CN114716750B - 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, and belongs to the technical field of high polymer materials. The polyolefin master batch comprises the following components in parts by weight: 35-78 parts of nonpolar polyolefin resin; 10-30 parts of expanded graphite; 1-3 parts of a coupling agent; 10-30 parts of compatilizer; 2-10 parts of an antioxidant; 0.1-2 parts of lubricant. The crystallinity of the nonpolar polyolefin resin is 60-90%, the testing method is DSC method, and the testing condition is that the temperature rising and dropping speed is 10 ℃/min. According to the polyolefin master batch disclosed by the invention, the long-term aging resistance effect of the ABS composite material is effectively improved 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, wherein the retention rate of tensile strength is still more than 92% after aging at 100 ℃/1000 h.
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 heat aging resistant ABS composite material, and a preparation method and application thereof.
Background
ABS is a terpolymer of three monomers, namely acrylonitrile (A), butadiene (B) and styrene (S), and is widely applied to automobile interior and exterior trim due to the excellent comprehensive physical and mechanical properties, dimensional stability, electrical properties, wear resistance, chemical resistance, dyeing property, finished product processing, machining and other properties.
In recent years, the attention of the automobile industry to long-term heat aging is increasing, and the aging of the automobile interior trim is mainly caused by the fact that the temperature in the automobile is too high in summer, so that the heat aging of the automobile interior trim is caused. ABS is one of the important defects that the ABS is easily oxidized and degraded under the action of hot oxygen due to the existence of carbon-carbon double bonds carried by butadiene in a molecular chain.
For solving the problem of poor long-term heat aging resistance of ABS resin, the prior art discloses an anti-aging ABS material, which improves the aging resistance of the ABS resin by adding 0.1-0.3 part of antioxidant 1010,0.2-0.6 part of antioxidant 2216,0.2-0.6 part of antioxidant and other antioxidants, however, the tensile property retention rate after an aging test at 90 ℃ for 500 hours is only 93.44 percent at the highest, and the antioxidant is easy to separate out from the ABS resin to the surface of the material due to the larger dosage of the antioxidant compared with the ABS resin with smaller molecular weight, so that the appearance of the ABS material is poor.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings of poor long-term heat aging resistance and poor appearance of the existing ABS resin, provide the polyolefin master batch, effectively improve the long-term aging resistance of the ABS composite material through the synergistic effect of the nonpolar polyolefin resin and the expanded graphite, and have better appearance.
The invention also aims at providing a preparation method of the polyolefin master batch.
The invention also aims to provide an application of the polyolefin master batch in improving the long-term heat aging resistance of the ABS composite material.
It is another object of the present invention to provide an ABS composite that is resistant to long term thermal aging.
It is still another object of the present invention to provide a method for preparing an ABS composite that is resistant to long term thermal aging.
Another object of the invention is to provide an application of the ABS composite material resistant to long-term thermal aging in preparing an automotive interior and/or an automotive exterior.
The above object of the present invention is achieved 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 testing method is DSC method.
The DSC method comprises heating 5mg polyolefin sample to 200deg.C at 10deg.C/min under nitrogen protection, maintaining the temperature for 5min, cooling to 30deg.C at 10deg.C/min, maintaining the temperature for 5min, and heating to 200deg.C at 10deg.C/min to obtain molten enthalpy ΔH f Crystallinity=Δh f ÷ΔH 0 X 100%. Wherein DeltaH 0 The enthalpy of fusion of the polymer at 100% crystallinity.
The following are to be described:
according to the polyolefin master batch disclosed by the invention, the long-term aging resistance effect of the ABS composite material is effectively improved through the synergistic effect of the nonpolar polyolefin resin and the expanded graphite.
The long-term aging resistance effect of the invention is that the test condition is 100 ℃/1000h, the percentage of the tensile strength to the tensile strength at normal temperature after aging is higher, and 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 specifically as follows:
the nonpolar polyolefin resin is a polymer with low surface energy, and has a driving force for migration to the surface in the polar ABS resin matrix, so that oxygen barrier can be formed inside the ABS matrix and even on the surface; and the crystallinity of the nonpolar polyolefin resin is higher, the resin is denser, and the crystalline 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 network structure, and the impermeable lamellar filler can effectively prolong the detour 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-crystallization nonpolar polyolefin resin and the expanded graphite, oxygen barrier is formed in the ABS matrix and even on the surface of the ABS matrix, so that the contact between oxygen and double bonds of the ABS resin is prevented or delayed, and the aging speed of the ABS is reduced, and therefore, the long-term aging resistance of the ABS resin can be improved.
The nonpolar polyolefin resin has a small crystallinity, and it is difficult to form a dense crystalline layer, and thus it is difficult to remarkably improve the aging resistance of the ABS resin.
When the crystallinity of the nonpolar polyolefin resin is higher than a certain level, after a relatively dense crystalline layer has been formed, the aging resistance of the composite material is not further improved even if the crystallinity is increased again.
The addition amount of the expanded graphite is too small, the barrier property to oxygen is poor, and a good heat aging resistance effect is not achieved.
The excessive addition of the expanded graphite is easy to cause agglomeration due to poor dispersion, but can reduce the barrier to oxygen and reduce the heat aging resistance effect.
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 heat aging resistance effect of the ABS composite, it is preferable that the crystallinity of the nonpolar polyolefin resin is 70 to 80%.
In order to further improve the long-term heat aging resistance effect of the ABS composite material, preferably, the expansion rate of the expanded graphite is 100-300 times, the testing method is a volume method, the volume change of the graphite before and after expansion is tested, and the ratio is the expansion rate.
Preferably, the nonpolar 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:
and uniformly mixing the components, and carrying out melt blending, extrusion and granulation at 130-230 ℃ by 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 heat 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 heat aging resistance of the ABS composite material.
The invention also protects a long-term heat aging resistant ABS composite material, which comprises the following components in parts by weight:
the master batch is any one of the polyolefin master batch.
The long-term heat aging resistant ABS composite material prepared by the invention can effectively improve the long-term aging resistant performance of the ABS composite material and has better tensile strength by adding a proper amount of polyolefin master batches. Because the dosage of the antioxidant in the master batch is less, the surface of the composite material is not easy to separate out due to the barrier effect of the expanded graphite when the requirement of long-term heat aging is met, and the good appearance of the composite material is maintained.
The invention also provides a preparation method of the ABS composite material resistant to long-term heat aging, which comprises the following steps: and uniformly mixing the components, performing melt extrusion and granulation at 200-240 ℃ by a double-screw extruder, and drying to obtain the ABS composite material resistant to long-term heat aging.
The invention also protects the application of the ABS composite material resistant to long-term heat aging in preparing automobile interiors and/or automobile exteriors.
The long-term heat aging resistant ABS composite material prepared by the method has good long-term aging resistant performance, can be widely applied to preparation of plastic products, and particularly protects application of the long-term heat aging resistant ABS composite material in preparation of automobile interiors and/or automobile exteriors.
The invention also protects the application of the long-term heat aging resistant ABS composite material in parts such as automobile interior door panels, decorative parts of instrument panels, automobile exterior grids, threshold, 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, wherein the long-term aging resistance effect of an ABS composite material is effectively improved 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 resistant performance, the retention rate of tensile strength is still more than 92% after aging at 100 ℃/1000h, the dosage of antioxidant in master batch is less, and meanwhile, less antioxidant is not easy to separate out to the surface of the composite material under the barrier action of expanded graphite, so that the good appearance of the composite material is maintained.
Drawings
FIG. 1 is an external view of an ABS composite material without small molecules precipitated on the surface.
FIG. 2 is an external view of an ABS composite material with small molecular precipitation on the surface
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
The invention adopts the following raw materials:
the nonpolar polyolefin resin 1 is polypropylene resin with the brand of H9018, the crystallinity of 70 percent and the manufacturer of Lanzhou petrochemical industry;
the nonpolar polyolefin resin 2 is polypropylene resin with the brand of SZ30S, the crystallinity of 60 percent and the manufacturer of China Korean petrochemical industry;
the nonpolar polyolefin resin 3 is polypropylene resin with the brand of H9012D, the crystallinity of 80 percent and the manufacturer of the nonpolar polyolefin resin is Zhanjiang petrochemical;
the nonpolar polyolefin resin 4 is polyethylene resin with the brand of HPDE8008, the crystallinity of 90 percent, and the manufacturer is Ningxia Baofeng;
the nonpolar polyolefin resin 5 is polypropylene resin with the trade name of SP179, the crystallinity of 40 percent and the manufacturer of Lanzhou petrochemical industry;
the expanded graphite 1 is expanded graphite with expansion ratio of 250 times, and is prepared by placing 300 mesh natural graphite in concentrated H with volume ratio of 3:1 2 SO 4 And concentrated HNO 3 Stirring at normal temperature, washing, drying, and standing at 900 deg.C (nitrogen atmosphere) for 15s;
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 3:1 2 SO 4 And concentrated HNO 3 In solutionStirring at normal temperature, washing, drying, and placing in 900 ℃ (nitrogen environment) for 8s;
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 3:1 2 SO 4 And concentrated HNO 3 Stirring at normal temperature, washing, drying, and standing at 700 deg.C (nitrogen atmosphere) for 10s;
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 3:1 2 SO 4 And concentrated HNO 3 Stirring at normal temperature, washing, drying, and placing in 1050 ℃ (nitrogen environment) for 15s;
the coupling agent is a silane coupling agent, which is commercially available and is the same for all examples and comparative examples; the method comprises the steps of carrying out a first treatment on the surface of the
The compatibilizer is polypropylene grafted maleic anhydride, commercially available and the same for all examples and comparative examples;
the antioxidants are hindered phenol antioxidants and phosphite antioxidants, the weight ratio of the hindered phenol antioxidants to the phosphite antioxidants is 1:1, and the antioxidants are commercially available and the same is used in all examples and comparative examples.
ABS resin, brand ABS8434, manufacturer: high bridge petrochemical industry;
the weathering agent is a hindered amine weathering agent, commercially available and the same for 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 nonpolar polyolefin resin; expanded graphite; a coupling agent; a compatibilizer; an antioxidant; lubricant
Wherein the specific contents of the components are shown in Table 1 below.
Table 1 polyolefin masterbatch compositions (in parts by weight) of examples
| 1 | 2 | 3 | |
| Nonpolar polyolefin resin 1 | 57.6 | 35 | 78 |
| Expanded graphite 1 | 20 | 30 | 10 |
| Coupling agent | 2 | 3 | 1 |
| Compatibilizing agent | 20 | 30 | 10 |
| Antioxidant | 4 | 10 | 2 |
| Lubricant | 0.2 | 0.2 | 0.2 |
Table 1, below
| 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 |
| Compatibilizing agent | 20 | 20 | 20 | 20 | 20 | 20 |
| Antioxidant | 4 | 4 | 4 | 4 | 4 | 4 |
| Lubricant | 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 nonpolar polyolefin resin, a coupling agent and a compatilizer, feeding the mixture mainly through a double-screw extruder, feeding expanded graphite through the side of the double-screw extruder, and carrying out melt blending, extrusion and granulation at 130-230 ℃ to obtain the composite material.
Example 10
The ABS composite material resistant to long-term heat aging comprises the following components in parts by weight:
90 parts of ABS resin; 10 parts of master batch; 0.4 parts of weather-proof agent; 0.2 parts of lubricant;
the master batch is the polyolefin master batch in example 1;
the preparation method of the ABS composite material resistant to long-term heat aging comprises the following steps:
and uniformly mixing the components, performing melt extrusion and granulation at 200-240 ℃ by a double-screw extruder, and drying to obtain the ABS composite material resistant to long-term heat aging.
Examples 11 to 18
Unlike example 8, the master batch is the polyolefin master batch in examples 2 to 9;
the remainder is the same as embodiment 10 and will not be described again here.
Example 19
The ABS composite material resistant to long-term heat aging comprises the following components in parts by weight:
85 parts of ABS resin; 15 parts of master batch; 0.2 part of weather-proof agent; 0.2 parts of lubricant;
the remainder is the same as embodiment 10 and will not be described again here.
Example 20
The ABS composite material resistant to long-term heat aging comprises the following components in parts by weight:
95 parts of ABS resin; 5 parts of master batch; 1 part of weather-proof agent; 0.2 parts of lubricant;
the remainder is the same as embodiment 10 and will not be described again here.
Comparative examples 1 to 5
The polyolefin master batch comprises the following components in parts by weight:
a nonpolar polyolefin resin; expanded graphite; a coupling agent; a compatibilizer; an antioxidant; lubricant
Wherein the specific contents of the components are shown in Table 2 below.
Table 2 polyolefin masterbatch compositions (in parts by weight) of respective comparative examples
The preparation method is the same as that of example 1, and will not be described here again.
Comparative examples 6 to 10
The ABS composite material comprises the following components in parts by weight:
90 parts of ABS resin; 10 parts of master batch; 0.4 parts of weather-proof agent; 0.2 parts of lubricant;
the master batch is the polyolefin master batch in comparative examples 1 to 5;
the remainder is the same as embodiment 10 and will not be described again here.
Comparative example 11
The ABS composite material comprises the following components in parts by weight:
99 parts of ABS resin; 1 part of master batch; 0.4 parts of weather-proof agent; 0.2 parts of lubricant;
the master batch is the polyolefin master batch in example 1;
the remainder is the same as embodiment 10 and will not be described again here.
Comparative example 12
The ABS composite material comprises the following components in parts by weight:
80 parts of ABS resin; 20 parts of master batch; 0.4 parts of weather-proof agent; 0.2 parts of lubricant;
the master batch is the polyolefin master batch in example 1;
the remainder is the same as embodiment 10 and will not be described again here.
Comparative example 13
The ABS composite material comprises the following components in parts by weight:
80 parts of ABS resin; 2 parts of an antioxidant;
the remainder is the same as embodiment 10 and will not be described again here.
Result detection
The ABS composites of the above examples and comparative examples were tested by the following performance test methods:
(1) Tensile strength at room temperature: 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 test condition of heat aging is 100 ℃/1000h, the tensile strength is tested after aging, the tensile speed in the test condition is 50mm/min, the test method is ISO527/2-2012, and the change of the tensile strength before and after 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, performing a thermal aging test, wherein the thermal aging test condition is 100 ℃/1000h, and visually checking whether precipitates exist on the surface of the aged sample plate.
Specific test results for examples 10 to 20 are shown in Table 3 below:
TABLE 3 Table 3
Specific test results of comparative examples 6 to 13 are shown in Table 4 below:
TABLE 4 Table 4
From the data, the ABS composite material resistant to long-term heat aging has excellent long-term heat aging resistance, the retention rate of tensile strength after aging at 100 ℃/1000h is still more than 91%, the dosage of the antioxidant in the master batch is less, and meanwhile, less antioxidant is not easy to separate out to the surface of the composite material under the barrier action of 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 long-term heat aging resistance of the ABS composite material was very poor.
As can be seen from examples 10 and 12, the addition amount of the master batch was too large, and although the retention of tensile strength after heat aging was as high as 95%, the decrease in the overall tensile strength was remarkable due to poor compatibility of the polyolefin master batch with the ABS matrix.
As can be seen from examples 10 and comparative example 13, the amount of the antioxidant used was large, and the antioxidant was easily precipitated on the surface of the composite material, resulting in deterioration of the appearance of the composite material.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (5)
1. The ABS composite material resistant to long-term heat aging is characterized by comprising the following components in parts by weight:
the polyolefin master batch comprises the following components in parts by weight:
the crystallinity of the nonpolar polyolefin resin is 70-80%, and the testing method is DSC method;
the expansion multiplying power of the expanded graphite is 100-300 times;
the nonpolar polyolefin resin is one or more of polyethylene, polypropylene and polybutene.
2. The long term heat aging resistant ABS composite of claim 1 wherein the compatibilizer is polypropylene grafted maleic anhydride.
3. The long term heat aging resistant ABS composite of claim 1 wherein the process for preparing the polyolefin master batch comprises the steps of:
and uniformly mixing the components, and carrying out melt blending, extrusion and granulation at 130-230 ℃ by a double-screw extruder to obtain the polyolefin master batch.
4. A method for preparing the ABS composite material resistant to long-term thermal aging according to any one of claims 1 to 3, comprising the steps of: and uniformly mixing the components, performing melt extrusion and granulation at 200-240 ℃ by a double-screw extruder, and drying to obtain the ABS composite material resistant to long-term heat aging.
5. Use of the long-term heat aging resistant ABS composite according to claim 4 for the production of automotive interiors and/or automotive exteriors.
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| Publication number | Priority date | Publication date | Assignee | Title |
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