CN114479289B - Scratch-resistant polypropylene composite material with high impact resistance and high stripping performance, and preparation method and application thereof - Google Patents
Scratch-resistant polypropylene composite material with high impact resistance and high stripping performance, and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a scratch-resistant polypropylene composite material with high impact resistance and high stripping performance, and a preparation method and application thereof. The polypropylene comprises the following components in parts by weight: 100 parts of polypropylene copolymer, 0-55 parts of filler, 5-25 parts of special auxiliary agent, 10-55 parts of flexibilizer, 0.01-0.1 part of scratch resistant agent, 0.1-1 part of lubricant and 0.1-1 part of antioxidant, wherein the special auxiliary agent is high-density polyethylene grafted maleic anhydride. According to the invention, the high-density polyethylene with specific density and the maleic anhydride are selected for grafting, and are added into the polypropylene material, so that the negative influence of the polarity of the scratch-resistant agent on the peeling strength can be reduced, the scratch-resistant performance and the peeling strength of the polypropylene material can be improved at the same time, and meanwhile, the specific copolymerized polypropylene is used as a matrix, so that the impact strength of the material can be improved on the basis of not reducing the scratch-resistant performance and the peeling strength.
Description
Technical Field
The invention belongs to the field of high polymer material modification, and in particular relates to a scratch-resistant polypropylene composite material with high impact resistance and high stripping performance, and a preparation method and application thereof.
Background
The polypropylene has the characteristics of low density, high cost performance, excellent heat resistance, rigidity, chemical corrosion resistance, easy processing, forming, recycling and the like, is widely applied to automobiles, and becomes the variety with the largest dosage and the fastest development speed in the plastic for automobiles. However, in different application scenarios, higher requirements are put on different properties of polypropylene materials. When the polypropylene material is used for automotive interior products, the scratch resistance of the material has higher requirements, however, the surface of the polypropylene is easily scratched by external force, so that the appearance of the product is greatly affected, and the wide application of the product is limited; when used in automotive exterior trim products, there is a need for better coatability (e.g., higher peel strength or adhesion to paint).
The existing method for modifying the scratch resistance is to blend and add scratch resistant agent into polypropylene material, such as Chinese patent CN107075010A, to improve the scratch resistance of polypropylene material by adding high-density polyethylene, but the high crystallinity and nonpolar of high-density polyethylene have a certain negative effect on the coating peel strength of polypropylene composite material; CN109705467a forms a protective film on the surface by adding phosphate and amide wax, which improves the coating adhesion of the material, but does not improve the scratch resistance.
Therefore, the existing polypropylene material needs to be independently modified according to different performances in different application scenes, so that the polypropylene material has single function and brings great inconvenience to application.
At present, although there is also research on comprehensive improvement of scratch resistance and coating performance, for example, patent CN113321869a, which selects ultra-high molecular weight grafted glycidyl methacrylate as a special auxiliary agent and improves the scratch resistance and coating performance of polypropylene, the ultra-high molecular weight polyethylene has high selling price, which clearly increases the production cost to a certain extent, so in order to reduce the production cost, a new auxiliary agent is needed to be provided, and the production cost is reduced while improving the scratch resistance and coating performance of polypropylene; at the same time, the impact properties of the composite material are still to be improved.
And along with the importance of people on the product performance, the polypropylene material has higher requirements on the performance, and besides good scratch resistance and high peel strength, the polypropylene material also has higher impact resistance, so that the polypropylene material has good impact resistance when being used for automobile interior decoration, and can reduce the damage to human bodies to a greater extent when the automobile is impacted.
Disclosure of Invention
The invention aims to overcome the defects of single function and high production cost of the existing polypropylene material and provide the scratch-resistant polypropylene composite material with high impact resistance and high stripping performance, wherein the scratch-resistant polypropylene composite material has better scratch resistance, coating performance and impact performance.
The invention also aims at providing a preparation method of the scratch-resistant polypropylene composite material with high impact resistance and high peeling property.
The invention also aims to provide the application of the scratch-resistant polypropylene composite material with high impact resistance and high peeling property in preparing automobile parts.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the scratch-resistant polypropylene composite material with high impact resistance and high peeling property comprises the following components in parts by weight:
wherein the copolymerized polypropylene is an ethylene-propylene copolymer with the crystallinity of 75-80%; the special auxiliary agent is high-density polyethylene grafted maleic anhydride, and in the high-density polyethylene grafted maleic anhydride, the grafting rate of the maleic anhydride is 0.2-2wt%; in the high-density polyethylene grafted maleic anhydride, the density of the high-density polyethylene is 0.950-0.960 g/cm 3 。
The crystallinity of the polypropylene copolymer of the present invention was measured by the X-ray diffraction method of Standard SH/T1827-2019.
High density polyethylene grafted maleic anhydride (HDPE-g-MAH), commonly used as a surfactant for fillers, is used to improve the dispersibility of the filler in the matrix, but the inventors creatively found that, if it is added to a polypropylene material, it can not only play a role of dispersing the filler, but also reduce the negative effect of the polarity of the scratch-resistant agent on the peel strength, thereby being capable of simultaneously improving the scratch-resistant performance and the peel strength of the polypropylene material, and the cost thereof is far lower than that of the ultra-high molecular weight polyethylene used in CN113321869a, thus greatly reducing the production cost of the material.
For High Density Polyethylene (HDPE), it is known that varying the density results in HDPE having different properties. The inventor further researches a lot of experiments show that only the high-density polyethylene with specific density is selected to be grafted with maleic anhydride and added into the polypropylene material, the polypropylene material with excellent scratch resistance can be obtained under the addition of less amount of scratch resistant agent, and the influence of the less amount of scratch resistant agent on the peel strength and mechanical property of the composite material can be further reduced; meanwhile, the grafting rate of maleic anhydride also affects the scratch resistance and the peeling strength of the finally prepared polypropylene material.
Under the condition of meeting the scratch resistance and the peeling strength, the inventor of the invention discovers that the obtained composite material has excellent impact performance at the same time by further research, for example, by selecting the copolymer polypropylene with specific ethylene content as a matrix. This is because, in the ethylene-propylene copolymer polypropylene, the random arrangement of ethylene and propylene disturbs the regularity of the molecular chain structure, and therefore crystalline regions and non-crystalline regions are formed in the copolymer, the non-crystalline regions being soft rubber phases uniformly dispersed in the pores of the crystalline regions, the rubber phases providing impact resistance. The high-density polyethylene chain segment in the HDPE-g-MAH and the polyethylene chain segment in the copolymerized polypropylene have good compatibility, so that the HDPE-g-MAH is uniformly dispersed in the polypropylene matrix, and the mechanical properties, especially the toughness (namely the impact resistance) of the composite material are further improved; further, the synergistic effect of the rubber phase in the polypropylene copolymer, the HDPE-g-MAH and the toughening agent can obviously improve the impact performance of the composite material. Regarding the content of the rubber phase in the polypropylene copolymer, it was found that if the content of the rubber phase is too low (i.e., the crystallinity is too high), the impact strength of the composite material is low; with the increase of the content of the rubber phase, the impact strength of the composite material gradually increases, but when the content of the rubber phase increases to a certain extent, the scratch resistance and rigidity of the composite material are reduced, so that the scratch-resistant polypropylene composite material with high impact resistance and high peeling property, which has good scratch resistance, coating property and impact property, can be obtained only by taking the ethylene-propylene copolymer with the proper content of the rubber phase as a matrix.
In order to further improve the scratch resistance and the peel strength of the polypropylene material, the grafting ratio of the maleic anhydride is more preferably 0.8 to 1.5wt%.
Preferably, the density of the high-density polyethylene is 0.954-0.956 g/cm 3 。
The high-density polyethylene grafted maleic anhydride can be prepared by a grafting method which is conventional in the prior art.
In the prior art, a melt grafting method is generally adopted to prepare high-density polyethylene grafted maleic anhydride, and the method specifically comprises the following steps:
s1, carrying out melt grafting on high-density polyethylene, maleic anhydride and an initiator at 160-200 ℃ to obtain a grafting mixture containing high-density polyethylene grafted maleic anhydride;
s2, adding dimethylbenzene into the grafting mixture obtained in the step S1 to purify the high-density polyethylene grafted maleic anhydride, and obtaining the high-density polyethylene grafted maleic anhydride after precipitation, filtration, drying and granulation;
wherein, in the step S1, the weight ratio of the high-density polyethylene to the maleic anhydride to the initiator is 50-65:0.6-1.8:0.4-1.6.
Preferably, the initiator is a peroxide initiator, more preferably di-t-butyl peroxide (DTBP).
Preferably, the time of melt grafting is 15 to 30 minutes.
It should be noted that conventional commercially available high density polyethylene can be used in the present invention to prepare the high density polyethylene grafted maleic anhydride.
Preferably, the toughening agent is an ethylene-alpha-olefin random copolymer (also known as POE).
Preferably, the scratch resistant agent is an amide type scratch resistant agent.
Further preferably, the scratch resistant agent is one or a combination of two of erucamide or oleamide.
Preferably, the filler is one or a combination of a plurality of talcum powder, calcium carbonate or basic magnesium sulfate whiskers. The addition of filler may increase the stiffness and modulus of the composite material, and further preferably the filler is basic magnesium sulfate whisker.
Preferably, the lubricant is stearate.
Further preferably, the stearate is one or a combination of several of zinc stearate, calcium stearate or magnesium stearate.
Preferably, the antioxidant is a hindered phenol antioxidant and/or a phosphite antioxidant.
Further preferably, the hindered phenol antioxidant is antioxidant 1010; the phosphite antioxidant is antioxidant 168.
The preparation method of the scratch-resistant polypropylene composite material with high impact resistance and high peeling property comprises the following steps:
the polypropylene, the filler, the special auxiliary agent, the toughening agent, the scratch resistant agent, the lubricant and the antioxidant are uniformly mixed according to a proportion, and then the mixture is prepared by melt extrusion, wherein the temperature of the melt extrusion is 170-210 ℃.
Preferably, the melt extrusion is performed by a 75D co-rotating twin-screw extruder, wherein the twin-screw extruder comprises a feeding section and a machine head, and the feeding section is sequentially 170 ℃, 200 ℃, 210 ℃, 205 ℃, 200 ℃ and 200 ℃.
The scratch-resistant polypropylene composite material with high impact resistance and high stripping performance is applied to the preparation of automobile parts.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the high-density polyethylene grafted maleic anhydride as a special additive to be added into the polypropylene material, so that the negative influence of the polarity of the scratch-resistant agent on the peeling strength can be reduced, the scratch-resistant performance and the peeling strength of the polypropylene material can be improved at the same time, the scratch-resistant performance can reach delta L less than 0.4 and the coating peeling strength can reach more than or equal to 1000gf/cm under the addition of a small amount of the scratch-resistant agent, and the specific copolymerized polypropylene is taken as a matrix, and the impact strength is 40kJ/m 2 Above, up to 58kJ/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The production process is simple, the production cost is low, and the method can simultaneouslyIs suitable for polypropylene matrix with wider melt index, and is beneficial to mass production.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art. The reagents and materials used in the present invention are commercially available unless otherwise specified.
The embodiment of the invention adopts the following raw materials:
ordinary polypropylene PP:
PP-1: copolymerized polypropylene, BX3900, having a crystallinity of 78%, purchased from korean elsen;
PP-2: copolymerized polypropylene, EP300M, with crystallinity of 77%, purchased from mesosea shell;
PP-3: copolymerized polypropylene, BX3950, having crystallinity of 79%, purchased from Korean Aisi Kai
PP-4: copolymerized polypropylene, EP246P, with crystallinity of 60%, available from bassell;
PP-5: homo polypropylene, H9018, purchased from lanzhou petrochemical;
and (3) filling:
calcium carbonate: 75T, purchased from chang omega;
whisker: WS-1S2 (basic magnesium sulfate whisker), available from Yingkoukang such as science and technology;
talc powder: TYT-777A (3000 mesh talc) was purchased from Liaoning additive source;
toughening agent:
POE: are commercially available;
scratch resistance agent:
erucamide: purchased from kappaphycus alvarezii chemical industry;
oleic acid amide: purchased from kappaphycus alvarezii chemical industry;
an antioxidant:
antioxidant 1010: are commercially available;
antioxidant 168: are commercially available;
and (3) a lubricant:
zinc stearate: are commercially available;
high density polyethylene:
HDPE-1: paxon AB50-003, density 0.950g/cm 3 Purchased from exxon mobil;
HDPE-2: paxon FD60-018, density 0.954g/cm 3 Purchased from exxon mobil;
HDPE-3: paxon BA54-030, density 0.956g/cm 3 Purchased from exxon mobil;
HDPE-4: HD 7957.04, density 0.960g/cm 3 Purchased from exxon mobil;
HDPE-5: paxon AA45-004 with a density of 0.945g/cm 3 Purchased from exxon mobil;
HDPE-6: paxon AA60-003, density 0.963g/cm 3 Purchased from exxon mobil;
maleic anhydride: purchased from shandong sink chemical company, inc;
di-tert-butyl peroxide: are commercially available;
the toughening agent, the lubricant and the di-t-butyl peroxide in the examples and comparative examples of the present invention are the same.
In the invention, the high-density polyethylene grafted maleic anhydride is prepared by the following method:
s1, performing melt grafting on high-density polyethylene, maleic anhydride and initiator di-tert-butyl peroxide according to the weight ratio of 50-65:0.6-1.8:0.4-1.6 at 160-180 ℃ for 15-30 min to obtain a grafting mixture containing high-density polyethylene grafted maleic anhydride;
s2, adding dimethylbenzene into the grafting mixture obtained in the step S1 to purify the high-density polyethylene grafted maleic anhydride, and obtaining the high-density polyethylene grafted maleic anhydride after precipitation, filtration, drying and granulation;
the grafting maleic anhydride of the high-density polyethylene with different grafting rates of the maleic anhydride can be obtained by adjusting the proportion of raw materials, the reaction temperature and the reaction time, wherein the grafting rate is the ratio of the maleic anhydride grafted onto the high-density polyethylene to the total mass of the high-density polyethylene participating in the reaction.
Details are shown in Table 1.
TABLE 1 formulation of high density polyethylene grafted maleic anhydride
Examples 1 to 20
This example provides a series of scratch resistant polypropylene composites with high impact and high peel properties, prepared according to the formulation in tables 2-4, according to a preparation method comprising the steps of:
s1, mixing polypropylene, a filler, a special auxiliary agent, a toughening agent, a scratch resistant agent, a lubricant and an antioxidant in a high-speed mixer for 5min according to the proportion of tables 2-4, wherein the rotating speed of the high-speed mixer is 800r/min, and uniformly mixing to obtain a mixture;
s2, melting, extruding and granulating the mixture obtained in the step S1 in a 75D homodromous double-screw extruder at 170-210 ℃ (the temperature from a feeding section to a machine head of the double-screw extruder is 170 ℃, 200 ℃, 210 ℃, 205 ℃, 200 ℃ and 200 ℃).
Table 2 the content (parts by weight) of the components in the scratch-resistant polypropylene composites of examples 1 to 9 having high impact resistance and high peel properties
TABLE 3 high impact, high peel scratch resistant Polypropylene composite of examples 10-14 content of the components (parts by weight)
TABLE 4 high impact, high peel scratch resistant Polypropylene composite of examples 15-20 the content of the components (parts by weight)
Comparative example 1
This comparative example differs from example 1 in that no special auxiliary agent, high density polyethylene grafted maleic anhydride, was added.
Comparative example 2
This comparative example differs from example 1 in that the high density polyethylene grafted maleic anhydride was replaced with 20.83 parts of high density polyethylene HDPE-1 and 4.17 parts of maleic anhydride.
Comparative example 3
This comparative example differs from example 1 in that the high density polyethylene grafted maleic anhydride was replaced with high density polyethylene HDPE-1.
Comparative example 4
This comparative example differs from example 1 in that the high density polyethylene grafted maleic anhydride was replaced with maleic anhydride.
Comparative example 5
This comparative example differs from example 1 in that the special auxiliary agent was replaced by B1.
Comparative example 6
This comparative example differs from example 1 in that the special auxiliary agent was replaced by B2.
Comparative example 7
This comparative example differs from example 1 in that the special auxiliary agent was replaced by B3.
Comparative example 8
This comparative example differs from example 1 in that the special auxiliary agent was replaced by B4.
Comparative example 9
This comparative example differs from example 1 in that polypropylene is replaced with polypropylene PP-4 having a lower crystallinity.
Comparative example 10
This comparative example differs from example 1 in that the polypropylene is replaced by homo-polypropylene PP-5.
Performance testing
The polypropylene prepared in the above examples and comparative examples was tested for scratch resistance and peel strength as follows:
1. scratch resistance: the test was performed according to the PV3952-2019-03 standard of the mass host factory, with a 10N load, and a Ford STUCCO texture panel, wherein the smaller the DeltaL value, the better the scratch resistance.
2. Peel strength test: testing according to standard NES M0141-2006-1 of Nissan of Dongfeng;
3. impact strength test: testing according to ISO 180-2000, wherein the notch type is A-type notch;
the test results are shown in Table 5.
TABLE 5 Performance test results
As can be seen from table 5:
the polypropylene composite material prepared by the embodiment of the invention has higher scratch resistance and better coating property (peeling strength) and impact strength under the addition of less amount of scratch resistant agent, wherein the scratch resistance is delta L<0.4, the peel strength is more than or equal to 1000gf/cm, and the impact strength is 40kJ/m 2 Above, up to 58kJ/m 2 Can meet the performance use requirements of the automobile parts.
The comparative results of examples 1-6 show that the scratch resistance and the peel strength of the prepared polypropylene composite material are improved simultaneously under the synergistic effect of the special auxiliary agent and the scratch resistant agent; the comparison results of examples 1, 7-9 and 12-13 show that the types and contents of other additives (such as filler, lubricant, toughening agent, antioxidant and the like) in the polypropylene composite material have little influence on the scratch resistance and the peeling strength of polypropylene; comparison of example 1 with examples 10-11 shows that polypropylene of different melt index can be used in the present invention with less impact of the melt index of the polypropylene matrix on scratch and peel strength; the comparison of the results of the example 1 and the example 14 shows that the amide scraping resistant agent can be used in the invention to cooperate with special auxiliary agents to obtain polypropylene with better scraping resistant performance and peeling strength.
The comparative results of examples 1, 15-20 and comparative examples 5-8 show that the density of the high-density polyethylene in the special auxiliary agent and the grafting ratio of maleic anhydride have a great influence on the scratch resistance and the peel strength of the polypropylene composite material:
the special auxiliary agent HDPE-g-MAH with different maleic anhydride grafting rates is selected in the embodiment 1 and the embodiment 15-17, and the scratch resistance of the material is improved firstly and then reduced along with the increase of the maleic anhydride grafting rate, and the peeling strength is in an improved trend, so that the maleic anhydride grafting rate of the special auxiliary agent needs to be kept within a certain range in order to ensure that the polypropylene composite material has better scratch resistance and peeling strength; in the comparative example 7, a special auxiliary agent with lower maleic anhydride grafting rate is selected, and the prepared polypropylene composite material has poorer scratch resistance and peeling strength; the comparative example 8 selects a special auxiliary agent with higher maleic anhydride grafting rate, and the prepared polypropylene composite material has obviously improved peel strength but obviously reduced scratch resistance.
In the embodiment 1 and the embodiment 18-20, the special auxiliary agent HDPE-g-MAH prepared from the high-density polyethylene with different densities is selected, and the fact that the prepared special auxiliary agent is added into the polypropylene material within the density range of the invention can improve the scratch resistance and the peeling strength of the polypropylene composite material; in comparative examples 5 and 6, the specific auxiliary agent was prepared by using high-density polyethylene outside the scope of the present invention, and the peel strength of the prepared polypropylene composite material was not improved.
The comparative example 1 is free from adding special auxiliary agents, and the peel strength and impact strength of the prepared polypropylene composite material are obviously lower than those of the examples of the invention; in the comparative example 2, maleic anhydride and high-density polyethylene are selected for blending, and the scratch resistance, the peeling strength and the impact strength of the prepared polypropylene composite material are obviously reduced compared with those of the examples; comparative example 3, to which only high-density polyethylene was added, had significantly lower peel strength and impact strength although the scratch resistance was improved; the comparative example 4 was added with only maleic anhydride, and the peel strength of the polypropylene composite material obtained was increased, but resulted in a significant decrease in scratch resistance and impact strength of the material.
In comparative example 9, the polypropylene copolymer with lower crystallinity is selected, and the scratch resistance of the obtained composite material is obviously poor; comparative example 10 uses a homo-polypropylene with high crystallinity that does not contain ethylene segments, resulting in a composite with poor impact strength.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (9)
1. The scratch-resistant polypropylene composite material with high impact resistance and high peeling property is characterized by comprising the following components in parts by weight:
wherein the copolymerized polypropylene is an ethylene-propylene copolymer with the crystallinity of 75-80%; the special auxiliary agent is high-density polyethylene grafted maleic anhydride, and in the high-density polyethylene grafted maleic anhydride, the grafting rate of the maleic anhydride is 0.2-2.0wt%; in the high-density polyethylene grafted maleic anhydride, the density of the high-density polyethylene is 0.950～0.960g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The scratch resistant agent is an amide scratch resistant agent.
2. The high impact, high peel performance scratch resistant polypropylene composite material according to claim 1, wherein the grafting of maleic anhydride is 0.8 to 1.5wt%.
3. The scratch resistant polypropylene composite material with high impact and high peel performance according to claim 1, wherein the high density polyethylene has a density of 0.954-0.956 g/cm 3 。
4. The high impact, high peel performance scratch resistant polypropylene composite material according to claim 1 wherein said toughening agent is an ethylene- α -olefin random copolymer.
5. The high impact, high peel performance scratch resistant polypropylene composite material of claim 1, wherein the filler is one or a combination of several of talc, calcium carbonate or basic magnesium sulfate whiskers.
6. The high impact, high peel performance scratch resistant polypropylene composite material of claim 1 wherein said filler is basic magnesium sulfate whisker.
7. The high impact, high peel performance scratch resistant polypropylene composite material according to claim 1 wherein said lubricant is a stearate.
8. The method for preparing the scratch-resistant polypropylene composite material with high impact resistance and high peeling property according to any one of claims 1 to 7, comprising the following steps:
the polypropylene, the filler, the special auxiliary agent, the toughening agent, the scratch resistant agent, the lubricant and the antioxidant are uniformly mixed according to a proportion, and then the mixture is prepared by melt extrusion, wherein the temperature of the melt extrusion is 170-210 ℃.
9. Use of the scratch-resistant polypropylene composite material with high impact resistance and high peeling property as defined in any one of claims 1 to 7 for preparing automobile parts.
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| CN202210101744.7A CN114479289B (en) | 2022-01-27 | 2022-01-27 | Scratch-resistant polypropylene composite material with high impact resistance and high stripping performance, and preparation method and application thereof |
| PCT/CN2023/071648 WO2023143067A1 (en) | 2022-01-27 | 2023-01-10 | Scratch-resistant polypropylene composite material with high impact resistance and high peeling performance, method for preparing same, and use thereof |
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| CN115851043B (en) * | 2022-12-15 | 2023-12-15 | 金发科技股份有限公司 | Spray polypropylene and preparation method and application thereof |
| CN115895348A (en) * | 2022-12-26 | 2023-04-04 | 广州鹿山新材料股份有限公司 | Polypropylene powder coating and preparation method and application thereof |
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