CN110643121A - High-heat-resistance metal silver spraying-free ASA material and preparation method thereof - Google Patents
High-heat-resistance metal silver spraying-free ASA material and preparation method thereof Download PDFInfo
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- CN110643121A CN110643121A CN201911055158.8A CN201911055158A CN110643121A CN 110643121 A CN110643121 A CN 110643121A CN 201911055158 A CN201911055158 A CN 201911055158A CN 110643121 A CN110643121 A CN 110643121A
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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
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Abstract
The invention relates to a high-heat-resistance metal silver spray-free ASA material which is prepared from the following components in parts by mass: 10-38 parts of ASA rubber powder, 45-80 parts of SAN resin, 0-15 parts of heat-resistant agent, 0-10 parts of toughening agent, 0.1-1 part of antioxidant, 0.1-1 part of ultraviolet absorber, 0.1-1 part of light stabilizer, 1-5 parts of coupling agent and 1-10 parts of metallic silver pigment. The high-heat-resistance metal silver spray-free ASA material can replace the conventional spray coating material to manufacture automobile exterior part products because of good heat resistance and uniformity. By adding the ASA heat-resistant agent into the metal silver spraying-free ASA material and simultaneously adding the toughening agent for promoting the uniform fusion and distribution of the inorganic coloring phase and the resin organic phase, the heat-resistant agent still maintains good molecular acting force with the ASA continuous phase after the macromolecular group of the heat-resistant agent is introduced, and the heat-resistant effect is improved remarkably.
Description
Technical Field
The invention relates to a high-heat-resistance metal silver spray-free ASA material and a preparation method thereof.
Background
The green and sustainable development is a necessary way for the society to live at present, the material serving as a basic framework for constructing various objects is bound to move to the front of the wave of environmental protection development, and the 'spraying-free' material has the fundamental purpose of replacing a paint spraying process and has the characteristic of being recyclable in percentage, so that the material is widely researched and applied to various plastic parts.
The ASA material is a spraying-free substrate material with the most excellent neutral cost ratio of general engineering plastics, has good light aging resistance, and has a price almost the same as that of an ABS material without weather resistance, so that the ASA material is used by a plurality of researchers to develop various spraying-free effects. The metal silver spraying-free ASA is one of the metal silver spraying-free ASA, different metal coloring agents such as silver powder, silver paste, aluminum strips and the like are added into an ASA base material, and the metal coloring agents can be fully dispersed and fused under the action of a dispersing auxiliary agent and a lubricating auxiliary agent, so that the metal silver spraying-free ASA finally presents metal flickering texture. However, in many studies, the overall rigidity of the material is reduced to different degrees due to the addition of excessive small-molecule additives after the metallic coloring pigment is added, which directly affects the overall heat resistance of the material, and the study on the mechanical properties of the material is rare.
The ASA material is a graft copolymer consisting of acrylic rubber without double bonds, acrylonitrile and propylene. Because the light aging resistance is superior to ABS, PC and other materials, the light aging resistance is widely used for external parts with direct illumination. For acrylate rubber, although the aging resistance is better than that of butadiene rubber containing double bonds, the impact toughness is less than half of that of ABS materials, which cannot meet most of the material performance requirements, so that an additional toughening agent is often added during modification as one of means for improving the impact of ASA. As is well known, toughness and rigidity are a characteristic mechanics of this trade-off, and when the impact strength of ASA is improved, the rigidity data such as heat resistance thereof is significantly reduced, and as an exterior part, heat resistance is a very important characteristic property, which directly affects the appearance of visible defects such as deformation, light loss and the like of a product under a high-temperature environment due to high temperature. For the spraying-free material, although the heat resistance of the material can be improved by the conventional heat-resistant auxiliary agent, the fluidity of the material is greatly reduced, and the metal effect is greatly reduced due to the compatibility problem of the heat-resistant agent and the metal coloring pigment, so that the significance of the metal effect of the metal silver spraying-free material is lost.
Disclosure of Invention
The invention provides a high-heat-resistance metal silver spray-free ASA material, which can replace the traditional spray coating material to manufacture automobile exterior part products because of excellent heat resistance and uniformity.
The first technical scheme of the invention) is realized by the following technical scheme:
the high-heat-resistance metal silver spraying-free ASA material is prepared from the following components in parts by mass:
ASA rubber powder: 10 to 38 portions of
SAN resin: 45 to 80 portions of
Heat-resistant agent: 0 to 15 parts of
A toughening agent: 0 to 10 parts of
Antioxidant: 0.1 to 1 portion
Ultraviolet absorber: 0.1 to 1 portion
Light stabilizer: 0.1 to 1 portion
Coupling agent: 1 to 5 portions of
Metallic silver pigment: 1 to 10 parts by weight of a surfactant,
the ASA rubber powder contains 30-70% of rubber, and is prepared by compounding 70% of rubber powder with a particle size of 50nm by mass and 30% of rubber powder with a particle size of 300nm by mass.
The coloring effect of the small-particle-size rubber powder is better than that of the large-particle-size rubber powder, but the impact toughness of the large-particle-size rubber powder is higher than that of the small-particle-size rubber powder. The ASA rubber powder prepared by the proportion has good coloring effect and impact toughness effect.
Further, the SAN resin has a relative molecular weight of 20, 0000-50, 0000, and a melt index of 5-40 g/10 min.
Furthermore, the heat-resistant agent is formed by mixing one or more than one of N-phenylmaleimide and alpha-methyl styrene according to any proportion.
Further, the toughening agent is a block copolymer EMA of ethylene and methyl acrylate, wherein the mass fraction of the methyl acrylate is 8-40%.
Further, the antioxidant is a hindered phenol antioxidant or a phosphite antioxidant.
Further, the ultraviolet absorbent is a benzotriazole absorbent.
Further, the light stabilizer is a hindered amine light stabilizer.
Further, the coupling agent is formed by mixing one or more than two of a silane coupling agent KH550 or an aluminate coupling agent ACA-K30 according to any proportion.
Further, the metallic silver pigment is formed by mixing one or more than two of aluminum powder, silver powder, aluminum paste, alumina powder or silver paste according to any proportion.
The scheme II) of the invention is realized by the following technical scheme:
the processing and preparation method of the high-heat-resistance metal silver spray-free ASA material comprises the following steps:
1) firstly, weighing the following components in parts by mass: 10-38 parts of ASA rubber powder, 45-80 parts of SAN resin, 0-15 parts of heat-resistant agent, 0-10 parts of toughening agent, 0.1-1 part of antioxidant, 0.1-1 part of ultraviolet absorbent, 0.1-1 part of light stabilizer, 1-5 parts of coupling agent and 1-10 parts of metallic silver pigment,
2) then premixing the metallic silver pigment, the coupling agent and the ASA rubber powder, fully mixing, drying for 7-9 hours in an oven at 75-85 ℃, and sealing for later use;
3) uniformly mixing the premixed raw materials in the step 2) with other raw materials, and then extruding and granulating.
Further, a double-screw extruder is adopted during extrusion granulation, and the conditions set by the double-screw extruder are as follows: the temperature is 200-240 ℃, and the rotating speed is 300-350 r/min; and (5) granulating and molding the extruded long strip by cooling water in a water tank.
Compared with the prior art, the invention has the following beneficial effects: the high-heat-resistance metal silver spray-free ASA material can replace the conventional spray coating material to manufacture automobile exterior part products because of good heat resistance and uniformity. By adding the ASA heat-resistant agent into the metal silver spraying-free ASA material and simultaneously adding the toughening agent for promoting the uniform fusion and distribution of the inorganic coloring phase and the resin organic phase, the heat-resistant agent still maintains good molecular acting force with the ASA continuous phase after the macromolecular group of the heat-resistant agent is introduced, and the heat-resistant effect is improved remarkably.
In order to improve the dispersion distribution of the metal inorganic pigment in the ASA material to a greater extent, the surface modification pretreatment is carried out on the pigment in advance, and the surface interfacial energy of the pigment is reduced by wetting with a coupling agent, so that the inorganic and organic contact fusion in a subsequent melt blending system is more flexible, and a more uniform color effect is shown.
The specific implementation is as follows
The invention is further illustrated by the following examples and embodiments
Example 1
ASA rubber powder: 29.5 parts
SAN resin: 55.5 parts of
Heat-resistant agent: 8 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
1) Accurately weighing ASA rubber powder, SAN resin, heat-resistant agent, toughening agent, antioxidant, ultraviolet absorbent, light stabilizer, coupling agent and metallic silver pigment,
2) then premixing the metallic silver pigment, the coupling agent and the ASA rubber powder, fully mixing, drying for 8 hours in an oven at 80 ℃, and sealing for later use;
3) uniformly mixing the premixed raw materials in the step 2) with other raw materials, and then extruding and granulating.
In this example 1, the ASA rubber powder is prepared from a tableted BP130 rubber powder, the rubber content of which is 55 parts, and the particle size composition of which is 50nm (70% by weight) and 300nm (30% by weight); the SAN resin is NX3260 of Ningbo Taiwan, and the AN content is about 32 parts; the heat-resistant agent is IZ1018M of Polyscope in the Netherlands, and the effective component of the heat-resistant agent is N-phenylmaleimide; the toughening agent EMA is selected from HP4051 of DuPont; the antioxidant is 1010 and 168 of BASF; UV absorbers and light stabilizers are UV-234 and 770 from BASF; the metal silver pigment is spherical aluminum powder TLQT5 of the golden Hao technology;
example 2
ASA rubber powder: 29.5 parts
SAN resin: 47.5 parts of
Heat-resistant agent: 16 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In this example, the content of heat-resistant agent is increased by 8 parts based on example 1, and the content of SAN resin is reduced by 8 parts, and other proportions and processing operation modes are unchanged.
Example 3
ASA rubber powder: 29.5 parts
SAN resin: 55.5 parts of
Heat-resistant agent: 8 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 5 portions of
Metallic silver pigment: 4.5 parts of
In this example, the content of 4 parts of aluminate coupling agent is increased on the basis of example 1, and other proportions and processing operation modes are not changed.
Example 4
ASA rubber powder: 29.5 parts
SAN resin: 55.5 parts of
Heat-resistant agent: 8 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Silane coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In the embodiment, the aluminate coupling agent is replaced by the silane coupling agent in an equal proportion on the basis of the embodiment 1, and other proportions and processing operation modes are not changed.
Example 5
ASA rubber powder: 29.5 parts
SAN resin: 55.5 parts of
Heat-resistant agent: 8 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In this example, all the raw materials were mixed in proportion and strand extruded for granulation without changing the formulation ratio of example 1, but a pre-mixing method was not used in the processing.
Example 6
ASA rubber powder: 10 portions of
SAN resin: 55.5 parts of
Heat-resistant agent: 8 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In this example, the lower limit of the amount of ASA powder is set to 10 parts based on example 1, and the other compounding ratios and processing operation are not changed.
Example 7
ASA rubber powder: 38 portions of
SAN resin: 55.5 parts of
Heat-resistant agent: 8 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In this example, the upper limit of the amount of ASA powder used was 38 parts based on example 1, and the other compounding ratios and processing operation were not changed.
Example 8
ASA rubber powder: 29.5 parts
SAN resin: 45 portions of
Heat-resistant agent: 8 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In this example, the lower limit of the amount of SAN resin used was set to 45 parts based on example 1, and the other formulation and processing operation were not changed.
Example 9
ASA rubber powder: 29.5 parts
SAN resin: 80 portions
Heat-resistant agent: 8 portions of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In this example, the amount of SAN resin used was set to an upper limit of 80 parts based on example 1, and other compounding ratios and processing operation were not changed.
Comparative example 1
ASA rubber powder: 29.5 parts
SAN resin: 63.5 parts of
A toughening agent: 7 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In the comparative example, the heat-resistant agent is removed on the basis of the example 1, the SAN resin content of 8 parts is increased, and other proportions and processing operation modes are unchanged.
Comparative example 2
ASA rubber powder: 29.5 parts
SAN resin: 62.5 portions
Heat-resistant agent: 8 portions of
Antioxidant: 0.3 part
Ultraviolet absorber: 0.4 portion of
Light stabilizer: 0.4 portion of
Aluminate coupling agent: 1 part of
Metallic silver pigment: 4.5 parts of
In the comparative example, the toughening agent is removed on the basis of the example 1, the SAN resin content of 7 parts is increased, and other proportions and processing operation modes are unchanged.
Performance testing and evaluation
The following test methods and standards were used to perform the performance tests on the material formulations:
material density (specific gravity): the method is carried out according to ISO 1183-1 standard, and the experimental method adopts the method A;
tensile strength: according to ISO 527-2 standard, the test conditions are as follows: the stretching speed is 50 mm/min;
flexural modulus: according to ISO 178 standard, the test conditions are as follows: the bending speed is 2 mm/min;
notched izod impact strength: according to ISO 180 standard, the test conditions are as follows: a 2mm gap at 23 ℃;
heat distortion temperature: according to ISO 75 standard, the test condition is 0.45MPa load;
and (3) high-temperature storage: placing 120mm by 2mm sample in 100 deg.C high temperature aging oven for 24hr, and observing deformation degree of sample;
evaluation of appearance color: observing the color difference value delta E of the color plate by using a color difference meter (the smaller the numerical value is, the better the effect is), wherein the size of the color plate is 120mm x 2 mm;
all the data for example 1 are best seen by comparing examples 1, 2, 3, 4, 5. Compared with the examples 1 and 2, the heat resistance of the material can be improved by the heat-resistant agent, but the heat resistance of the metal silver spray-free ASA material is improved to a certain extent, the addition amount of the heat-resistant agent is doubled, the thermal deformation is improved by only 2 ℃, and the impact strength and the color difference value are greatly influenced; comparing example 1 with examples 3 and 4, it can be seen that the amount of the coupling agent does not have much influence on the mechanical properties, but the excessive amount of the coupling agent is small molecular substances, so that the coupling agent can migrate to the surface of a product to influence the color effect of the material; the selection of a proper coupling agent is very critical, and in example 4, the mechanical property and the color difference value are greatly reduced after the conventional silane coupling agent is replaced. For example 5, if no pre-mixing is adopted, the overall material performance is reduced to different degrees, and the color difference is seriously deviated, which shows that the pre-mixing treatment of the pigment is very important for the metallic silver spray-free material.
From comparative examples 1 and 2, the heat-resistant agent is a direct factor affecting the heat-resistant effect of the material. The toughening agent only affects the toughness of the material conventionally, but the EMA toughening agent selected by the invention can improve the toughness, but has little influence on thermal deformation, and because rigid methyl methacrylate macromolecules exist in the EMA toughening agent, the compatibility of the whole material is greatly improved, so that the thermal deformation temperature of the material is not greatly improved after the toughening agent is removed.
The above embodiments are merely illustrative of the technical solutions of the present invention, and the present invention is not limited to the above embodiments, and any modifications or alterations according to the principles of the present invention should be within the protection scope of the present invention.
Claims (10)
1. A high heat-resistant metal silver spraying-free ASA material is characterized in that: the adhesive is prepared from the following components in parts by mass:
ASA rubber powder: 10 to 38 portions of
SAN resin: 45 to 80 portions of
Heat-resistant agent: 0 to 15 parts of
A toughening agent: 0 to 10 parts of
Antioxidant: 0.1 to 1 portion
Ultraviolet absorber: 0.1 to 1 portion
Light stabilizer: 0.1 to 1 portion
Coupling agent: 1 to 5 portions of
Metallic silver pigment: 1 to 10 parts by weight of a surfactant,
the ASA rubber powder contains 30-70% of rubber, and is prepared by compounding 70% of rubber powder with a particle size of 50nm by mass and 30% of rubber powder with a particle size of 300nm by mass.
2. The high heat-resistant metallic silver spray-free ASA material as claimed in claim 1, wherein: the SAN resin has the relative molecular weight of 20, 0000-50 and 0000-melt index of 5-40 g/10 min.
3. The high heat-resistant metallic silver spray-free ASA material as claimed in claim 1, wherein: the heat-resistant agent is formed by mixing one or more than one of N-phenylmaleimide and alpha-methylstyrene according to any proportion.
4. The high heat-resistant metallic silver spray-free ASA material as claimed in claim 1, wherein: the toughening agent is a block copolymer EMA of ethylene and methyl acrylate, wherein the mass fraction of the methyl acrylate is 8-40%.
5. The high heat-resistant metallic silver spray-free ASA material as claimed in claim 1, wherein: the antioxidant is hindered phenol antioxidant or phosphite antioxidant.
6. The high heat-resistant metallic silver spray-free ASA material as claimed in claim 1, wherein: the ultraviolet absorbent is a benzotriazole absorbent.
7. The high heat-resistant metallic silver spray-free ASA material as claimed in claim 1, wherein: the light stabilizer is hindered amine light stabilizer.
8. The high heat-resistant metallic silver spray-free ASA material as claimed in claim 1, wherein: the coupling agent is one or more than two of a silane coupling agent KH550 or an aluminate coupling agent ACA-K30 mixed according to any proportion.
9. The high heat-resistant metallic silver spray-free ASA material as claimed in claim 1, wherein: the metal silver pigment is formed by mixing one or more than two of aluminum powder, silver powder, aluminum paste, alumina powder or silver paste according to any proportion.
10. The preparation method of the high heat-resistant metallic silver spray-free ASA material as claimed in any one of claims 1 to 9, wherein the preparation method comprises the following steps: comprises the following steps:
1) firstly, weighing the following components in parts by mass: 10-38 parts of ASA rubber powder, 45-80 parts of SAN resin, 0-15 parts of heat-resistant agent, 0-10 parts of toughening agent, 0.1-1 part of antioxidant, 0.1-1 part of ultraviolet absorbent, 0.1-1 part of light stabilizer, 1-5 parts of coupling agent and 1-10 parts of metallic silver pigment,
2) then premixing the metallic silver pigment, the coupling agent and the ASA rubber powder, fully mixing, and drying in an oven at 75-85 ℃ for 7-9 hours;
3) uniformly mixing the premixed raw materials in the step 2) with other raw materials, and then extruding and granulating.
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| CN111675892A (en) * | 2020-05-28 | 2020-09-18 | 宁波泰甬汽车零部件有限公司 | High-heat-resistance electroplating-free PC/ASA alloy material for automotive heat dissipation grating |
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