CN115785572B - Super thermo-oxidative aging resistant polypropylene composition and preparation method and application thereof - Google Patents
Super thermo-oxidative aging resistant polypropylene composition and preparation method and application thereof Download PDFInfo
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- CN115785572B CN115785572B CN202211607013.6A CN202211607013A CN115785572B CN 115785572 B CN115785572 B CN 115785572B CN 202211607013 A CN202211607013 A CN 202211607013A CN 115785572 B CN115785572 B CN 115785572B
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- 230000032683 aging Effects 0.000 title claims abstract description 64
- -1 polypropylene Polymers 0.000 title claims abstract description 56
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 54
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 54
- 239000000203 mixture Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000003822 epoxy resin Substances 0.000 claims abstract description 31
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 31
- 239000003365 glass fiber Substances 0.000 claims abstract description 24
- 229920006150 hyperbranched polyester Polymers 0.000 claims abstract description 23
- 239000003963 antioxidant agent Substances 0.000 claims description 20
- 230000003078 antioxidant effect Effects 0.000 claims description 19
- 238000012360 testing method Methods 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 229920001112 grafted polyolefin Polymers 0.000 claims description 2
- 229920001910 maleic anhydride grafted polyolefin Polymers 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 2
- 235000013824 polyphenols Nutrition 0.000 claims description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229920005629 polypropylene homopolymer Polymers 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 19
- 238000007667 floating Methods 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 18
- 230000014759 maintenance of location Effects 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 6
- 229920005989 resin Polymers 0.000 abstract description 6
- 239000011347 resin Substances 0.000 abstract description 6
- 230000007774 longterm Effects 0.000 abstract description 4
- 239000002861 polymer material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 238000011056 performance test Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 230000001590 oxidative effect Effects 0.000 description 6
- 230000006866 deterioration Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 230000003712 anti-aging effect Effects 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 239000004842 bisphenol F epoxy resin Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical group O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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Abstract
The application discloses a super thermo-oxidative aging resistant polypropylene composition, a preparation method and application thereof, and relates to the field of high polymer materials. The super thermo-oxidative aging resistant polypropylene composition comprises polypropylene, glass fiber, compatilizer, epoxy resin and hydroxyl-terminated hyperbranched polyester; the molecular weight of the hydroxyl-terminated hyperbranched polyester is 500-1300; the molecular weight of the epoxy resin is 800-2000. The application utilizes hyperbranched polyester and epoxy resin to react in the aging process, gradually migrates to the surface of the material in the aging process and gradually fills gaps between the resin matrix and glass fiber to form good combination, can greatly improve the thermo-oxidative aging performance of the system, and has the performance retention rate reaching more than 90% after long-term high-temperature aging, and meanwhile, the floating fiber on the surface of the material is greatly improved in the aging process.
Description
Technical Field
The application relates to the field of high polymer materials, in particular to a super thermo-oxidative aging resistant polypropylene composition, and a preparation method and application thereof.
Background
Compared with other general plastics, polypropylene (PP) has the advantages of good mechanical property, small density, good rigidity, high strength, good electrical insulation property and the like, but because the polypropylene contains unstable tertiary carbon groups, the polypropylene is easy to be attacked by heat and oxygen to cause performance deterioration, such as yellowing, surface cracking and pulverization, and the mechanical property is greatly reduced, so that a plurality of products have long-term thermo-oxidative aging resistance requirements on the polypropylene.
At present, the method for improving the ageing performance of a polypropylene system is commonly used, such as adding an efficient antioxidant, compounding a plurality of antioxidants, loading the antioxidant, adding high molecular weight hindered amine and the like, but has limited heat ageing resistance. In addition, the epoxy resin is added into the system, and the surface of the polypropylene composition is covered by the epoxy resin with low melting point and high fluidity so as to achieve the anti-aging effect. However, the inventor adds epoxy resin into the glass fiber reinforced polypropylene material, and the same anti-aging effect cannot be achieved; and aiming at the glass fiber reinforced polypropylene material, the surface floating fiber is easy to deteriorate in the aging process, and the phenomenon of surface floating fiber deterioration in the aging process is difficult to overcome by the conventional thermo-oxidative aging technology.
Disclosure of Invention
The application provides a super thermo-oxidative aging resistant polypropylene composition, a preparation method and application thereof, which are used for improving thermo-oxidative aging resistant performance of a material and improving the problem of surface floating fiber deterioration of the material in the thermo-oxidative aging process.
In order to solve the technical problems, one of the purposes of the application is to provide a super thermo-oxidative aging resistant polypropylene composition, which comprises the following components in parts by weight:
polypropylene: 44-89 parts;
glass fiber: 5-40 parts;
and (3) a compatilizer: 0.5-2 parts;
epoxy resin: 2-5 parts;
hydroxyl-terminated hyperbranched polyesters: 2-5 parts;
wherein the molecular weight of the hydroxyl-terminated hyperbranched polyester is 500-1300; the molecular weight of the epoxy resin is 800-2000.
By adopting the scheme, the hyperbranched polyester with proper molecular weight and the epoxy resin are added into the formula system, the added hyperbranched polyester reacts with the epoxy resin in the aging process, and reacts with the epoxy resin, and gradually migrates to the surface of the material in the aging process and gradually fills gaps between the resin matrix and the glass fiber, the hyperbranched polyester with molecular weight has strong migration capability in the system to form good combination, the thermal oxidation aging performance of the system can be greatly improved, the performance retention rate still reaches more than 90% after long-term high-temperature aging, and meanwhile, the floating fiber on the surface of the material is also greatly improved in the aging process.
Preferably, the epoxy resin is one or more of bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol type glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin and aliphatic glycidyl ester epoxy resin.
Preferably, the weight part of the glass fiber is 10-25 parts.
As a preferable scheme, the polypropylene is copolymerized polypropylene and/or homopolymerized polypropylene, and the melt mass flow rate of the polypropylene under the test condition of 230 ℃ and 2.16kg is 0.5-100g/10min.
Preferably, the compatilizer is maleic anhydride grafted polyolefin or acrylic acid grafted polyolefin, and the grafting rate is 0.1-2%.
Preferably, the composition further comprises 0.1 to 0.5 part by weight of an antioxidant.
Preferably, the antioxidant is hindered phenol antioxidant and/or phosphite antioxidant.
Preferably, the hindered phenol antioxidant is 1010, and the phosphite antioxidant is 168.
Preferably, the hydroxyl-terminated hyperbranched polyester is a fatty hyperbranched polyester.
Preferably, the hydroxyl-terminated hyperbranched polyester has 4 to 12 hydroxyl-terminated groups.
In order to solve the above technical problems, a second object of the present application is to provide a polypropylene composition with super thermo-oxidative aging resistance, comprising the steps of:
(1) Weighing other components except glass fiber, adding into high-speed mixing equipment, mixing for 1-3 min at 1000-2000 rpm to obtain premix;
(2) The premix is added through a main feeding port of double-screw extrusion equipment, glass fibers are added through a side feeding port, the temperature of each area of the screw is 190-230 ℃, and the polypropylene composition is obtained through vacuum extrusion granulation.
In order to solve the above technical problems, a third object of the present application is to provide an application of a polypropylene composition with super thermo-oxidative aging resistance in the field of automobile parts, such as automobile engine peripheral parts and the like.
Compared with the prior art, the embodiment of the application has the following beneficial effects:
the application utilizes the reaction of hydroxyl-terminated hyperbranched polyester and epoxy resin in the aging process, gradually migrates to the surface of the material in the aging process and gradually fills gaps between the resin matrix and the glass fiber to form good combination, can greatly improve the thermo-oxidative aging performance of the system, and has the performance retention rate reaching more than 90% after long-term high-temperature aging, and meanwhile, the floating fiber on the surface of the material is greatly improved in the aging process.
Drawings
Fig. 1: the surface of the super heat oxidation resistant polypropylene composition is free from fiber floating;
fig. 2: a surface light fiber floating condition of the super heat oxidation resistant polypropylene composition of the present application;
fig. 3: the surface of the super heat-resistant oxidation polypropylene composition is obviously fiber floating;
fig. 4: is a surface severe fiber-floating condition of the super heat-resistant oxidation polypropylene composition of the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Table 1 below shows the sources of the raw materials in the examples and comparative examples of the present application, and the antioxidant and glass fiber were obtained commercially, and the same antioxidant and glass fiber were used in the parallel test, unless otherwise specified.
TABLE 1 sources and performance parameters of the raw materials in examples and comparative examples of the present application
Examples 1 to 9
A super thermo-oxidative aging resistant polypropylene composition is shown in table 2, and comprises polypropylene, glass fiber, compatilizer, epoxy resin, hydroxyl-terminated hyperbranched polyester and antioxidant; the epoxy resin is bisphenol A type epoxy resin, and the compatilizer is maleic anhydride grafted PP; the antioxidant is 1010 and 168 with the mass ratio of 1: 1.
TABLE 2 Components and contents in examples 1-9 and comparative examples 1-7
The preparation method of the super thermo-oxidative aging resistant polypropylene composition comprises the following steps:
(1) Weighing other components except glass fiber according to the weight ratio, adding the components into a high-speed mixer for mixing for 3 minutes at the rotating speed of 2000 rpm to obtain premix;
(2) The premix is added through a main feeding port of a double-screw extruder, the glass fiber is added through a side feeding port, the temperature of each area of the screw is 190-230 ℃, and the polypropylene composition is obtained through vacuum extrusion granulation.
Performance test
1. Tensile strength retention before and after aging: the heat aging test box is selected according to the GB/T7141-2008 method B, the temperature of the oven is set to be 150 ℃, and the ventilation amount of the oven is controlled to be 5-20 times/h; the polypropylene composition particles are injected into GB T1040 standard dumbbell type tensile bars in an injection molding machine, and the injection molding temperature is 200 ℃; the date T0 of putting the sample is recorded, the date T1 of taking out is recorded after aging for a period of time, the aging time is T1-T0, the aging time is 720h, 1500h and 2500h, the tensile strength T1 and T2 of the sample bar are respectively tested at T0 and T1, the retention rate of the tensile strength is T2/T1 x 100%, the tensile strength is tested according to ISO 527-1-1993, and the test results are shown in Table 3.
2. Surface fiber floating condition: while the tensile strength retention test before and after aging was performed, the fiber floating state of the surface before and after aging of the sample bar was observed, the fiber floating-free state was shown in fig. 1, the slightly fiber floating state was shown in fig. 2, the clearly fiber floating state was shown in fig. 3, the severely fiber floating state was shown in fig. 4, and the fiber floating state was recorded as shown in table 3.
3. Flexural modulus: the GB/T9341-2008 standard was used to test polypropylene compositions, test samples were prepared according to the standard, and the test results are shown in Table 3.
TABLE 3 Performance test results for examples 1-9 and comparative examples 1-7
As can be seen from the performance detection results of the embodiment 1 and the comparative examples 1-3 in the table 3, the hydroxyl-terminated hyperbranched polyester and the epoxy resin react in the aging process and react with the epoxy resin, gradually migrate to the surface of the material in the aging process and gradually fill gaps between the resin matrix and the glass fiber to form good combination, so that the thermo-oxidative aging performance of the system can be greatly improved, meanwhile, the floating fiber on the surface of the material is greatly improved in the aging process, the retention rate of the finally obtained polypropylene composition reaches over 83% after 2500h, and the flexural modulus reaches over 1150 MPa.
As can be seen from the performance test results of examples 1 and 9 and comparative example 4 in Table 3, the hyperbranched polyester with smaller molecular weight has strong migration capability in the system, the hydroxyl-terminated hyperbranched polyester with larger molecular weight has difficult migration in the aging process of the material, and the gap between the resin matrix of the material and the glass fiber is difficult to fill, so that the effects of resisting thermal oxidation aging and improving surface floating fiber deterioration are not achieved.
As is clear from the results of the performance test of example 1 and comparative example 5 in Table 3, when the amount of the epoxy resin or the hydroxyl-terminated hyperbranched polyester added is insufficient, the gap filler migrating between the resin matrix and the glass fiber is insufficient, resulting in insufficient thermal oxidative aging resistance, and the ability to improve the deterioration of the surface float is not obvious.
As can be seen from the results of performance tests of example 1 and comparative example 6 in Table 3, when the molecular weight of the epoxy resin is 800-2000, the migration ability is stronger when the epoxy resin and the hydroxyl-terminated hyperbranched polyester interact and migrate together in the aging process, and finally, the material is superior in thermal oxidative aging resistance and the surface floating fiber improvement effect is better.
From the results of the performance tests of examples 1 and 8 and comparative example 7 in Table 3, it was found that the addition of the antioxidant has little effect on the flexural modulus, but can slightly improve the thermal oxidative aging resistance of the polypropylene composition, but has limited improvement ability, and when the hydroxyl-terminated hyperbranched polyester is not added, the antioxidant having a higher content cannot improve the thermal oxidative aging resistance of the polypropylene composition, and the thermal oxidative aging resistance is decreased linearly with the disappearance of the efficacy of the antioxidant.
As can be seen from the performance test results of examples 1 and 5-7 in Table 3, the glass fiber has an enhanced effect on the material, so that the flexural modulus of the material is improved, and when the addition amount of the glass fiber is controlled to be 10-25kg, the rigidity and the thermal oxidative aging resistance of the material can be ensured to meet higher standards, and the comprehensive performance is improved.
The foregoing embodiments have been provided for the purpose of illustrating the general principles of the present application, and are not to be construed as limiting the scope of the application. It should be noted that any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art without departing from the spirit and principles of the present application are intended to be included in the scope of the present application.
Claims (10)
1. The super thermo-oxidative aging resistant polypropylene composition is characterized by comprising the following components in parts by weight:
polypropylene: 44-89 parts;
glass fiber: 5-40 parts;
and (3) a compatilizer: 0.5-2 parts;
epoxy resin: 2-5 parts;
hydroxyl-terminated hyperbranched polyesters: 2-5 parts;
wherein the molecular weight of the hydroxyl-terminated hyperbranched polyester is 500-1300, and the molecular weight of the epoxy resin is 800-2000.
2. The super thermo-oxidative aging resistant polypropylene composition according to claim 1, wherein the epoxy resin is one or more of bisphenol a type epoxy resin, bisphenol F type epoxy resin, polyphenol type glycidyl ether epoxy resin, aliphatic glycidyl ester epoxy resin.
3. The super thermo-oxidative aging polypropylene composition according to claim 1, wherein the glass fiber is 10 to 25 parts by weight.
4. The super thermo-oxidative aging resistant polypropylene composition according to claim 1, wherein the polypropylene is a copolymerized polypropylene and/or a homo-polypropylene, and the polypropylene has a melt mass flow rate of 0.5-100g/10min at 230 ℃ under 2.16kg test conditions.
5. The super thermo-oxidative aging resistant polypropylene composition according to claim 1, wherein the compatibilizer is a maleic anhydride grafted polyolefin or an acrylic acid grafted polyolefin having a grafting ratio of 0.1 to 2%.
6. The super thermo-oxidative aging resistant polypropylene composition according to claim 1, further comprising 0.1 to 0.5 parts by weight of an antioxidant.
7. The super thermo-oxidative aging resistant polypropylene composition according to claim 6, wherein the antioxidant is a hindered phenol antioxidant and/or a phosphite antioxidant.
8. The super thermo-oxidative aging resistant polypropylene composition according to claim 1, wherein the hydroxyl-terminated hyperbranched polyester is a aliphatic hyperbranched polyester having a hydroxyl-terminated number of 4 to 12.
9. A process for preparing a super thermo-oxidative aging resistant polypropylene composition according to any one of claims 1 to 8, comprising the steps of:
(1) Weighing other components except glass fiber, adding into high-speed mixing equipment, mixing for 1-3 min at 1000-2000 rpm to obtain premix;
(2) The premix is added through a main feeding port of double-screw extrusion equipment, glass fibers are added through a side feeding port, the temperature of each area of the screw is 190-230 ℃, and the polypropylene composition is obtained through vacuum extrusion granulation.
10. Use of a super thermo-oxidative aging resistant polypropylene composition according to any one of claims 1 to 8 in the field of automotive parts.
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CN101098923A (en) * | 2005-01-14 | 2008-01-02 | 巴斯福股份公司 | Flowable polyolefins |
CN106633398A (en) * | 2016-12-18 | 2017-05-10 | 合肥会通新材料有限公司 | Anti-floating fire, heat-resistant and anti-aging polypropylene material and a preparation method thereof |
CN109762247A (en) * | 2018-12-25 | 2019-05-17 | 合肥卡洛塑业科技有限公司 | A kind of high heat resistance oxygen aging glass fiber reinforced polypropylene composite material and preparation method thereof |
CN110452456A (en) * | 2019-07-22 | 2019-11-15 | 南京聚隆科技股份有限公司 | A kind of high weld strength long glass fiber reinforced polypropylene material and preparation method thereof |
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US6673870B2 (en) * | 2002-05-13 | 2004-01-06 | The Procter & Gamble Company | Compositions of polyolefins and hyperbranched polymers with improved tensile properties |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101098923A (en) * | 2005-01-14 | 2008-01-02 | 巴斯福股份公司 | Flowable polyolefins |
CN106633398A (en) * | 2016-12-18 | 2017-05-10 | 合肥会通新材料有限公司 | Anti-floating fire, heat-resistant and anti-aging polypropylene material and a preparation method thereof |
CN109762247A (en) * | 2018-12-25 | 2019-05-17 | 合肥卡洛塑业科技有限公司 | A kind of high heat resistance oxygen aging glass fiber reinforced polypropylene composite material and preparation method thereof |
CN110452456A (en) * | 2019-07-22 | 2019-11-15 | 南京聚隆科技股份有限公司 | A kind of high weld strength long glass fiber reinforced polypropylene material and preparation method thereof |
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