: slight cracks exist on the surface of the sample, and the length of each crack is 1-5 mm;
moderate cracking: the surface of the sample has obvious cracks, and the length of each crack is 5-10 mm;
obvious cracks: the surface of the sample has obvious cracks, and the length of the cracks is more than 10 mm.
The test results are shown in tables 3 and 4.
TABLE 3
TABLE 4
As can be seen from tables 3 and 4, the products obtained in the examples of the present invention have good intrinsic tensile strength (> 90MPa) and high low temperature impact strength (not less than 25KJ/m at-55 ℃ C.)2) (ii) a The low-temperature impact strength and the low-temperature falling ball impact test result have a certain relation, and no obvious cracks appear on the surface of each product after the low-temperature falling ball impact test, which indicates that each product can meet the requirements of the low-temperature-55 ℃ falling ball impact test. It can be known from the comparison of the performances of the products in the examples 2 to 6 that the addition of the toughening agent and the copolymerized nylon 6 in the product components affects both the normal-temperature tensile property and the low-temperature impact resistance of the product, and the product can take both the normal-temperature tensile property and the low-temperature impact resistance into consideration in a specific range, while the copolymerized nylon 6 or the toughening agent in the B components of the products in the comparative examples 7 and 8 has too much addition content, so that the product is difficult to take both excellent normal-temperature tensile strength and excellent low-temperature impact resistance into consideration. As can be seen from a comparison of examples 1 and 2, when employed in the product compositionWhen POE and maleic anhydride grafting POE are matched as the toughening agent, compared with a product which only uses POE as the toughening agent, the low-temperature impact resistance effect is better, and as can be seen from comparison between the embodiment 1 and the embodiments 7-10, the POE is different in proportion of maleic anhydride grafting POE, the performance of the product is also different, and the mass proportion of the POE to the maleic anhydride grafting POE is (2-4): the effect is best at 1 time. On the other hand, it is clear from the comparison between example 1 and examples 14 and 15 that the room temperature tensile properties and low temperature impact resistance are better when the preferable graft ratio of maleic anhydride grafted POE is used. From the comparison of the performances of example 1 and examples 13 and 16, it can be seen that when the matrix resin in the product is selected as high-fluidity polypropylene copolymer, the dispersibility and moldability of each component are better, and the overall effect is better.
Compared with the product performance of the example 1, the product obtained in the comparative examples 1-3 can exert a synergistic effect only when the copolymerized nylon 6 and the toughening agent exist in the product components at the same time, so that the normal-temperature tensile strength of the product is improved, and the low-temperature impact resistance of the product is enhanced; as can be seen from the product performances of comparative examples 4-5, the types of the toughening agent and the nylon of the product have great influence on the performance of the product, and the effect of the product is difficult to achieve by selecting the toughening agent and the nylon outside the protection range of the claims; in the products of comparative examples 9 and 10, the addition ratio of the component A and the component B is not proper, and the ideal technical effect is difficult to achieve.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A polypropylene composition with low-temperature impact resistance is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
30-60 parts of polypropylene, 40-60 parts of long glass fiber, 3-7 parts of compatilizer and 0.2-2 parts of processing aid;
the component B comprises the following components in parts by weight:
35-75 parts of polypropylene, 15-25 parts of a toughening agent, 610-30 parts of copolymerized nylon and 0.2-2 parts of a processing aid; the toughening agent comprises at least one of POE, maleic anhydride grafted ethylene propylene diene monomer rubber and ethylene-ethyl acrylate copolymer;
the mass ratio of the component A to the component B is (5-7.5): (2.5-5).
2. The low temperature impact resistant polypropylene composition of claim 1, wherein the toughening agent is a mixture of POE and maleic anhydride grafted POE.
3. The low temperature impact resistant polypropylene composition according to claim 2, wherein the grafting ratio of the maleic anhydride grafted POE in the toughening agent is 0.8-1.0%.
4. The low temperature impact resistant polypropylene composition according to claim 2, wherein the mass ratio of POE to maleic anhydride grafted POE is (2-4): 1.
5. The low temperature impact resistant polypropylene composition according to claim 1, wherein the polypropylene in the component A and the component B is a polypropylene copolymer, and the melt index of the polypropylene in the component A and the component B is not less than 80g/10min at 230 ℃ under a load of 2.16 kg.
6. The low temperature impact resistant polypropylene composition according to claim 1, wherein the compatibilizer is at least one of maleic anhydride grafted polypropylene, acrylic acid grafted polypropylene, and glycidyl acrylate grafted polypropylene.
7. A process for preparing a low temperature impact resistant polypropylene composition according to any one of claims 1 to 6, comprising the steps of:
(1) preparation of component A: uniformly mixing the polypropylene, the compatilizer and the processing aid in the component A according to a ratio, putting the mixture into a double-screw extruder, then putting the long glass fiber subjected to pre-dispersion treatment, and performing melt extrusion granulation to obtain a component A;
(2) preparation of the component B: uniformly mixing all the components in the component B according to the proportion, and putting the mixture into a double-screw extruder for melt extrusion granulation to obtain the component B;
(3) and uniformly mixing the component A and the component B according to the proportion, melting, extruding and granulating to obtain the low-temperature impact resistant polypropylene composition.
8. The method for preparing the low temperature impact resistant polypropylene composition according to claim 7, wherein the temperature of the twin-screw extruder in the step (1) during melt extrusion granulation is 210-250 ℃, the component A enters an infiltration die head in the twin-screw extruder, and the temperature of the infiltration die head is 270-320 ℃; the temperature of the double-screw extruder in the step (2) during melt extrusion granulation is 210-250 ℃; and (3) the temperature of the double-screw extruder in the step (3) is 210-250 ℃ during melt extrusion granulation.
9. Use of the low temperature impact resistant polypropylene composition according to any one of claims 1 to 6 for the preparation of packaging boxes for military materials.
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| 李祖德主编: "《塑料加工技术应用手册》", 中国物资出版社 * |
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