CN113372660B - ASA composite material and preparation method thereof - Google Patents
ASA composite material and preparation method thereof Download PDFInfo
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- CN113372660B CN113372660B CN202110758686.0A CN202110758686A CN113372660B CN 113372660 B CN113372660 B CN 113372660B CN 202110758686 A CN202110758686 A CN 202110758686A CN 113372660 B CN113372660 B CN 113372660B
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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 an ASA composite material and a preparation method thereof, wherein the ASA composite material comprises the following components in parts by weight: 20-60 parts of SAN resin, 20-40 parts of ASA high-rubber powder, 3-8 parts of compatilizer, 5-30 parts of glass fiber, 0.5-5 parts of modified porous filler, 0.2-0.6 part of antioxidant and 0.2-0.5 part of lubricant, wherein the SAN resin is an acrylonitrile-styrene copolymer polymerized by an emulsion method or a suspension method, and comprises 30-36% of acrylonitrile by mass percentage, and the weight-average molecular weight M W 10-18 ten thousand; the ASA high-glue powder is acrylonitrile-acrylate-styrene copolymer, wherein the content of acrylate-olefin rubber phase is 40-60%, the content of acrylonitrile is 11-15wt%, the average particle diameter is 100-1000nm, and the weight average molecular weight M W Is 12-50 ten thousand. The dielectric constant of the ASA composite material is lower than that of the conventional ASA material, the weather resistance and the impact toughness of the ASA composite material are both higher than those of the conventional ASA material, and the ASA composite material is suitable for preparing automotive millimeter wave radars.
Description
Technical Field
The invention relates to the field of composite material preparation, in particular to an ASA composite material and a preparation method thereof.
Background
With the progress of social economy, the requirements of automobiles on characteristics such as intelligent driving, safety and collision avoidance are higher and higher, and the millimeter wave radar becomes one of sensors commonly used by intelligent automobiles. Millimeter wave radars have high requirements for the dielectric constant and the dielectric loss of the material for manufacturing parts, and if the dielectric constant of the material is high, there may be a risk that signals are weakened when radar waves penetrate the material.
The dielectric constant of the prior ASA is generally 3.2-3.4, which can adversely affect the radar wave penetration. Moreover, the weather resistance, impact toughness and the like of the existing ASA material are difficult to meet the requirements of automobile exterior parts.
Therefore, how to provide an ASA composite material suitable for automotive millimeter wave radars becomes a technical problem which needs to be solved urgently in the field.
Disclosure of Invention
The invention aims to provide a new technical scheme of an ASA composite material suitable for automotive millimeter wave radars.
According to a first aspect of the present invention, an ASA composite is provided.
The ASA composite material comprises the following components in parts by weight:
the SAN resin is an acrylonitrile-styrene copolymer polymerized by an emulsion method or a suspension method, and comprises 30-36% of acrylonitrile by mass percent and a weight average molecular weight M W 10-18 ten thousand;
the ASA high-rubber powder is acrylonitrile-acrylate-styrene copolymer, wherein the content of acrylate-olefin rubber phase is 40-60%, the content of acrylonitrile is 11-15wt%, the average particle diameter is 100-1000nm, and the weight average molecular weight M is W Is 12-50 ten thousand.
Optionally, the compatibilizer is at least one of acrylonitrile-styrene-maleic anhydride terpolymer, styrene-maleic anhydride binary copolymer, acrylonitrile-styrene grafted maleic anhydride, and styrene grafted maleic anhydride.
Optionally, the content of maleic anhydride in the compatibilizer is 1% -20%.
Optionally, the glass fiber is a modified cordierite-based glass fiber.
Optionally, the content of the metal oxide in the modified cordierite-based glass fiber is as follows by mass percent:
SiO 2 40-45 percent of CaO, 5-15 percent of CaO, 10-20 percent of MgO and Al 2 O 3 12-15% of B 2 O 3 7-15% and Fe 2 O 3 Is 1-3%.
Optionally, the modification method of the modified cordierite-based glass fiber is specifically as follows:
soaking cordierite-based glass fiber in anhydrous sulfuric acid for 0.5-1h, draining, washing with water, performing post-treatment in 5% ammonia gas atmosphere until the impregnation liquid of the glass fiber is neutral, and drying at 140 ℃ under 120-.
Optionally, the modified porous filler is a modified molecular sieve, and the framework SiO of the modified molecular sieve 2 /Al 2 O 3 Has a molar ratio of 4.8-5.8 and a bulk density of 0.55-0.75g/cm 3 Total specific surface area of 260-700m 2 And the modified molecular sieve is dried and subjected to silane coupling treatment.
Optionally, the antioxidant is at least one of an antioxidant 1076, an antioxidant 1010, an antioxidant 168 and an antioxidant 627, wherein the antioxidant 1076 is octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, the antioxidant 1010 is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], the antioxidant 168 is tris (2, 4-di-tert-butylphenyl) phosphite, and the antioxidant 627A is bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite.
Optionally, the lubricant is at least one of stearate, stearamide, stearate and silicone oil.
According to a second aspect of the present invention, there is provided a method of preparing the ASA composite of the present disclosure.
The preparation method of the ASA composite material comprises the following steps:
step (1): weighing SAN resin, ASA high-glue powder, a compatilizer, glass fiber, modified porous filler, an antioxidant and a lubricant according to a ratio;
step (2): stirring the raw materials for 3-10min, extruding the raw materials by a double-screw extruder, and then performing water-cooling granulation, wherein the temperature of the double-screw extruder is 260 ℃ for 220 plus materials, the rotating speed of the screw is 300-500 rpm, the double-screw extruder is divided into 8 temperature control areas from a feed inlet to an outlet, the temperature of each temperature control area is 230 ℃ for plus materials, 240 ℃ for plus materials, 260 ℃ for plus materials, 250 ℃ for plus materials, 230 ℃ for plus materials, and 240 ℃ for plus materials, and the rotating speed of the screw is 450rpm for plus materials.
The dielectric constant of the ASA composite material is lower than that of the conventional ASA material, the weather resistance and the impact toughness of the ASA composite material are both higher than those of the conventional ASA material, and the ASA composite material is suitable for preparing automotive millimeter wave radars.
Detailed Description
Various exemplary embodiments of the present invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.
In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
The ASA composite material provided by the disclosure comprises the following components in parts by weight:
the SAN resin is acrylonitrile-styrene copolymer polymerized by emulsion method or suspension method, and comprises 30-36% of acrylonitrile by mass percentage and weight average molecular weight M W 10-18 ten thousand;
the ASA high-glue powder is acrylonitrile-acrylate-styrene copolymer, wherein the content of acrylate-olefin rubber phase is 40-60%, the content of acrylonitrile is 11-15wt%, the average particle diameter is 100-1000nm, and the weight average molecular weight M W Is 12-50 ten thousand.
In one embodiment of the ASA composite of the present disclosure, the compatibilizer is at least one of an acrylonitrile-styrene-maleic anhydride terpolymer, a styrene-maleic anhydride bipolymer, an acrylonitrile-styrene grafted maleic anhydride, and a styrene grafted maleic anhydride.
Furthermore, the content of the maleic anhydride in the compatilizer is 1-20%.
In one embodiment of the ASA composite of the present disclosure, the glass fibers are modified cordierite-based glass fibers. The cordierite-based glass fiber has a main crystal form of cordierite and has a lower dielectric constant compared with the common E-type glass fiber.
Further, the content of the metal oxide in the modified cordierite-based glass fiber is as follows in percentage by mass:
SiO 2 40-45 percent of CaO, 5-15 percent of CaO, 10-20 percent of MgO and Al 2 O 3 12-15% of B 2 O 3 7-15% and Fe 2 O 3 Is 1-3%.
Further, the modification method of the modified cordierite-based glass fiber is as follows:
soaking cordierite-based glass fiber in anhydrous sulfuric acid for 0.5-1h, draining, washing with water, performing post-treatment in 5% ammonia gas atmosphere until the impregnation liquid of the glass fiber is neutral, and drying at 140 ℃ under 120-.
After the cordierite-based glass fiber is treated by anhydrous sulfuric acid, silicon hydroxyl on the surface of the glass fiber can be removed, so that the purpose of inhibiting the water absorption effect of the glass fiber is achieved, and the dielectric property of the composite material is more stable.
In one embodiment of the ASA composite of the present disclosure, the modified porous filler is a modified molecular sieve, the framework SiO of which is modified molecular sieve 2 /Al 2 O 3 The molar ratio of (A) is 4.8-5.8, and the bulk density is 0.55-0.75g/cm 3 Total specific surface area of 260-700m 2 And the modified molecular sieve is dried and subjected to silane coupling treatment. With SiO 2 /Al 2 O 3 Molecular sieves that are frameworks have a low dielectric constant. In addition, the molecular sieve has a porous structure, so that the dielectric constant and the dielectric loss of the composite material can be further reduced.
In one embodiment of the ASA composite of the present disclosure, the antioxidant is at least one of antioxidant 1076, antioxidant 1010, antioxidant 168 and antioxidant 627, wherein the antioxidant 1076 is octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, the antioxidant 1010 is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], the antioxidant 168 is tris (2, 4-di-tert-butylphenyl) phosphite, and the antioxidant 627A is bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite.
In one embodiment of the ASA composite of the present disclosure, the lubricant is at least one of a stearate, an amide stearate, a stearate, and a silicone oil.
The present disclosure also provides a preparation method of the ASA composite material, comprising the following steps:
step (1): weighing SAN resin, ASA high-glue powder, a compatilizer, glass fiber, modified porous filler, an antioxidant and a lubricant according to a proportion.
Step (2): stirring the raw materials for 3-10min, extruding the raw materials by a double-screw extruder, and then performing water-cooling granulation, wherein the temperature of the double-screw extruder is 260 ℃ for 220 plus materials, the rotating speed of the screw is 300-500 rpm, the double-screw extruder is divided into 8 temperature control areas from a feed inlet to an outlet, the temperature of each temperature control area is 230 ℃ for plus materials, 240 ℃ for plus materials, 260 ℃ for plus materials, 250 ℃ for plus materials, 230 ℃ for plus materials, and 240 ℃ for plus materials, and the rotating speed of the screw is 450rpm for plus materials.
The experimental procedures used in the examples below are conventional unless otherwise specified, the materials and reagents used therein are commercially available, and the equipment used in the experiments are well known to those skilled in the art without otherwise specified.
SAN resin is a product of Taiwan Chimei; the high glue powder is selected from Korea brocade lake petrochemical products; the antioxidant and the lubricant adopt commercial products.
The raw materials of examples 1-3 and comparative examples 1-3 were prepared according to the formulation in table 1, respectively, the raw materials were stirred for 3-10min until uniform, and the strands extruded by a twin-screw extruder were water-cooled and pelletized to obtain ASA composites. The specific temperature of each temperature control zone of the twin-screw extruder is 220 ℃, 230 ℃, 250 ℃, 240 ℃ and 230 ℃, and the screw rotating speed is 400 rpm.
TABLE 1
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| SAN resin (parts) | 42 | 50 | 32 | 25 | 34 | 37 |
| ASA high-gel powder (parts) | 30 | 28 | 27 | 30 | 35 | 28 |
| Modified cordierite-based glass fiber (part) | 22 | 15 | 30 | / | / | 30 |
| Ordinary glass fibre (share) | / | / | / | 30 | 25 | / |
| Compatilizer (parts) | 4 | 5 | 7 | 2 | 6 | / |
| Modified molecular sieve (fraction) | 3 | 2 | 4 | / | / | 5 |
| Antioxidant (in) | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.1 |
| Lubricant (portions) | 0.3 | 0.4 | 0.4 | 0.3 | 0.4 | 0.3 |
The products of the above examples and comparative examples were dried in a forced air oven at 80 ℃ for 4 hours and then injection molded into standard bars using a plastic injection molding machine. The injection molded bars were tested for performance after being left at 23 ℃ for at least 24 hours at 50% relative humidity. In addition, blow molding evaluations were carried out for each of the comparative examples and examples, and the overall level of material was evaluated by the surface quality of the article, the uniformity of wall thickness, and the stability of blow molding.
The product performance test method comprises the following steps:
the physical properties of the ASA particles are tested with reference to ISO527, ISO178 standard. The examples and comparative examples were evaluated by testing the ASA material in accordance with GB/T12636 for dielectric constant and dielectric loss at 30 GHz. The results of the performance tests on each sample are shown in table 2.
TABLE 2
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Tensile Strength (MPa) | 75 | 66 | 84 | 82 | 77 | 53 |
| Flexural Strength (MPa) | 102 | 95 | 110 | 108 | 103 | 84 |
| Dielectric constant | 2.78 | 2.85 | 2.83 | 3.23 | 3.35 | 3.06 |
| Dielectric loss | 0.0027 | 0.0025 | 0.0028 | 0.0067 | 0.0077 | 0.0045 |
As can be seen from table 2, the ASA composite material prepared according to the method of the present disclosure has a lower dielectric constant and dielectric loss, and has superior flexural strength.
Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.
Claims (6)
1. The ASA composite material is characterized by comprising the following components in parts by weight:
20-60 parts of SAN resin,
20-40 parts of ASA high-adhesive powder,
3-8 parts of a compatilizer,
5-30 parts of glass fiber,
0.5 to 5 portions of modified porous filler,
0.2 to 0.6 portion of antioxidant,
0.2-0.5 part of lubricant; wherein the content of the first and second substances,
the SAN resin is an acrylonitrile-styrene copolymer polymerized by an emulsion method or a suspension method, and comprises 30-36% of acrylonitrile by mass percent and a weight average molecular weight M W 10-18 ten thousand;
the ASA high-rubber powder is acrylonitrile-acrylate-styrene copolymer, wherein the content of acrylate rubber phase is 40-60%, the content of acrylonitrile is 11-15wt%, the average particle diameter is 100-1000nm, and the weight average molecular weight M W Is 12 to 50 ten thousand;
the glass fiber is modified cordierite-based glass fiber, and the content of metal oxide in the modified cordierite-based glass fiber is as follows in percentage by mass:
SiO 2 40-45 percent of CaO, 5-15 percent of CaO, 10-20 percent of MgO and Al 2 O 3 12-15% of B 2 O 3 7-15% and Fe 2 O 3 1 to 3 percent;
the modification method of the modified cordierite-based glass fiber comprises the following specific steps:
soaking cordierite-based glass fiber in anhydrous sulfuric acid for 0.5-1h, draining, washing with water, performing post-treatment in 5% ammonia gas atmosphere until the glass fiber impregnation solution is neutral, and drying at 140 ℃ under 120-;
the modified porous filler is a modified molecular sieve, and the skeleton SiO of the modified molecular sieve 2 /Al 2 O 3 Has a molar ratio of 4.8-5.8 and a bulk density of 0.55-0.75g/cm 3 Total specific surface area 260-700m 2 And the modified molecular sieve is dried and subjected to silane coupling treatment.
2. The ASA composite of claim 1, wherein the compatibilizer is at least one of an acrylonitrile-styrene-maleic anhydride terpolymer and a styrene-maleic anhydride terpolymer.
3. The ASA composite as claimed in claim 2, wherein the compatibilizer has a maleic anhydride content of 1-20%.
4. The ASA composite of claim 1, wherein the antioxidant is at least one of antioxidant 1076, antioxidant 1010, antioxidant 168, and antioxidant 626, wherein the antioxidant 1076 is octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, the antioxidant 1010 is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], the antioxidant 168 is tris (2, 4-di-tert-butylphenyl) phosphite, and the antioxidant 626 is bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite.
5. The ASA composite according to claim 1, wherein the lubricant is at least one of a stearate, a stearamide, a stearate and a silicone oil.
6. A method of preparing an ASA composite as claimed in any one of claims 1 to 5 comprising the steps of:
step (1): weighing SAN resin, ASA high-glue powder, a compatilizer, glass fiber, modified porous filler, an antioxidant and a lubricant according to a proportion;
step (2): stirring the raw materials for 3-10min, extruding the raw materials by a double-screw extruder, and then performing water-cooling granulation, wherein the temperature of the double-screw extruder is 260 ℃ for 220 plus materials, the rotating speed of the screw is 300-500 rpm, the double-screw extruder is divided into 8 temperature control areas from a feed inlet to an outlet, the temperature of each temperature control area is 230 ℃ for plus materials, 240 ℃ for plus materials, 260 ℃ for plus materials, 250 ℃ for plus materials, 230 ℃ for plus materials, and 240 ℃ for plus materials, and the rotating speed of the screw is 450rpm for plus materials.
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