CN109401165B - Heat-resistant AES resin composition with tiger skin lines reduced or eliminated and preparation thereof - Google Patents
Heat-resistant AES resin composition with tiger skin lines reduced or eliminated and preparation thereof Download PDFInfo
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- CN109401165B CN109401165B CN201811116131.0A CN201811116131A CN109401165B CN 109401165 B CN109401165 B CN 109401165B CN 201811116131 A CN201811116131 A CN 201811116131A CN 109401165 B CN109401165 B CN 109401165B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/04—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to rubbers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/08—Copolymers of styrene
- C08L25/12—Copolymers of styrene with unsaturated nitriles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a heat-resistant AES resin composition with tiger skin lines reduced or eliminated and a preparation method thereof; the composition comprises the following components in parts by weight: 30-50 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer, 40-65 parts of acrylonitrile-styrene copolymer, 5-20 parts of heat-resistant agent and 0.1-5.0 parts of processing aid; the crosslinking degree of the ethylene propylene diene monomer of the acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer is 40-70 wt%. The method is simple and easy to implement, and the prepared thermoplastic AES resin composition can completely avoid the tiger skin line defect on the surface of an injection molding part, has excellent mechanical properties, and is particularly suitable for automobile exterior trimming part products with larger size and more complex structure; such as automobile grilles, pillar panels, tail trim panels, etc.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a heat-resistant AES resin composition with tiger skin lines reduced or eliminated and a preparation method thereof.
Background
Acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (AES) is a weather resistant engineering plastic, which has a structure similar to that of acrylonitrile-butadiene-styrene graft copolymer (ABS), retains the excellent mechanical and physical properties of ABS as an engineering plastic, and has superior low temperature resistance compared to ASA resin. Most of the materials are applied to outdoor occasions with certain weather resistance and high low temperature resistance requirements, such as automobile exterior trimming parts, co-extruded profiles, outdoor fences and the like.
However, when AES resin is used for molding large-sized products, such as automobile grilles, empennage decorative plates and the like, tiger skin line defects are easy to appear on the surfaces of the products, and the appearance of the products is seriously influenced. The Tiger stripe defect is caused by unstable flow of resin in the process of processing and molding, and is a product with the surface presenting alternate stripe-shaped defects, similar to Tiger patterns, so that the Tiger stripe is called as Tiger stripe or flow mark in academia. Particularly, for thin-wall long-flow injection molded parts, such as heat dissipation grids, upright post plates, empennage decorative plates and the like, the tiger skin line defect is more serious, and obviously, the appearance defect directly influences the attractiveness of the parts and is difficult to accept by consumers, so that the application of AES resin in the field of automobile exterior trim is greatly limited; in addition, automobile exterior parts such as heat dissipation grids and the like have higher requirements on heat-resistant temperature, so the invention designs the heat-resistant AES resin with the tiger skin lines reduced or eliminated, and the heat-resistant AES resin has important scientific significance and commercial value.
At present, the effective method for improving the tiger stripes of the resin mainly uses small molecular substances, and the method can better improve the tiger stripe defects, but can generally cause the reduction of the heat resistance and the mechanical strength of the resin; patent CN102964686B discloses a polypropylene composite material for eliminating tiger stripes and a preparation method thereof, wherein the polypropylene composite material is prepared from the following components: 39.2-80% of polypropylene, 5-15% of sansevieria trifasciata stripe auxiliary agent, 10-40% of filling mineral, 0.3-1% of antioxidant, 0.5-5% of lubricant and 1-10% of compatilizer; the polypropylene composite material prepared by the method has stronger tensile strength and notch strength, but does not give out the change of the heat resistance of the material; the tiger stripe eliminating assistant used in the patent is micromolecular polypropylene, and actually, the use of the micromolecular substance generally influences the heat resistance of the material. Patent CN 105419143A discloses a heat-resistant ASA resin composition for eliminating tiger stripes and a preparation method thereof, wherein the tiger stripes are well eliminated by using SAN resin with low molecular weight.
In addition, the effective method for improving the tiger stripes of the resin also has the effect of improving the dispersion effect or the compatibility effect among the components in the resin; patent CN101914243 discloses a polypropylene composition for injection molding of automobile parts with good appearance and a preparation method thereof, which is prepared from the following components: 50-78% of polypropylene resin, 2-20% of elastomer, 2-10% of ethylene-propylene block copolymer and the balance of auxiliary agent, wherein the ethylene-propylene block copolymer is added to improve the dispersion of the elastomer in the polypropylene base material and the interfacial strength between the elastomer and the polypropylene base material, thereby overcoming the appearance defect of tiger skin texture generated by a workpiece. Chinese patent CN101885878A discloses a polypropylene resin composition, which comprises polypropylene, a filler, a toughening agent, a heat stabilizer, a lubricant and an appearance improver, wherein the appearance improver is an acrylate-carboxyl-containing olefin-ethylene terpolymer or an epoxy aliphatic polymer, and because the appearance improver has good compatibility with the polypropylene, the toughening agent and other components, and the polar group has good compatibility with the filler, the lubricant and other components, the appearance defects such as tiger skin lines or flow marks are avoided.
However, there is no report on an AES resin composition in which tiger stripes are reduced or eliminated and a method for preparing the same.
Disclosure of Invention
The invention aims to provide a heat-resistant AES resin composition with tiger stripes reduced or eliminated and a preparation method thereof, aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention relates to a heat-resistant AES resin composition, which comprises the following components in parts by weight:
the crosslinking degree of the ethylene propylene diene monomer of the acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer is 40-70 wt%.
Preferably, the weight-average molecular weight of the acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer is 50,000-500,000, and the weight percentage content of the ethylene propylene diene monomer is 20-80 wt%.
Preferably, the acrylonitrile-styrene copolymer has a weight average molecular weight of 100,000-500,000 and an acrylonitrile content of 15-40 wt%.
Preferably, the heat-resistant agent is an N-phenylmaleimide-styrene-maleic anhydride copolymer. Other common heat-resistant agents are: copolymers of N-phenylmaleimide and alpha-methylstyrene-acrylonitrile copolymers; however, the copolymer molecular chain of the N-phenylmaleimide has high rigidity and polarity, poor compatibility with acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer and styrene-acrylonitrile copolymer, poor processing fluidity, easy generation of unstable flow and obvious tiger skin texture; alpha-methylstyrene-acrylonitrile copolymers have poor high-temperature thermal stability and low heat-resistant efficiency, and are not suitable for eliminating tiger stripes of heat-resistant AES.
Preferably, the processing aid comprises one or a mixture of several of a lubricant, an antioxidant and a mold release agent.
Preferably, the lubricant is pentaerythritol stearate or ethylene bis-stearamide, the antioxidant is a hindered phenol or phosphite antioxidant, and the release agent is a silicone release agent.
The invention also relates to a preparation method of the heat-resistant AES resin composition with the tiger skin lines reduced or eliminated, and the preparation method comprises the following steps:
s1, weighing the raw materials according to the proportion, and premixing in a high-speed mixer;
s2, feeding the premix obtained in the step S1 into a double-screw extruder through a metering device, melting and compounding materials under the conveying, shearing and mixing of screws, and then performing extrusion, strip drawing, cooling and grain cutting to obtain the heat-resistant AES resin composition.
Preferably, the length-diameter ratio of the screw of the double-screw extruder is 36-44, the extrusion temperature is 180-250 ℃, and the screw rotating speed is 200-500 r/min.
Compared with the prior art, the invention has the following beneficial effects:
1. the composition of the invention reduces or eliminates the tiger skin line defect by adopting the combined action of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymers with different crosslinking degrees and a heat-resistant agent with high heat-resistant efficiency, good processing fluidity and good compatibility with AES resin; and when the crosslinking degree of the acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer is 40-70%, the tiger skin line defect of the prepared AES resin composition can be well reduced or eliminated. On one hand, in the system, the crosslinking degree of the ethylene propylene diene monomer is too low, so that the rubber is easy to deform in the injection molding process of the AES resin, and the tiger skin stripes are easy to generate due to the unstable flow; on the other hand, in the system of the invention, the crosslinking degree of the ethylene propylene diene monomer is too high, and the ethylene propylene diene monomer in the AES resin is too hard, so that the mechanical property is deteriorated, and the practical use of a molded product is influenced.
2. The preparation method disclosed by the invention is simple in process and low in cost, the preparation process is easy to control, no side reaction is generated, and the method is very suitable for industrial production.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications can be made by those skilled in the art after reading the disclosure of the present invention, and equivalents fall within the scope of the appended claims.
The raw materials, parameters and grades used in the examples were as follows:
the weight-average molecular weight of the acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer is 50,000-500,000, the content of ethylene propylene diene monomer is 20-80 wt%, and the crosslinking degree of ethylene propylene diene monomer is 20-90 wt%. The acrylonitrile-styrene copolymer has a weight average molecular weight of 100,000-500,000 and a content of acrylonitrile in the range of 15-40 wt%. The heat-resistant agent is an N-phenylmaleimide-styrene-maleic anhydride copolymer. The processing aid comprises one or more of lubricant (pentaerythritol stearate or ethylene bis stearamide), antioxidant (hindered phenol or phosphite antioxidant) and silicone release agent, and the dosage can be any value of 0.5-3.0 parts by weight; for convenience of comparison, the processing aids in the following examples and comparative examples were lubricant EBS and antioxidant Ciba IG-1076 (1: 1 by mass ratio) in an amount of 0.6 parts by weight.
Example 1
30 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 40 percent), 65 parts of acrylonitrile-styrene copolymer, 5 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid. Weighing the raw materials according to the parts by weight, and preparing the heat-resistant AES resin composition with the tiger skin lines reduced or eliminated by adopting the following method:
(1) fully mixing the prepared raw materials in a high-speed mixer for 30 min;
(2) and (2) feeding the premix prepared in the step (1) into a double-screw extruder through a metering device, melting and compounding materials under the conveying, shearing and mixing of screws, and then carrying out extrusion, bracing, cooling and grain cutting to obtain the heat-resistant AES resin composition with the tiger skin lines reduced or eliminated. The length-diameter ratio of the screw of the double-screw extruder is 36-44, the extrusion temperature is 180-250 ℃, and the rotating speed of the screw is 200-500 r/min.
Example 2
40 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 50 percent), 50 parts of acrylonitrile-styrene copolymer, 10 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Example 3
50 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (60 percent of crosslinking degree of ethylene propylene diene monomer), 40 parts of acrylonitrile-styrene copolymer, 10 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Example 4
35 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 70 percent), 45 parts of acrylonitrile-styrene copolymer, 20 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Example 5
35 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 50 percent), 45 parts of acrylonitrile-styrene copolymer, 20 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Example 6
30 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 70 percent), 65 parts of acrylonitrile-styrene copolymer, 5 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Comparative example 1
30 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 90 percent), 65 parts of acrylonitrile-styrene copolymer, 5 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Comparative example 2
40 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 80 percent), 50 parts of acrylonitrile-styrene copolymer, 10 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Comparative example 3
50 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (30 percent of crosslinking degree of ethylene propylene diene monomer), 40 parts of acrylonitrile-styrene copolymer, 10 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Comparative example 4
35 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 20%), 45 parts of acrylonitrile-styrene copolymer, 20 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Comparative example 5
90 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 50 percent), 10 parts of heat-resistant agent (N-phenylmaleimide-styrene-maleic anhydride copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Comparative example 6
40 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 50 percent), 50 parts of acrylonitrile-styrene copolymer, 10 parts of heat-resistant agent (copolymer of N-phenylmaleimide) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Comparative example 7
40 parts of acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer (the crosslinking degree of the ethylene propylene diene monomer is 50 percent), 50 parts of acrylonitrile-styrene copolymer, 10 parts of heat-resistant agent (alpha-methylstyrene-acrylonitrile copolymer) and 0.6 part of processing aid.
The specific preparation method is the same as that of example 1.
Performance testing
Test specimens were prepared from the AES resin compositions prepared in examples 1 to 5 and comparative examples 1 to 4 under the same injection conditions, and the test items for the physical properties, the light aging resistance and the antifungal properties were as follows:
tensile strength: the test is carried out according to ISO527 standard, the test speed is 50mm/min,
flexural modulus: testing according to ISO178 standard, with testing speed of 1 mm/min;
notched izod impact strength at 23 ℃: testing according to ISO180 standard, wherein the thickness of the sample strip is 4 mm;
heat distortion temperature: testing according to ISO75 standard under 0.45 MPa;
melt flow rate: testing according to ISO1183 standard under 220 deg.C/10 kg
Tiger skin lines: visual evaluation showed a tendency to tiger stripes on black flakes having a size of 350mm (length) 100mm (width) 3.2mm (thickness) which were produced by injection molding with an extrusion compound using an injection machine at an injection speed of 30 mm/s. The tiger stripe on the surface of the black sheet was measured by naked eyes under a light source of a 40W fluorescent lamp. "eliminated" refers to a sheet that does not have any tiger stripes across the surface of the sheet under the test conditions. "significant" means that tiger stripes appear on the surface of the test sheet under the test conditions. By "very distinct" is meant that very distinct tiger stripes appear on the surface of the test sheet under the test conditions. "slight" means that slight tiger stripes appear but not noticeable on the surface of the test sheet under the test conditions.
TABLE 1 comparison of Performance between examples and comparative examples
As can be seen from the results in Table 2, the AES resin composition of the invention is excellent in reducing or eliminating the tiger stripes problem of AES resins. It can be seen from examples 1 to 5 and comparative examples 1 to 4 that the degree of crosslinking of the ethylene-propylene-diene rubber is 40 to 70%. The tiger skin lines of the AES resin are well reduced or eliminated; it can be seen from examples 2, 5 and 4 that when the crosslinking degree of the epdm rubber is 40%, the tiger skin pattern defect on the AES resin surface is slight even if the heat-resistant agent content is 20%, and the tiger skin pattern is mainly related to the decrease in the melt index after the heat-resistant agent content is increased; when the content of the heat-resistant agent is 20%, the tiger stripes of the AES resin with the crosslinking degree of 20% are more severe than those of the AES resin with the crosslinking degree of 40%, which shows that the crosslinking degree of the ethylene propylene diene monomer greatly affects the severity of the tiger stripes of the AES resin. By comparing example 2 with comparative example 5, it can be seen that, without adding acrylonitrile-styrene copolymer, the melt flow rate, tensile strength and flexural modulus of the resin are poor and the tiger stripe phenomenon is very severe, i.e., in such a resin system, no effect is exerted even with the degree of crosslinking defined by the present invention. By comparing example 2 and comparative examples 6 to 7, it can be seen that, as the heat-resistant agent, the copolymer of N-phenylmaleimide and the α -methylstyrene-acrylonitrile copolymer are both serious in tiger stripes of the AES resin, mainly because: the copolymer molecular chain of the N-phenylmaleimide has high rigidity and polarity, poor compatibility with acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer and styrene-acrylonitrile copolymer, poor processing fluidity, easy generation of unstable flow and obvious tiger skin texture; alpha-methylstyrene-acrylonitrile copolymers have poor high-temperature thermal stability and low heat-resistant efficiency, and are not suitable for eliminating tiger stripes of heat-resistant AES.
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (7)
1. The heat-resistant AES resin composition is characterized by consisting of the following components in parts by weight:
the crosslinking degree of the ethylene propylene diene monomer of the acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer is 40-70 wt%;
the heat-resistant agent is an N-phenylmaleimide-styrene-maleic anhydride copolymer.
2. The heat-resistant AES resin composition as recited in claim 1, wherein the weight average molecular weight of the acrylonitrile-ethylene propylene diene monomer-styrene graft copolymer is 50,000-500,000, and the weight percentage content of the ethylene propylene diene monomer is 20-80 wt%.
3. The heat-resistant AES resin composition as recited in claim 1, wherein the styrene-acrylonitrile copolymer has a weight average molecular weight of 100,000-500,000 and a content of acrylonitrile in a weight percentage of 15-40 wt%.
4. The heat-resistant AES resin composition of claim 1, wherein the processing aid comprises one or a mixture of lubricants, antioxidants, and mold release agents.
5. The heat-resistant AES resin composition of claim 4, wherein the lubricant is pentaerythritol stearate or ethylene bis-stearamide; the antioxidant is hindered phenol or phosphite ester antioxidant; the release agent is a silicone release agent.
6. A method for preparing the heat-resistant AES resin composition as claimed in claim 1, comprising the steps of:
s1, weighing the raw materials according to the proportion, and premixing in a high-speed mixer;
s2, feeding the premix obtained in the step S1 into a double-screw extruder through a metering device, melting and compounding materials under the conveying, shearing and mixing of screws, and then performing extrusion, strip drawing, cooling and grain cutting to obtain the heat-resistant AES resin composition.
7. The method for preparing the heat-resistant AES resin composition as recited in claim 6, wherein the length-diameter ratio of the screw of the twin-screw extruder is 36-44, the extrusion temperature is 180-250 ℃, and the screw rotation speed is 200-500 rpm.
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| CN112759852B (en) * | 2020-12-29 | 2022-07-12 | 金发科技股份有限公司 | Acrylonitrile-styrene copolymer material and preparation method thereof |
| CN113512252B (en) * | 2021-07-06 | 2023-01-24 | 上海金发科技发展有限公司 | Polypropylene composition and preparation method thereof |
| CN116082784B (en) * | 2023-04-10 | 2023-06-27 | 佛山市塑聚新材料科技有限公司 | Flame-retardant composite material and preparation method and application thereof |
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| EP3299415A1 (en) * | 2015-05-19 | 2018-03-28 | Denka Company Limited | Heat-resistant resin composition and method for producing same |
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| EP3299415A1 (en) * | 2015-05-19 | 2018-03-28 | Denka Company Limited | Heat-resistant resin composition and method for producing same |
| CN105419143A (en) * | 2015-12-24 | 2016-03-23 | 上海锦湖日丽塑料有限公司 | Heat-resistant ASA resin composition with tiger wrinkle defect eliminated and preparation method thereof |
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