CN112745615B - PMMA/ASA material and preparation method thereof - Google Patents
PMMA/ASA material and preparation method thereof Download PDFInfo
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- CN112745615B CN112745615B CN201911038759.8A CN201911038759A CN112745615B CN 112745615 B CN112745615 B CN 112745615B CN 201911038759 A CN201911038759 A CN 201911038759A CN 112745615 B CN112745615 B CN 112745615B
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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
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
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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
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a PMMA/ASA material and a preparation method thereof, wherein the PMMA/ASA material is prepared from 60-70 parts of polymethyl methacrylate, 25-35 parts of ASA high rubber powder, 5-10 parts of impact modifier, 0.5-1 part of brightening agent, 0.1-0.5 part of heat stabilizer, 0.1-0.5 part of lubricant and 0.5-2 parts of toner dye according to parts by weight, wherein the ASA rubber content of the ASA high rubber powder is more than or equal to 60% and the grain diameter is less than 350nm. According to the invention, the brightening agent is added into the PMMA/ASA material, so that a similar paint film effect is formed on the surface of the part, the brightness of the material is improved, and meanwhile, the anti-impact modifier is selected, so that the material has excellent low-temperature impact toughness.
Description
Technical Field
The invention belongs to the technical field of high polymer alloy materials, and particularly relates to a PMMA/ASA material and a preparation method thereof.
Background
Compared with the traditional ABS resin, the acrylonitrile-styrene-acrylate terpolymer (ASA) has the advantages that the introduced acrylate rubber without double bonds replaces butadiene rubber, so that the ABS resin can be comparable with the ABS resin in mechanical and processing properties, and in addition, the weather resistance is improved substantially, so that the ABS resin is more and more widely applied, and is especially applied to outdoor parts.
Polymethyl methacrylate (PMMA) has excellent light transmittance and good weather resistance, and after alloying with other resins, the weather resistance and the surface gloss are improved, but the impact toughness is unsatisfactory. PMMA/ASA alloy is a good material in industry in the future, and because of the excellent weather resistance and surface gloss, the conventional PMMA/ASA alloy can meet the parts with general appearance requirements, but the impact toughness of the alloy is reduced, and the conventional PMMA/ASA alloy can not meet the requirements on occasions with extremely high requirements on the black appearance brightness and higher requirements on the low-temperature impact toughness although the impact toughness of the PMMA/ASA alloy is higher than that of PMMA raw material resin, so that the application of the conventional PMMA/ASA alloy is limited.
Disclosure of Invention
Based on the above, the PMMA/ASA material provided by the invention solves the problem that the existing PMMA/ASA alloy material cannot meet the requirements of high blackness and brightness in appearance and low-temperature impact toughness at the same time, and the addition of the brightening agent to the PMMA/ASA material enables the part to form a paint film-like effect on the surface, so that the brightness of the material is improved, and meanwhile, the impact modifier is selected, so that the PMMA/ASA alloy material is excellent in low-temperature impact toughness.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the PMMA/ASA material is prepared from the following components in parts by weight:
the ASA glue content of the ASA high glue powder is more than or equal to 60 percent, and the grain diameter is less than 350nm. When the rubber powder content is increased, the impact resistance of the material is improved, but not any ASA with high rubber powder content can meet the final aim of the invention (achieve the effect of high blackness and brightness), so that the requirement of high blackness and brightness in appearance can be met on the basis of increasing the impact resistance only by selecting special rubber powder with small particle size (less than 350 nm).
Further, the impact modifier is AN AN/St grafted silicon-acrylic high weather resistant impact modifier. The AN/St grafted silicon-acrylic acid type high weather-resistant impact modifier has the characteristics of chemical resistance, good coloring lining and fluidity, and the physical properties of the silicon-containing toughening agent are beneficial to the low-temperature impact resistance of the material, and the low-temperature impact toughness of the material is obviously improved when the AN/St grafted silicon-acrylic acid type high weather-resistant impact modifier is added into a composite material.
Further, the brightening agent is polyvinyl acetate.
Further, the heat stabilizer is at least one selected from the group consisting of hindered amine heat stabilizers, hindered phenol heat stabilizers and triphenyl phosphite heat stabilizers.
Further, the lubricant is a silicone master batch taking AS AS a carrier.
Further, the toner dye is a compound of transparent red, transparent yellow and transparent blue. The three proportions are not limited in the invention, and it is understood that the person skilled in the art can adjust the proportion according to actual requirements, and compared with the black powder or the black master batch, the organic dye has stronger dyeing property, the blackness of the material is darker, and the hue is adjusted according to the requirements, so that the method is not only used for adjusting the single color of the black powder or the black master batch.
The invention also aims to provide a preparation method of the PMMA/ASA material, which comprises the following steps:
a. uniformly mixing polymethyl methacrylate, ASA high rubber powder, an impact modifier, a brightening agent, a heat stabilizer, a lubricant and a toner dye according to the weight portion ratio to obtain a mixed material;
b. and (3) feeding the mixed material into a double-screw extruder, and fully melting, compounding, extruding, bracing, cooling and granulating to obtain the PMMA/ASA material.
Further, the temperature of each section of screw rod of the double screw rod extruder is 220-250 ℃, and the rotating speed of the screw rod is 100-500 revolutions per minute.
Preferably, the temperature of each section of screw of the double-screw extruder is preferably 230-240 ℃, and the screw rotating speed is 400-500 revolutions per minute.
Compared with the prior art, the invention has the following beneficial effects:
conventionally, if PMMA is taken AS a main body, the impact toughness of the material is reduced, and the impact toughness of the material is ensured under the condition that the appearance of high blackness is not affected, in the invention, in order to ensure the appearance black brightness of the material, proper ASA rubber powder (namely, the particle size is less than 350 nm) is selected, meanwhile, a brightening agent is properly added, a silicone master batch with AS AS a carrier is used AS a lubricant, and a dye with high blackness is used; in addition, in order to ensure the impact toughness of the material, the invention selects rubber powder with the rubber content of more than 60 percent; a certain amount of silicon-containing impact modifier is used (to be controlled within a suitable range, otherwise affecting the appearance of the material). Thereby solving the problem of the decrease of impact toughness of PMMA as a main material. .
The PMMA/ASA material is prepared by adopting a double-screw extrusion process, and has the advantages of simple and continuous flow, high production efficiency and stable product quality.
The PMMA/ASA material of the invention has high black brightness and high glossiness in appearance.
The PMMA/ASA material disclosed by the invention simultaneously maintains good mechanical properties, is particularly beneficial to low-temperature impact toughness, and can be used for the product field with high requirements on appearance black brightness and low-temperature toughness.
Detailed Description
In order that the invention may be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments that are illustrated below. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
All materials in the embodiment of the invention are known commercial products, and the units of the materials are parts by weight and specifically comprise:
the PMMA resin is PMMA-CM211 of Taiwan Qimei;
ASA high rubber powder is A-960A of Keya;
the impact modifier is SX006 of Mitsubishi Li yang;
the brightening agent is polyvinyl acetate (commercially available);
the heat stabilizer is hindered phenol antioxidant 1076[ i.e. Irganox1076 beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate n-stearyl alcohol ester of CIBA ] and triphenyl phosphite antioxidant 168[ i.e. Irganox168 tris (2, 4-di-tert-butylphenyl) phosphite of CIBA ];
the lubricant is a Dow Corning MB50-008 silicone master batch;
the toner dye was transparent red, transparent yellow, and transparent blue (commercially available).
Example 1
60 parts of PMMA-CM211 resin, 35 parts of ASA high-rubber powder A-960A,5 parts of impact modifier SX006,0.5 part of brightening agent polyvinyl acetate, 0.5 part of photo-thermal stabilizer (1076:168=1:2, mass ratio) and 0.3 part of lubricant silicone master batch MB50-008 and 0.8 part of toner dye (transparent red: transparent yellow: transparent blue=1:1:1.5, mass ratio) are stirred and mixed uniformly at a high speed, and then are fed into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the high-black bright PMMA/ASA material with good low-temperature impact resistance is obtained by fully melting and compounding materials under the conveying and shearing actions of the screws of a double-screw extruder, extruding the materials through the machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Example 2
After mixing 65 parts of PMMA-CM211 resin, 25 parts of ASA high-glue powder A-960A,10 parts of impact modifier SX006,0.5 part of brightening agent polyvinyl acetate, 0.3 part of photo-thermal stabilizer (1076:168=1:2, mass ratio) and 0.2 part of lubricant silicone master batch MB50-008 and 1 part of toner dye (transparent red: transparent yellow: transparent blue=1:1:1.5, mass ratio) at high speed, feeding into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the high-black bright PMMA/ASA material with good low-temperature impact resistance is obtained by fully melting and compounding materials under the conveying and shearing actions of the screws of a double-screw extruder, extruding the materials through the machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Example 3
70 parts of PMMA-CM211 resin, 25 parts of ASA high-rubber powder A-960A,5 parts of impact modifier SX006,0.5 part of brightening agent polyvinyl acetate, 0.2 part of photo-thermal stabilizer (1076:168=1:2, mass ratio) and 0.5 part of lubricant silicone master batch MB50-008 and 2 parts of toner dye (transparent red: transparent yellow: transparent blue=2:1:1, mass ratio) are stirred and mixed uniformly at a high speed, and then are sent into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the high-black bright PMMA/ASA material with good low-temperature impact resistance is obtained by fully melting and compounding materials under the conveying and shearing actions of the screws of a double-screw extruder, extruding the materials through the machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Example 4
60 parts of PMMA-CM211 resin, 35 parts of ASA high-rubber powder A-960A,5 parts of impact modifier SX006,1 part of brightening agent polyvinyl acetate, 0.1 part of photo-thermal stabilizer (1076:168=1:2, mass ratio) and 0.2 part of lubricant silicone master batch MB50-008 and 0.5 part of toner dye (transparent red: transparent yellow: transparent blue=1:1:1.5, mass ratio) are stirred and mixed uniformly at a high speed, and then are fed into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the high-black bright PMMA/ASA material with good low-temperature impact resistance is obtained by fully melting and compounding materials under the conveying and shearing actions of the screws of a double-screw extruder, extruding the materials through the machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Example 5
65 parts of PMMA-CM211 resin, 25 parts of ASA high-rubber powder A-960A,10 parts of impact modifier SX006,1 part of brightening agent polyvinyl acetate, 0.4 part of photo-thermal stabilizer (1076:168=1:2, mass ratio) and 0.1 part of lubricant silicone master batch MB50-008 and 0.9 part of toner dye (transparent red: transparent yellow: transparent blue=1:1:1.5, mass ratio) are stirred and mixed uniformly at a high speed, and then are fed into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the high-black bright PMMA/ASA material with good low-temperature impact resistance is obtained by fully melting and compounding materials under the conveying and shearing actions of the screws of a double-screw extruder, extruding the materials through the machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Example 6
70 parts of PMMA-CM211 resin, 25 parts of ASA high-glue powder A-960A,5 parts of impact modifier SX006,1 part of brightening agent polyvinyl acetate, 0.2 part of photo-thermal stabilizer (1076:168=1:2, mass ratio) and 0.2 part of lubricant silicone master batch MB50-008 and 1 part of toner dye (transparent red: transparent yellow: transparent blue=2:1:1, mass ratio) are stirred and mixed uniformly at a high speed, and then are sent into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the high-black bright PMMA/ASA material with good low-temperature impact resistance is obtained by fully melting and compounding materials under the conveying and shearing actions of the screws of a double-screw extruder, extruding the materials through the machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Comparative example 1
60 parts of PMMA-CM211 resin, 35 parts of ASA high-strength rubber powder XC-500 (rubber powder content is 50-52%), 5 parts of impact modifier SX006,0.5 part of brightening agent polyvinyl acetate, 0.5 part of photo-thermal stabilizer (1076:168=1:2, mass ratio), 0.3 part of lubricant silicone master batch MB50-008 and 0.8 part of toner dye (transparent red: transparent yellow: transparent blue=1:1:1.5, mass ratio) are stirred and mixed uniformly at a high speed, and then fed into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the PMMA/ASA material is obtained by fully melting and compounding materials under the conveying and shearing actions of a screw of a double-screw extruder, extruding by a machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Comparative example 2
65 parts of PMMA-CM211 resin, 25 parts of ASA high-glue powder A-960A,10 parts of MBS toughening agent, 0.5 part of brightening agent polyvinyl acetate, 0.3 part of photo-thermal stabilizer (1076:168=1:2, mass ratio) and 0.2 part of lubricant silicone master batch MB50-008 and 1 part of toner dye (transparent red: transparent yellow: transparent blue=1:1:1.5, mass ratio) are stirred and mixed uniformly at a high speed, and then are sent into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the PMMA/ASA material is obtained by fully melting and compounding materials under the conveying and shearing actions of a screw of a double-screw extruder, extruding by a machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Comparative example 3
After mixing 60 parts of PMMA-CM211 resin, 35 parts of ASA high-strength rubber powder A-960A,5 parts of impact modifier SX006,0.1 part of photo-thermal stabilizer (1076:168=1:2 by mass ratio), 0.2 part of lubricant A-C540A (ethylene acrylic acid copolymer) and 0.5 part of toner dye (transparent red: transparent yellow: transparent blue=1:1:1.5 by mass ratio) at a high speed, feeding into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the PMMA/ASA material is obtained by fully melting and compounding materials under the conveying and shearing actions of a screw of a double-screw extruder, extruding by a machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
Comparative example 4
65 parts of PMMA-CM211 resin, 25 parts of ASA high-glue powder A-960A,10 parts of impact modifier SX006,1 part of brightening agent polyvinyl acetate, 0.4 part of photo-thermal stabilizer (1076:168=1:2, mass ratio) and 0.1 part of lubricant silicone master batch MB50-008 and 10 parts of black master batch-2014 (cabot) are stirred and mixed uniformly at a high speed, and then are sent into a double-screw extruder, wherein the working temperatures of each section of the double-screw extruder are as follows: the high-black bright PMMA/ASA material with good low-temperature impact resistance is obtained by fully melting and compounding materials under the conveying and shearing actions of the screws of a double-screw extruder, extruding the materials through the machine head, bracing, cooling and granulating.
The prepared PMMA/ASA material is injection molded into standard sample bars for testing according to standard sizes, and is tested according to the physical property testing standard of the table 1, and the performance testing results are shown in the table 2.
TABLE 1
TABLE 2
TABLE 3 Table 3
As can be seen from tables 2 and 3, by properly controlling the proportion adjustment and selection of the components (the silicone master batch of AS carrier is adopted AS the lubricant), not only has the effects of lubrication and apparent brightening, but also has good compatibility with matrix resin, other lubricants can have lubricating effect, but have relatively poor compatibility, the product surface is easy to generate a hazing phenomenon under the condition of high-temperature injection molding, compared with the traditional black master batch and the like, the black dyeing power of the toner dye is greatly enhanced, the blackening effect is greatly improved visually, the blackness value (L value) is also greatly reduced, the AN/St grafted silicon-acrylic acid impact modifier is selected AS the toughening agent, the compatibility with matrix material is good, the low-temperature impact resistance of the material is greatly improved, the polyvinyl acetate can be separated out to the surface of the product in the molding process, the polyvinyl acetate is similar to the surface of the product, the product is increased in brightness of the product compared with the existing black PMMA/ASA material, the toughness is maintained in the aspect of the mechanical property of the material, the low-temperature impact resistance is higher, the low-temperature impact resistance is better, the product has good brightness, and can meet the requirements of high-temperature impact resistance and high-brightness requirements on the actual conditions, and can meet the high-temperature requirements and high-grade and black impact.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (7)
1. The PMMA/ASA material is characterized by being prepared from the following components in parts by weight:
60 to 70 parts of polymethyl methacrylate,
25 to 35 parts of ASA high rubber powder,
5-10 parts of impact modifier,
0.5-1 part of brightening agent,
0.1 to 0.5 part of heat stabilizer,
0.1 to 0.5 part of lubricant,
0.5-2 parts of toner dye;
the ASA glue content of the ASA high glue powder is more than or equal to 60 percent, and the grain diameter is less than 350nm; the impact modifier is AN AN/St grafted silicon-acrylic acid type high weather-resistant impact modifier; the brightening agent is polyvinyl acetate.
2. The PMMA/ASA material of claim 1 wherein the heat stabilizer is selected from at least one of a hindered amine heat stabilizer, a hindered phenol heat stabilizer and a triphenyl phosphite heat stabilizer.
3. A PMMA/ASA material according to claim 1 wherein the lubricant is a silicone masterbatch with AS carrier.
4. The PMMA/ASA material according to claim 1, wherein the toner dye is a combination of transparent red, transparent yellow and transparent blue.
5. A method for preparing a PMMA/ASA material according to any one of claims 1 to 4, comprising the steps of:
a. uniformly mixing polymethyl methacrylate, ASA high rubber powder, an impact modifier, a brightening agent, a heat stabilizer, a lubricant and a toner dye according to the weight portion ratio to obtain a mixed material;
b. and (3) feeding the mixed material into a double-screw extruder, and fully melting, compounding, extruding, bracing, cooling and granulating to obtain the PMMA/ASA material.
6. The method according to claim 5, wherein the temperature of each section of screw of the twin-screw extruder is 220-250 ℃ and the rotational speed of the screw is 100-500 rpm.
7. The method according to claim 6, wherein the temperature of each section of screw of the twin-screw extruder is preferably 230-240 ℃ and the screw rotation speed is 400-500 rpm.
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