CN111875898A - ASA resin suitable for automotive millimeter wave radar and preparation method thereof - Google Patents
ASA resin suitable for automotive millimeter wave radar and preparation method thereof Download PDFInfo
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- CN111875898A CN111875898A CN202010598369.2A CN202010598369A CN111875898A CN 111875898 A CN111875898 A CN 111875898A CN 202010598369 A CN202010598369 A CN 202010598369A CN 111875898 A CN111875898 A CN 111875898A
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention relates to ASA resin suitable for automotive millimeter wave radar and a preparation method thereof; comprises the following components in parts by weight: 45-70 parts of styrene-acrylonitrile (SAN) copolymer, 25-40 parts of acrylate-styrene-acrylonitrile rubber powder (ASA) rubber powder, 3-15 parts of organic-inorganic hybrid resin, 0.1-1 part of antioxidant, 0.1-1 part of lubricant and 0.4-1 part of weather-resistant agent. During preparation, all the components are added into a mixing stirrer for mixing; and feeding the obtained mixture into a double-screw extruder through a weight-loss feeding machine, and blending and granulating to obtain the ASA resin suitable for the automotive millimeter wave radar. The introduction of the organic-inorganic hybrid resin can effectively reduce the dielectric constant of the ASA resin, can effectively reduce the millimeter wave radar wave absorption of the material, and simultaneously the obtained ASA resin can keep good impact toughness and weather resistance, and is suitable for automobile exterior parts.
Description
Technical Field
The invention belongs to the fields of polymer blending and polymer molding processing, and relates to ASA resin suitable for automotive millimeter wave radar and a preparation method thereof; in particular to ASA resin which has low ASA resin dielectric constant, high weather resistance and impact toughness and is suitable for automotive millimeter wave radars and a preparation method thereof.
Background
In recent years, with the improvement of the requirements of automobiles on characteristics such as intelligent driving and safe collision avoidance, millimeter wave radars have become one of sensors in intelligent automobile design, and have high requirements on dielectric constants and dielectric losses of parts, and if the dielectric constant of a material is high, there is a risk that a signal is weakened when a radar wave penetrates through the material. The dielectric constant of ordinary ASA is generally 3.2-3.4, which may have some influence on the radar wave penetration. On the other hand, as an outdoor product used for a long time, the automobile exterior trim has clear requirements on weather resistance, impact toughness and the like of the material.
The ASA resin is an acrylonitrile-acrylate-styrene terpolymer and is widely applied to automobile exterior trimming parts due to excellent weather resistance, dimensional stability and impact toughness. Chinese patent 201010265169.1 reports a highly weather-resistant acrylic resin and a preparation method thereof, the material can meet the basic requirements of automobile exterior parts on the material, but the dielectric constant of ASA cannot be effectively reduced, and the prepared relevant automobile exterior parts can possibly interfere with automobile millimeter wave radar signals. Chinese patent 201710706302.4 reports that an ASA resin mixture with high wave-transmitting rate and a radome prepared from the ASA resin mixture successfully reduce the dielectric constant of the ASA resin and improve the transmittance of radar waves by adding glass beads into the ASA resin, but the glass beads are inorganic fillers, so that the toughness of ASA is significantly affected, and the requirement of automobile exterior parts on the toughness of materials cannot be met.
According to the invention, by adding organic-inorganic hybrid molecules with good compatibility with ASA resin, the dielectric constant of the ASA resin is reduced on the premise of not influencing the weather resistance, the dimensional stability and the impact toughness of the ASA resin, so that the absorption of the ASA resin on automobile millimeter wave radar signals is reduced, and the ASA resin is expected to be applied to areas such as automobile grids, rearview mirrors, column plates and the like
Disclosure of Invention
The invention aims to provide ASA resin suitable for automotive millimeter wave radar. The invention also aims to provide a preparation method of the ASA resin suitable for the automotive millimeter wave radar.
The purpose of the invention is realized by the following technical scheme:
the ASA resin composition suitable for the automotive millimeter wave radar comprises the following components in parts by weight:
the organic-inorganic hybrid resin is characterized in that the organic-inorganic hybrid resin is polyhedral oligomeric silsesquioxane (POSS) which is shown in the following formula,
in the formula, the POSS cage-shaped molecule top chain segment is acrylate polymer, styrene-acrylonitrile copolymer and epoxy polymer chain segment. The structural design has the advantages that the Si-O-Si structure can effectively reduce the dielectric constant of the ASA resin, and the R group is the organic group, so that the compatibility of the POSS cage and the ASA resin can be effectively improved. Meanwhile, the compatibility and weather resistance of the organic-inorganic hybrid resin and the ASA resin are also considered. Such as dodecafluoroheptyl-propyl cage-type silsesquioxane, the dielectric constant of the resin may be low, but the compatibility with ASA resin is poor, and the performance of the resin is greatly reduced when the resin is blended with ASA resin, so that the resin cannot meet the practical use.
Preferably, the molecular weight of the SAN resin is 80000-200000. Wherein the acrylonitrile content is 26-38%.
Preferably, the ASA rubber powder has a butyl acrylate rubber content of 30-60% and a rubber particle size of 100-600 nm.
Preferably, the antioxidant is one or a mixture of more of 2, 6-di-tert-butyl-4-methylphenol, octadecyl beta- (3, 5-di-tert-butyl-4-hydroxy-phenyl) propionate, dilauryl thiodipropionate, distearyl thiodipropionate, tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-di-tert-butyl) tetraol diphosphite and pentaerythritol diphosphite dioctadecyl ester.
Preferably, the lubricant is one or a mixture of silane polymer, fatty acid salt, fatty acid amide, stearic acid, butyl stearate, oleamide and ethylene bisstearamide.
Preferably, the weather resisting agent is one or a mixture of several of an ultraviolet absorber and a hindered amine weather resisting agent.
In a second aspect, the present invention also relates to a preparation method of the ASA resin composition suitable for automotive millimeter wave radar, comprising the steps of:
the method comprises the following steps:
s1, adding the styrene-acrylonitrile copolymer, the acrylate-styrene-acrylonitrile rubber powder, the organic-inorganic hybrid resin, the antioxidant, the lubricant and the weather-resistant agent into a mixing stirrer for mixing;
s2, feeding the mixture obtained in the step S1 into a double-screw extruder through a weight-loss feeder, and then blending and granulating through the double-screw extruder to obtain the ASA resin composition.
Preferably, the temperature of a machine barrel of the double-screw extruder is 190-250 ℃, and the rotating speed of a screw is 300-700 rpm.
The action mechanism of the invention is as follows: the inorganic structure in the organic-inorganic hybrid resin can effectively reduce the dielectric constant and dielectric loss of the ASA resin, the organic structure part ensures the compatibility of the resin and an ASA matrix, and the weather resistance and impact toughness of the ASA resin are not influenced.
Compared with the prior art, the invention has the beneficial effects that:
1) the common method for reducing the dielectric constant of ASA is a method of adding an inorganic filler, but the ASA resins prepared by the methods have difficulty in obtaining higher impact toughness and obviously reduced weather resistance, and are difficult to meet the requirements of automobiles on exterior parts; the specific organic-inorganic hybrid resin is added to reduce the dielectric constant of the ASA resin, and simultaneously, the weather resistance and impact toughness of the ASA resin are kept;
2) the organic-inorganic hybrid resin has obvious advantages in impact toughness and weather resistance compared with the organic filler while keeping low dielectric constant;
3) the method is simple and easy to implement, and finally the plastic part can effectively meet the basic requirements of the automobile exterior trimming parts and is suitable for application to automobile grids, column plates, rearview mirrors and other parts.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Examples 1 to 5
Examples 1 to 5 relate to ASA resin materials suitable for automotive millimeter wave radars, the ASA resin materials comprising the components and the contents shown in Table 1; SAN resin is Taiwan Qimei PN128, ASA rubber powder is Korea brocade lake XC500, organic and inorganic hybrid resin is POSS, wherein the top chain segment of cage-shaped POSS molecules is a methyl acrylate polymer chain segment (Wangwen Pingyi, ATRP method for preparing POSS/PMMA composite material and characterization, high polymer material science and engineering [ J ],2007,23 (4): 247-249), and antioxidant is Irganox 168 of Ciba company; the lubricant is N, N-ethylene bis stearamide sold in the market, and the weather resisting agent is hindered amine antioxidant (Ciba, 770 DF).
TABLE 1 Components and parts by weight
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| SAN resin | 62 | 62 | 62 | 62 | 62 |
| ASA rubber powder | 35 | 33 | 31 | 28 | 23 |
| Organic-inorganic hybrid resin | 3 | 5 | 7 | 10 | 15 |
| Antioxidant agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Lubricant agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Weather-resistant agent | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 |
The preparation method comprises the following steps:
a. weighing corresponding raw materials according to the components and the weight in the table 1;
b. then mixing SAN resin, ASA rubber powder, organic-inorganic hybrid resin, antioxidant, lubricant and weather-resistant agent in a mixing stirrer;
c. and c, blending and granulating the mixture obtained in the step b through a double-screw extruder to obtain the ASA resin particles suitable for the automotive millimeter wave radar, wherein the cylinder temperature of the extruder is 220 ℃, and the screw rotating speed is 500 rpm.
Example 6
The embodiment relates to ASA suitable for an automotive millimeter wave radar, and the preparation method comprises the following steps:
a. weighing the following raw materials in parts by weight:
b. then mixing SAN resin, ASA rubber powder, organic-inorganic hybrid resin, antioxidant, lubricant and weather-resistant agent in a mixing stirrer;
c. and c, blending and granulating the mixture obtained in the step b through a double-screw extruder to obtain the ASA resin particles suitable for the automotive millimeter wave radar, wherein the cylinder temperature of the extruder is 190 ℃, and the screw rotating speed is 700 rpm.
The weight average molecular weight of the SAN resin is 120000, and the glass transition temperature is 104 ℃;
the ASA rubber powder contains 55% of acrylate rubber, and the rubber particle size is 200 nm;
the organic-inorganic hybrid particles are POSS, wherein a cage-shaped molecular top chain segment of POSS is a polystyrene chain segment; (POSS Synthesis according to the references: Wangwen Heng et al, preparation of POSS/PS composites and their thermal Properties research, plastics science & technology [ J ],2012,40 (5): 46-49)
Irganox 1010 from Ciba, Inc.;
the lubricant is commercially available pentaerythritol stearic acid;
the weather resisting agent is TINUVIN 234.
Example 7
The embodiment relates to ASA suitable for automotive millimeter wave radar, and the preparation method is the same as that in embodiment 6, except that:
a. preparing the following components in parts by weight:
b. then mixing SAN resin, ASA rubber powder, organic-inorganic hybrid resin, antioxidant, lubricant and weather-resistant agent in a mixing stirrer;
c. and c, blending and granulating the mixture obtained in the step b through a double-screw extruder to obtain the ASA resin particles suitable for the automotive millimeter wave radar, wherein the cylinder temperature of the extruder is 250 ℃, and the rotating speed of the screws is 300 rpm.
The molecular weight of the SAN resin is 150000, and the glass transition temperature is 105.5 ℃;
the ASA rubber powder contains 53% of acrylate rubber, and the rubber particle size is 300 nm;
the organic-inorganic hybrid particles are POSS, R is styrene-acrylonitrile copolymer (POSS synthetic reference: Charter bin et al, preparation and performance research of Vinyl-POSS/St/AN composite materials, plastic science and technology [ J ], 2011.3, 39 (5): 46-49 ]);
the antioxidant is compounded by Irganox 1076 and Irganox 168 of an antioxidant Ciba company, and the ratio is 1: 1;
the lubricant is a mixture of methylene bis stearamide and N, N-ethylene bis stearamide in a ratio of 1: 1;
the weather resisting agent is TINUVIN 622.
Comparative example 1
The present comparative example was mainly used to compare the difference between a conventional ASA resin (ASA resin typical of current automotive exterior parts) and an ASA resin of the present invention suitable for automotive millimeter wave radars. The formula comprises 62 parts of SAN resin, 35 parts of ASA rubber powder and 0.2 part of antioxidant; 0.2 part of lubricant, 0.6 part of weather resistant agent, and the types and preparation methods of the related raw materials are the same as those of example 1.
Comparative example 2
The comparison example is mainly used for comparing the difference between the ASA resin and the ASA resin which is suitable for the automotive millimeter wave radar after the dielectric constant of the ASA resin is reduced by adding the inorganic filler.
The comparative example is carried out according to the following mixture ratio, the mica powder is high-purity mica sold in the market, and other raw materials and the preparation method are the same as those in the example 4:
comparative example 3
The comparison example is mainly used for comparing the difference between the ASA resin and the ASA resin which is suitable for the automotive millimeter wave radar after the dielectric constant of the ASA resin is reduced by adding the inorganic filler.
The comparative example is carried out according to the following mixture ratio, the grain diameter of the glass microsphere is 30 μm, and other raw materials and preparation methods are the same as those of the example 4:
comparative example 4
The comparative example is mainly used for comparing the difference between the ASA resin prepared by adding dodecafluoroheptyl-propyl polyhedral oligomeric silsesquioxane and the ASA resin suitable for the automotive millimeter wave radar of the invention
Comparative example dodecafluoroheptylpropyl polyhedral oligomeric silsesquioxane was prepared according to the following formulation, with reference to CN101875667B, and other starting materials and preparation methods as in example 4:
effects of the implementation
The physical properties of the ASA particles were tested with reference to ISO527, ISO179, ISO75, ISO178 standard. 800KJ/m according to SAE J2527 by testing the dielectric constant of ASA at 10GHz2After irradiation, the weathering resistance of the as-colored ASA resin was evaluated, and the examples and comparative examples were evaluated
The test results are shown in table 2:
TABLE 2 ASA resin test results of examples 1-7 and comparative examples 1-2
The results of examples 1 to 5 show that the organic-inorganic hybrid resin can significantly reduce the dielectric constant of the ASA resin after the organic-inorganic hybrid resin is added, and the dielectric constant tends to decrease with the increase of the content of the organic-inorganic hybrid resin. Through the embodiment 4 and the comparative example 1, the ASA resin suitable for the automotive millimeter wave radar has no obvious difference in impact toughness and weather resistance with general ASA resin, can meet the basic requirements of automotive exterior parts, but has obviously reduced dielectric constant, and is more beneficial to penetrating millimeter wave radar waves. Through the example 4 and the comparative examples 2 and 3, the organic-inorganic hybrid resin of the invention has obvious advantages in impact toughness and weather resistance compared with the addition of inorganic filler while keeping low dielectric constant. With the aid of example 4 and comparative example 4, although comparative example 4 is also an organic-inorganic hybrid resin, the resin prepared in comparative example 4 has significantly lower notched impact strength than the ASA resin prepared in example 4 according to the invention, which is suitable for automotive millimeter-wave radars, regardless of the flexural modulus, due to the poor compatibility of the characteristic functional groups with the ASA resin matrix. Can not meet the performance requirements of automobile part materials.
In conclusion, the method is simple and easy to implement, the specific organic-inorganic hybrid resin is selected to be added into the ASA resin, so that the dielectric constant of the ASA resin can be effectively reduced, the impact toughness and excellent weather resistance of the ASA resin are ensured, and the ASA resin is expected to be applied to parts such as automobile grilles, column plates, rearview mirrors and the like.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. An ASA resin composition suitable for automotive millimeter wave radar, which comprises the following components in parts by weight:
2. the ASA resin composition suitable for automotive millimeter wave radars according to claim 1, wherein the styrene-acrylonitrile copolymer has a weight average relative molecular mass of 80,000-200,000.
3. The ASA resin composition suitable for automotive millimeter wave radars as claimed in claim 1, wherein the acrylate-styrene-acrylonitrile rubber powder has a butyl acrylate rubber content of 30% -60% and a rubber particle size of 100-600 nm.
4. The ASA resin composition suitable for automotive millimeter wave radars according to claim 1, wherein the organic-inorganic hybrid resin is a composite of polyhedral oligomeric silsesquioxane, the molecular structure of which is as follows:
wherein, the POSS cage-shaped molecule top chain segment is acrylate polymer, styrene-acrylonitrile copolymer and epoxy polymer chain segment.
5. The ASA resin composition suitable for automotive millimeter wave radars according to claim 4, wherein the saturated polyolefin-based molecules comprise ethylene-propylene polymer segments.
6. The ASA resin composition suitable for automotive millimeter wave radars according to claim 1, wherein the antioxidant is one or a mixture of 2, 6-di-tert-butyl-4-methylphenol, octadecyl beta- (3, 5-di-tert-butyl-4-hydroxy-phenyl) propionate, dilauryl thiodipropionate, distearyl thiodipropionate, tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-di-tert-butyl) quarternary alcohol diphosphite, and dioctadecyl pentaerythritol diphosphite.
7. The ASA resin composition suitable for automotive millimeter wave radars according to claim 1, wherein the lubricant is one or a mixture of silane polymer, fatty acid salt, fatty acid amide, stearic acid, butyl stearate, oleamide, ethylene bis stearamide, polyolefin wax.
8. The ASA resin composition suitable for automotive millimeter wave radars according to claim 1, wherein the weather resistant agent is one or a mixture of ultraviolet absorbers and hindered amine weather resistant agents.
9. A method for preparing an ASA resin composition suitable for automotive millimeter wave radars as claimed in claim 1, comprising the steps of:
s1, adding the styrene-acrylonitrile copolymer, the acrylate-styrene-acrylonitrile rubber powder, the organic-inorganic hybrid resin, the antioxidant, the lubricant and the weather-resistant agent into a mixing stirrer for mixing;
s2, feeding the mixture obtained in the step S1 into a double-screw extruder through a weight-loss feeder, and then blending and granulating through the double-screw extruder to obtain the ASA resin composition.
10. The method for preparing the polypropylene composition according to claim 9, wherein the barrel temperature of the twin-screw extruder is 190 to 250 ℃ and the screw rotation speed is 300 to 700 rpm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113372660A (en) * | 2021-07-05 | 2021-09-10 | 安徽江淮汽车集团股份有限公司 | ASA composite material and preparation method thereof |
| CN113416366A (en) * | 2021-06-22 | 2021-09-21 | 上海锦湖日丽塑料有限公司 | ASA resin composition with ultrasonic absorption performance and preparation method and application thereof |
| CN114685909A (en) * | 2020-12-30 | 2022-07-01 | 上海汽车集团股份有限公司 | Resin composition and method for producing the same |
| CN116574350A (en) * | 2023-04-26 | 2023-08-11 | 中山市富恒科技有限公司 | ASA composite material for automobiles and preparation method thereof |
| CN114891307B (en) * | 2022-03-31 | 2023-12-19 | 金发科技股份有限公司 | ASA material and preparation method and application thereof |
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