CN114716750A - Polyolefin master batch and preparation method and application thereof - Google Patents
Polyolefin master batch and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a polyolefin master batch and a preparation method and application thereof, belonging to the technical field of high polymer materials. The polyolefin master batch comprises the following components in parts by weight: 35-78 parts of non-polar polyolefin resin; 10-30 parts of expanded graphite; 1-3 parts of a coupling agent; 10-30 parts of a compatilizer; 2-10 parts of an antioxidant; 0.1-2 parts of a lubricant. The crystallinity of the nonpolar polyolefin resin is 60-90%, the testing method is a DSC method, and the testing condition is that the temperature rising and reducing rate is 10 ℃/min. The polyolefin master batch effectively improves the long-term aging resistance effect of the ABS composite material through the synergistic effect of the nonpolar polyolefin resin and the expanded graphite. The invention discloses a long-term thermal aging resistant ABS composite material, the retention rate of the test tensile strength after aging at 100 ℃/1000h is still more than 92%.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polyolefin master batch, a preparation method and application thereof, and a long-term thermal aging resistant ABS composite material, a preparation method and application thereof.
Background
ABS is a terpolymer of three monomers of acrylonitrile (a), butadiene (B) and styrene (S), and is widely used in interior and exterior automotive trim because of its excellent comprehensive physical and mechanical properties, dimensional stability, electrical properties, wear resistance, chemical resistance, dyeability, finished product processing and machining properties.
In recent years, the automobile industry has more and more high attention to long-term thermal aging, and the aging of the automobile interior is mainly caused by overhigh temperature in summer, which can cause the thermal aging of the automobile interior. ABS has carbon-carbon double bonds carried by butadiene in molecular chains, is easy to be oxidized and degraded under the action of thermal oxygen, and is one of important defects for limiting the use of ABS.
For solving the problem of poor long-term heat aging resistance of the ABS resin, the prior art discloses an anti-aging ABS material, wherein 0.1-0.3 part of antioxidant 1010, 0.2-0.6 part of antioxidant 2216, 0.2-0.6 part of antioxidants such as ultraviolet absorbers and the like are added to improve the aging resistance of the ABS resin, however, the tensile property retention rate of the ABS resin after an aging test at 90 ℃ for 500 hours is only 93.44% at most, and the antioxidant is small relative to the molecular weight of the ABS resin due to the large using amount of the antioxidant, so that the antioxidant is easily separated from the ABS resin to the surface of the ABS resin, and the appearance of the ABS material is poor.
Disclosure of Invention
The invention aims to solve the technical problems of poor long-term thermal aging resistance and poor appearance of the conventional ABS resin, and provides the polyolefin master batch, which effectively improves the long-term aging resistance of the ABS composite material and has better appearance through the synergistic effect of the nonpolar polyolefin resin and the expanded graphite.
The invention also aims to provide a preparation method of the polyolefin master batch.
The invention also aims to provide application of the polyolefin master batch in improving the long-term heat aging resistance of the ABS composite material.
The invention also aims to provide the ABS composite material with long-term heat aging resistance.
The invention further aims to provide a preparation method of the ABS composite material with long-term heat aging resistance.
The invention also aims to provide application of the long-term heat aging resistant ABS composite material in preparing automobile interior and/or automobile exterior.
The above purpose of the invention is realized by the following technical scheme:
the polyolefin master batch comprises the following components in parts by weight:
the crystallinity of the nonpolar polyolefin resin is 60-90%, and the test method is a DSC method.
The specific test method of DSC method comprises heating 5mg polyolefin sample to 200 deg.C at a heating rate of 10 deg.C/min under nitrogen protection, holding the temperature for 5min, cooling to 30 deg.C at a cooling rate of 10 deg.C/min, holding the temperature for 5min, heating to 200 deg.C at a heating rate of 10 deg.C/min, and performing secondary heatingObtaining the heat content delta H of fusion in the process of secondary temperature risefDegree of crystallinity ═ Δ Hf÷ΔH0X 100%. Wherein Δ H0The enthalpy of fusion of the polymer at 100% crystallinity.
Wherein, it is required to be noted that:
the polyolefin master batch effectively improves the long-term aging resistance effect of the ABS composite material through the synergistic effect of the nonpolar polyolefin resin and the expanded graphite.
The long-term aging resistance effect of the invention refers to that the test condition is 100 ℃/1000h, the percentage of the test tensile strength after aging to the tensile strength at normal temperature is higher, the long-term aging resistance performance is good, namely the long-term aging resistance effect is good.
The action mechanism of each component of the polyolefin master batch is as follows:
the nonpolar polyolefin resin is a polymer with low surface energy, and has a driving force of migrating to the surface in the polar ABS resin matrix, so that oxygen barrier can be formed in the ABS matrix and even on the surface; the crystallization degree of the nonpolar polyolefin resin is higher, the resin is denser, and the crystallization layer of the nonpolar polyolefin resin can effectively prolong the diffusion time of oxygen molecules in the polymer, so that the long-term heat aging resistance can be improved.
The expanded graphite is of a lamellar net structure, and the airtight lamellar filler can effectively prolong the circuitous path of diffusion and permeation of oxygen molecules in the polymer, so that the gas barrier property of the composite material is improved.
According to the invention, through the synergistic effect of the high-crystalline nonpolar polyolefin resin and the expanded graphite, oxygen barrier is formed in the ABS matrix and even on the surface of the ABS matrix, and the contact of oxygen and double bonds of the ABS resin is prevented or delayed, so that the aging speed of the ABS is reduced, and the long-term aging resistance of the ABS resin can be improved.
The non-polar polyolefin resin has a low crystallinity, and it is difficult to form a dense crystalline layer, and therefore, it is difficult to significantly improve the aging resistance of the ABS resin.
When the crystallinity of the nonpolar polyolefin resin is more than a certain degree, the aging resistance of the composite material cannot be further improved even if the crystallinity is increased after a denser crystalline layer is formed.
The addition amount of the expanded graphite is too small, the barrier property to oxygen is poor, and the good thermal aging resistant effect cannot be achieved.
The addition of the expanded graphite is too much, agglomeration is easily caused due to poor dispersion, the oxygen barrier is reduced, and the heat-resistant aging effect is reduced.
The coupling agent is used for enhancing the compatibility of the expanded graphite and the matrix.
The coupling agent may be selected from silane coupling agents.
The compatilizer can improve the compatibility of the polyolefin master batch and the ABS matrix.
In order to further improve the long-term thermal aging resistance of the ABS composite material, the crystallinity of the nonpolar polyolefin resin is preferably 70-80%.
In order to further improve the long-term thermal aging resistance of the ABS composite material, preferably, the expansion ratio of the expanded graphite is 100-300 times, the test method is a volume method, the volume change of the graphite before and after expansion is tested, and the ratio is the expansion ratio.
Preferably, the non-polar polyolefin resin is one or more of polyethylene, polypropylene and polybutylene.
Preferably, the compatibilizer is polypropylene grafted maleic anhydride.
The invention also provides a preparation method of the polyolefin master batch, which comprises the following steps:
uniformly mixing the components, and carrying out melt blending, extrusion and granulation at 130-230 ℃ by using a double-screw extruder to obtain the polyolefin master batch.
The invention also protects the application of the polyolefin master batch in improving the long-term thermal aging resistance of the ABS composite material.
The polyolefin master batch can effectively improve the long-term aging resistance effect of the ABS composite material, so that the polyolefin master batch can be used for improving the long-term thermal aging resistance of the ABS composite material.
The invention also discloses a long-term thermal aging resistant ABS composite material, which comprises the following components in parts by weight:
the master batch is the polyolefin master batch.
The long-term heat aging resistant ABS composite material prepared by the invention can effectively improve the long-term aging resistance of the ABS composite material by adding a proper amount of polyolefin master batches, and has better tensile strength. Because the dosage of the antioxidant in the master batch is less, the long-term thermal aging requirement is met, and meanwhile, less antioxidant is difficult to separate out of the surface of the composite material under the barrier effect of the expanded graphite, so that the good appearance of the composite material is maintained.
The invention also provides a preparation method of the long-term thermal aging resistant ABS composite material, which comprises the following steps: the components are uniformly mixed, and the ABS composite material with long-term thermal aging resistance is obtained after melt extrusion, granulation and drying at the temperature of 200-240 ℃ by a double-screw extruder.
The invention also protects the application of the long-term heat aging resistant ABS composite material in the preparation of automotive interior and/or automotive exterior.
The long-term heat aging resistant ABS composite material prepared by the invention has better long-term aging resistance, can be widely applied to the preparation of plastic products, and particularly protects the application of the heat aging resistant ABS composite material in the preparation of automotive interiors and/or automotive exteriors.
The invention also protects the application of the long-term thermal aging resistant ABS composite material in parts such as automobile interior door panels, decorative parts of instrument panels, automobile exterior decorative grids, doorsills, reflector shells and the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a polyolefin master batch, which comprises nonpolar polyolefin resin, expanded graphite, a coupling agent, a compatilizer, an antioxidant and a lubricant, and effectively improves the long-term aging resistance effect of an ABS composite material through the synergistic effect of the nonpolar polyolefin resin and the expanded graphite.
The invention discloses a long-term heat aging resistant ABS composite material, which has excellent long-term heat aging resistance, the retention rate of the test tensile strength after aging at 100 ℃/1000h is still more than 92%, the dosage of an antioxidant in master batches is less, and less antioxidant is difficult to separate out on the surface of the composite material under the barrier effect of expanded graphite, so that the good appearance of the composite material is maintained.
Drawings
FIG. 1 is an appearance diagram of an ABS composite material without small molecule precipitation on the surface.
FIG. 2 is an appearance diagram of an ABS composite material with small molecule precipitation on the surface
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
The invention adopts the following raw materials:
the nonpolar polyolefin resin 1 is polypropylene resin with the mark of H9018 and the crystallinity of 70 percent, and the manufacturer is Lanzhou petrochemical;
the nonpolar polyolefin resin 2 is polypropylene resin with the trademark of SZ30S and the crystallinity of 60 percent, and is made by China Korean petrochemical industry;
the nonpolar polyolefin resin 3 is polypropylene resin with the brand number of H9012D and the crystallinity of 80 percent, and is made into Zhanjiang petrochemical;
the nonpolar polyolefin resin 4 is polyethylene resin, the trademark is HPDE 8008, the crystallinity is 90%, the manufacturer is Ningxia Baofeng;
the non-polar polyolefin resin 5 is polypropylene resin with the trademark SP179, the crystallinity is 40 percent, and the manufacturer is Lanzhou petrochemical;
the expanded graphite 1 is expanded graphite with expansion ratio of 250 times, and is prepared by mixing natural 300-mesh graphitePlacing graphite in concentrated H with volume ratio of 3:12SO4And concentrated HNO3Stirring, washing and drying the solution at normal temperature, and then placing the solution at 900 ℃ (nitrogen environment) for 15 s;
the expanded graphite 2 is expanded graphite with expansion ratio of 100 times, and is prepared by placing 300 mesh natural graphite in concentrated H with volume ratio of 3:12SO4And concentrated HNO3Stirring, washing, drying at normal temperature, and standing at 900 deg.C (nitrogen environment) for 8 s;
the expanded graphite 3 is expanded graphite with expansion ratio of 50 times, and is prepared by placing 300 mesh natural graphite in concentrated H with volume ratio of 3:12SO4And concentrated HNO3Stirring, washing and drying the solution at normal temperature, and then placing the solution at 700 ℃ (nitrogen environment) for 10 s;
the expanded graphite 4 is expanded graphite with expansion ratio of 400 times, and is prepared by placing 300 mesh natural graphite in concentrated H with volume ratio of 3:12SO4And concentrated HNO3Stirring, washing and drying the solution at normal temperature, and then placing the solution at 1050 ℃ (nitrogen environment) for 15 s;
the coupling agent is a silane coupling agent, which is commercially available and is the same for all examples and comparative examples; (ii) a
The compatibilizer was polypropylene grafted maleic anhydride, the same one commercially available and used in all examples and comparative examples;
the antioxidant is a hindered phenol antioxidant and a phosphite antioxidant, the weight ratio of the hindered phenol antioxidant to the phosphite antioxidant is 1:1, and the antioxidant is commercially available and is the same as that used in all the examples and comparative examples.
ABS resin, designation ABS 8434, manufacturer: high bridge petrochemical;
the weather resistant agent is a hindered amine type weather resistant agent, which is commercially available and the same as that used in all examples and comparative examples.
The lubricant is a fatty acid, commercially available and the same for all examples and comparative examples.
Examples 1 to 3
The polyolefin master batch comprises the following components in parts by weight:
a non-polar polyolefin resin; expanded graphite; a coupling agent; a compatibilizing agent; an antioxidant; lubricant agent
Wherein the specific contents of each component are shown in the following table 1.
TABLE 1 polyolefin masterbatch composition (in parts by weight)
| 1 | 2 | 3 | |
| Nonpolar polyolefin resin 1 | 57.6 | 35 | 78 |
| Expanded graphite 1 | 20 | 30 | 10 |
| Coupling agent | 2 | 3 | 1 |
| Compatilizer | 20 | 30 | 10 |
| Is resistant to oxidationAgent for treating cancer | 4 | 10 | 2 |
| Lubricant agent | 0.2 | 0.2 | 0.2 |
TABLE 1
| 4 | 5 | 6 | 7 | 8 | 9 | |
| Nonpolar polyolefin resin 1 | 57.6 | 57.6 | 57.6 | |||
| Nonpolar polyolefin resin 2 | 57.6 | |||||
| Nonpolar polyolefin resin 3 | 57.6 | |||||
| Nonpolar polyolefin resin 4 | 57.6 | |||||
| Expanded graphite 1 | 20 | 20 | 20 | |||
| Expanded graphite 2 | 20 | |||||
| Expanded graphite 3 | 20 | |||||
| Expanded graphite 4 | 20 | |||||
| Coupling agent | 2 | 2 | 2 | 2 | 2 | 2 |
| Compatilizer | 20 | 20 | 20 | 20 | 20 | 20 |
| Antioxidant agent | 4 | 4 | 4 | 4 | 4 | 4 |
| Lubricant agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
The preparation method of the polyolefin master batch comprises the following steps:
uniformly mixing the nonpolar polyolefin resin, the coupling agent and the compatilizer, feeding the mixture mainly through a double-screw extruder, feeding the expanded graphite laterally through the double-screw extruder, and carrying out melt blending, extrusion and granulation at 130-230 ℃ to obtain the expanded graphite.
Example 10
The long-term thermal aging resistant ABS composite material comprises the following components in parts by weight:
90 parts of ABS resin; 10 parts of master batch; 0.4 part of weather resisting agent; 0.2 part of a lubricant;
the master batch is the polyolefin master batch in the embodiment 1;
the preparation method of the long-term thermal aging resistant ABS composite material comprises the following steps:
the components are uniformly mixed, and the ABS composite material with long-term thermal aging resistance is obtained after melt extrusion, granulation and drying at the temperature of 200-240 ℃ by a double-screw extruder.
Examples 11 to 18
The long-term thermal aging resistant ABS composite material is different from the ABS composite material in the embodiment 8 in that the master batch is the polyolefin master batch in the embodiment 2-9;
the rest is the same as the embodiment 10, and the description is omitted.
Example 19
The long-term thermal aging resistant ABS composite material comprises the following components in parts by weight:
85 parts of ABS resin; 15 parts of master batch; 0.2 part of weather resistant agent; 0.2 part of a lubricant;
the rest is the same as the embodiment 10, and the description is omitted.
Example 20
The long-term thermal aging resistant ABS composite material comprises the following components in parts by weight:
95 parts of ABS resin; 5 parts of master batch; 1 part of weather resistant agent; 0.2 part of a lubricant;
the rest is the same as the embodiment 10, and the description is omitted.
Comparative examples 1 to 5
The polyolefin master batch comprises the following components in parts by weight:
a non-polar polyolefin resin; expanded graphite; a coupling agent; a compatibilizing agent; an antioxidant; lubricant agent
Wherein the specific contents of each component are shown in the following table 1.
TABLE 2 polyolefin masterbatch composition in respective proportions (by weight)
The preparation method is the same as that of example 1, and is not described in detail herein.
Comparative examples 6 to 10
An ABS composite material comprises the following components in parts by weight:
90 parts of ABS resin; 10 parts of master batch; 0.4 part of weather resisting agent; 0.2 part of a lubricant;
the master batch is the polyolefin master batch in comparative examples 1-5;
the rest is the same as the embodiment 10, and the description is omitted.
Comparative example 11
An ABS composite material comprises the following components in parts by weight:
99 parts of ABS resin; 1 part of master batch; 0.4 part of weather resistant agent; 0.2 part of a lubricant;
the master batch is the polyolefin master batch in the embodiment 1;
the rest is the same as the embodiment 10, and the description is omitted.
Comparative example 12
An ABS composite material comprises the following components in parts by weight:
80 parts of ABS resin; 20 parts of master batch; 0.4 part of weather resistant agent; 0.2 part of a lubricant;
the master batch is the polyolefin master batch in the embodiment 1;
the rest is the same as the embodiment 10, and the description is omitted.
Comparative example 13
An ABS composite material comprises the following components in parts by weight:
80 parts of ABS resin; 2 parts of an antioxidant;
the rest is the same as the embodiment 10, and the description is omitted.
Result detection
The ABS composites of the above examples and comparative examples were tested by the following performance test methods:
(1) normal temperature tensile strength: the tensile speed in the test conditions was 50mm/min, and the test method was ISO 527/2-2012.
(2) Tensile strength retention after heat aging: the testing condition of the thermal aging is 100 ℃/1000h, the tensile strength is tested after the aging, the tensile speed in the testing condition is 50mm/min, the testing method is ISO527/2-2012, and the tensile strength change before and after the aging is compared.
(3) Appearance test after heat aging: and (3) injection molding the composite material into a square plate with the thickness of 2mm, carrying out a heat aging test under the test condition of 100 ℃/1000h, and visually checking whether precipitates exist on the surface of the aged sample plate.
The specific test results of examples 10 to 20 are shown in Table 3 below:
TABLE 3
The specific test results of comparative examples 6 to 13 are shown in Table 4 below:
TABLE 4
The data show that the long-term thermal aging resistant ABS composite material has excellent long-term thermal aging resistance, the retention rate of the tested tensile strength after aging at 100 ℃/1000h is still more than 91%, the dosage of the antioxidant in the master batch is less, and less antioxidant is difficult to precipitate on the surface of the composite material under the barrier effect of the expanded graphite, so that the good appearance of the composite material is maintained.
As can be seen from example 10 and comparative example 11, the addition amount of the master batch was too small, and the tensile strength retention after heat aging was only 67%, indicating that the ABS composite material had very poor long-term heat aging resistance.
As can be seen from example 10 and comparative example 12, the addition amount of the master batch was too large, and the tensile strength retention after heat aging was as high as 95%, but the decrease in the overall tensile strength was significant due to the poor compatibility of the polyolefin master batch with the ABS matrix.
As can be seen from example 10 and comparative example 13, the antioxidant used in a large amount easily precipitates on the surface of the composite material, resulting in deterioration of the appearance of the composite material.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The polyolefin master batch is characterized by comprising the following components in parts by weight:
the crystallinity of the nonpolar polyolefin resin is 60-90%, and the test method is a DSC method.
2. The polyolefin masterbatch of claim 1, wherein the nonpolar polyolefin resin has a crystallinity of 70 to 80%.
3. The polyolefin masterbatch according to claim 1, wherein the expanded graphite has an expansion ratio of 100 to 300 times.
4. The polyolefin masterbatch of claim 1, wherein the non-polar polyolefin resin is one or more of polyethylene, polypropylene, and polybutylene.
5. The polyolefin masterbatch of claim 1, wherein said compatibilizer is polypropylene grafted maleic anhydride.
6. The method for preparing the polyolefin masterbatch of any one of claims 1 to 5, comprising the following steps:
uniformly mixing the components, and carrying out melt blending, extrusion and granulation at 130-230 ℃ by using a double-screw extruder to obtain the polyolefin master batch.
7. The use of the polyolefin masterbatch of any one of claims 1 to 5 for improving the long-term thermal aging resistance of ABS composite materials.
8. The long-term thermal aging resistant ABS composite material is characterized by comprising the following components in parts by weight:
the masterbatch is the polyolefin masterbatch of any one of claims 1 to 5.
9. A method for preparing the long-term heat aging resistant ABS composite material according to claim 8, characterized by comprising the following steps: the components are uniformly mixed, and the ABS composite material with long-term thermal aging resistance is obtained after melt extrusion, granulation and drying at the temperature of 200-240 ℃ by a double-screw extruder.
10. Use of the long-term heat aging resistant ABS composite according to claim 8 for the production of automotive interiors and/or exteriors.
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| CN202210290648.1A Active CN114716750B (en) | 2022-03-23 | 2022-03-23 | Polyolefin master batch and preparation method and application thereof |
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