CN115572449B - Ultraviolet-resistant high-toughness PMMA (polymethyl methacrylate) composition and preparation method and application thereof - Google Patents
Ultraviolet-resistant high-toughness PMMA (polymethyl methacrylate) composition and preparation method and application thereof Download PDFInfo
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2207/53—Core-shell polymer
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Abstract
The invention discloses an ultraviolet-resistant high-toughness PMMA composition, and a preparation method and application thereof. The PMMA composition provided by the invention comprises the following components in parts by weight: 75-85 parts of PMMA resin, 15-25 parts of toughening agent, 0.1-0.5 part of toughening synergist, 0.5-3 parts of ultraviolet blocking agent, 0-0.5 part of antioxidant and 0-1 part of lubricant; the toughening agent is a toughening agent with methyl methacrylate as a shell and organic silicon and acrylic ester as cores, and the core content is more than or equal to 30 wt%; the toughening synergist is nano silicon dioxide; the ultraviolet blocking agent is nano barium sulfate and/or nano titanium dioxide. The toughness of the material is effectively improved by selecting a specific type of toughening agent and cooperating with nano silicon dioxide, and meanwhile, the toughness of the material is further improved by selecting a specific type of ultraviolet blocking agent, so that the weather resistance of the material is improved, and the toughening agent and the toughening system cooperate.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to an ultraviolet-resistant and high-toughness PMMA composition, and a preparation method and application thereof.
Background
With the diversification development of market demands, the LED industry has a new bright point, wherein the market of ultraviolet germicidal lamps is rapidly rising. The ultraviolet sterilizing lamp adopts UVC LED to sterilize, and can prevent some germs from spreading through air or spreading through the surface of objects in public places such as hospitals, schools, houses, movie theatres, buses, offices and the like. In addition, UVC LEDs are also increasingly used in small-sized appliances involving air and water disinfection treatments, such as humidifiers, air conditioners, pet water feeders, and the like.
However, conventional electrical housing materials such as ABS, PC/ABS, ASA materials are inferior in weatherability and are extremely prone to color differences under the action of short wavelength uv light. PMMA material is one of materials with better weather resistance in thermoplastic materials, and still has difficulty in meeting the high weather resistance requirement of short wave ultraviolet resistance. In addition, PMMA material has poor notch impact strength, and cannot meet the requirements of complex product structures or assembly procedures such as screw driving and the like (generally, the notch impact strength is more than or equal to 5.5 KJ/m) 2 )。
Therefore, there is a need to develop a PMMA composition that is more uv resistant and has high toughness.
Disclosure of Invention
The invention provides a PMMA composition with ultraviolet resistance and high toughness, which overcomes the defects of poor weather resistance and poor toughness in the prior art, and the toughening system formed by selecting a toughening agent with methyl methacrylate as a shell, organic silicon and acrylic ester as cores and cooperating with nano silicon dioxide as a toughening synergist effectively improves the toughness of PMMA materials, and meanwhile, selects a specific type of ultraviolet blocking agent, so that the weather resistance of the materials is improved, and the toughness of the materials is further improved by cooperating with the toughening system.
Another object of the present invention is to provide a method for preparing the above PMMA composition.
It is a further object of the present invention to provide the use of the above PMMA composition.
In order to solve the technical problems, the invention adopts the following technical scheme:
a PMMA composition with ultraviolet resistance and high toughness comprises the following components in parts by weight:
75-85 parts of PMMA resin,
15-25 parts of toughening agent,
0.1 to 0.5 part of toughening synergist,
0.5 to 3 parts of ultraviolet blocking agent,
0 to 0.5 part of antioxidant,
0-1 part of lubricant;
the toughening agent is a toughening agent taking methyl methacrylate as a shell and an organosilicon-acrylate copolymer as a core, wherein the content of the organosilicon-acrylate copolymer is more than or equal to 30wt.%;
the toughening synergist is nano silicon dioxide;
the ultraviolet blocking agent is nano barium sulfate and/or nano titanium dioxide.
The invention adopts the core-shell type toughening agent, the toughening agent takes methyl methacrylate as a shell and takes the organosilicon-acrylic ester copolymer as a core, and the toughening agent has good compatibility with PMMA resin, and can be uniformly dispersed in a PMMA system. Wherein, the organic silicon has a flexible and thermally stable-Si-O-bond, which can form a plurality of obvious hollows in the PMMA matrix. The inventor researches and discovers that acrylic ester 'pellets' exist in the cavities, and the pellets are uniformly dispersed and uniformly sized to form a 'core' in a core-shell structure. When the external force acts, the core of the toughening agent serves as a stress concentration point, absorbs energy and dissipates energy, plays roles in generating silver marks and blocking further development of cracks, and improves the toughness of the material. In addition, the core-shell type toughening agent does not contain carbon-carbon double bonds, and yellowing is not easy to occur due to the fact that the carbon-carbon double bonds are broken when UVC is irradiated.
In the PMMA composition of the invention, the core content in the toughening agent cannot be too low, and in the case that the core content is less than 30wt.%, an effective toughening effect cannot be achieved.
Preferably, the content of the organosilicon and the acrylic ester in the toughening agent is 35 to 50wt.%.
According to the invention, the nano silicon dioxide is used as a toughening synergist, and can play a certain role in filling in a core-shell structure, so that the structural stability of the toughening agent is further enhanced and stabilized, namely, the nano silicon dioxide can play a role in synergistic toughening, and the toughness of the PMMA composition is further improved.
The nano barium sulfate and/or nano titanium dioxide serving as inorganic materials can play a role in absorbing and blocking ultraviolet rays, so that negative influence of the ultraviolet rays on the PMMA composition is reduced to a certain extent, and meanwhile, the nano barium sulfate and the nano titanium dioxide can play a role in nucleating to further strengthen a toughening system and form a synergistic effect.
Preferably, the average particle size of the nano silicon dioxide is less than or equal to 16nm.
More preferably, the nanosilica has an average particle size of 7 to 12nm.
The average particle size of the nano-silica should be in a proper range, and when the average particle size of the nano-silica is large, the nano-silica has limited synergistic effect with the organosilicon-acrylate copolymer component in the toughening agent, so that the toughness of the PMMA composition is difficult to improve in a synergistic manner, and the nucleation toughening effect of the toughening agent can be damaged.
Preferably, the average particle size of the ultraviolet blocking agent is less than or equal to 100nm.
More preferably, the ultraviolet blocking agent has an average particle diameter of 20 to 60nm.
When the particle size of the ultraviolet blocking agent is too large, the scattering effect on ultraviolet rays is reduced, and the toughness of the material is affected, resulting in reduced toughness.
Preferably, the ultraviolet blocking agent is a mixture of nano barium sulfate and nano titanium dioxide according to the mass ratio of 1:1-9.
The nano barium sulfate and the nano titanium dioxide are of spherical structures, and have little influence on the mechanical properties of the material. Meanwhile, the particle size is small, the activity is large, ultraviolet rays can be reflected and scattered, and can be absorbed, so that the ultraviolet rays are more resistant to blocking, and the composite performance of the ultraviolet rays is far better than that of filling powder with a sheet-shaped structure. The chemical and physical stability of the ultraviolet blocking agent adopted by the invention is far better than that of an organic ultraviolet absorbent and is also better than that of other inorganic nano particles, such as nano calcium carbonate, nano zinc oxide and the like. Meanwhile, the nano titanium dioxide also has the coloring capability and good color surface covering power.
In addition, the inventor researches and discovers that although the weather resistance of materials can be improved by common organic weather-proofing agents (such as hindered amine light stabilizers and benzotriazole ultraviolet light absorbers) in the market, the materials can only work at a wavelength of more than 280nm and can easily lose the efficacy under UV-C irradiation.
Preferably, the PMMA resin has a melt flow rate of 2-8 g/10min at 230 ℃ and 3.8 kg.
Melt flow rates were tested according to the ISO 1133-2011 standard method.
Optionally, the antioxidant is one or more of hindered phenols, phosphites and thio antioxidants.
Preferably, the lubricant is a PETS-type lubricant.
The PETS lubricant has the effect of high temperature resistance, so that the PMMA composition provided by the invention has better weather resistance.
The invention also provides a preparation method of the ultraviolet-resistant high-toughness PMMA composition, which comprises the following steps:
mixing PMMA resin, a toughening agent, a toughening synergist, an ultraviolet blocking agent, a lubricant and an antioxidant, adding the mixture into an extruder, and carrying out melt mixing, extrusion and granulation to obtain the ultraviolet-resistant and high-toughness PMMA composition.
Preferably, the extruder is a double-screw extruder, the temperature of the machine head is 210-230 ℃, and the temperature of the machine body screw cylinder is 220-230 ℃.
The invention also protects the application of the ultraviolet-resistant and high-toughness PMMA composition in preparing humidifiers, air-conditioning shells and pet water feeders.
Compared with the prior art, the invention has the beneficial effects that:
the invention develops a PMMA composition with ultraviolet resistance and high toughness, which adopts methyl methacrylate as a shell, organic silicon and acrylic ester as a core as a toughening agent, and cooperates with nano silicon dioxide as a toughening synergist, so that the toughness of PMMA material is effectively improved by a formed toughening system, and meanwhile, the toughness of the material is further improved by the synergistic effect of the toughening system by selecting a specific type of ultraviolet blocking agent, so that the weather resistance of the material is improved.
Detailed Description
The invention is further described below in connection with the following detailed description.
The raw materials in examples and comparative examples are all commercially available;
PMMA resin-1, taiwan Qimei CM-205, has a melt flow rate of 2g/CM at 230 ℃ and 3.8kg 3 ；
PMMA resin-2, taiwan Qimei CM-207, has a melt flow rate of 8g/CM at 230℃and 3.8kg 3 ；
Toughening agent-1, mitsubishi yang of Japan, S-2030, methyl methacrylate as shell, organosilicon-acrylate copolymer as core, core content of 30wt.%;
toughening agent-2, winzhou LongOu plastic technology, SL-1050, methyl methacrylate as a shell, and organosilicon-acrylate copolymer as a core, wherein the core content is 50wt.%;
toughening agent-3, new Shenzhen Pasteur material, S203, methyl methacrylate as shell, organosilicon-acrylic ester copolymer as core, core content 35wt.%;
toughening synergist-1, yingzhangchuanggusa, R974, nano silicon dioxide with an average particle size of 12nm;
toughening synergist-2, yingzhangchuanggusa, R974, nano silicon dioxide with an average particle size of 16nm;
toughening synergist-3, japanese Deshan, QS-40, nano silicon dioxide with average particle size of 7nm;
ultraviolet blocking agent-1, dekkaido island gold, nanometer barium sulfate, average particle diameter of 60nm;
ultraviolet blocking agent-2, well Jin Yan, nanometer barium sulfate, average particle size 50nm;
ultraviolet blocking agent-3, yingzhangyu Degusa, AEROXIDE P25, nanometer titanium dioxide, average particle diameter 21nm;
ultraviolet blocking agent-4, zhejiang Zhi Tai nanometer, VK-T25Q, nanometer titanium dioxide, average grain diameter is 30nm;
antioxidants, antioxidant 168, commercially available;
lubricants, PETS-type lubricants, commercially available.
Toughening agent-4, winzhou LongOu plastic technology, SL-1020, methyl methacrylate as a shell, and organosilicon-acrylate copolymer as a core, wherein the core content is 20 wt%;
ACR, commercially available, acrylate tougheners;
MBS, commercially available, methyl methacrylate butadiene styrene toughening agents;
nano zinc oxide with an average particle size of 30nm, which is commercially available;
ultraviolet absorber, UV-531, commercially available;
unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Examples 1 to 17
Examples 1 to 17 each provide a PMMA composition, the component contents are shown in Table 1, and the preparation method is as follows:
all the components were mixed according to table 1 and fed into a twin screw extruder at a head temperature of 215 ℃ and a body screw temperature of 225 ℃ and melt-mixed and extrusion-pelletized to obtain a PMMA composition.
TABLE 1 component content (parts by weight) of PMMA compositions of examples 1 to 17
Comparative examples 1 to 7
Comparative examples 1 to 7 each provided a PMMA composition, the component contents are shown in Table 2, and the preparation method is as follows:
all the components were mixed according to table 2 and fed into a twin screw extruder at a head temperature of 215 ℃ and a body screw temperature of 225 ℃ and melt-mixed and extrusion pelletized to obtain a PMMA composition.
TABLE 2 comparative examples 1 to 7 component contents (parts by weight) of PMMA compositions
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | |
| PMMA resin-1 | 80 | 80 | 80 | 80 | 80 | 80 | 80 |
| Toughening agent-1 | / | / | / | 20 | 20 | 20 | 20 |
| Toughening agent-4 | 20 | / | / | / | / | / | / |
| ACR | / | 20 | / | / | / | / | / |
| MBS | / | / | 20 | / | / | / | / |
| Toughening synergist-1 | 0.3 | 0.3 | 0.3 | / | 0.3 | 0.3 | 0.3 |
| Ultraviolet blocking agent-1 | 1 | 1 | 1 | 1 | / | / | / |
| Ultraviolet absorber | / | / | / | / | / | 1 | / |
| Nano zinc oxide | / | / | / | / | / | / | 1 |
| Antioxidant | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
| Lubricant | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 |
Performance testing
The PMMA compositions prepared in the above examples and comparative examples were subjected to performance testing by the following methods:
notched Izod impact Strength: according to ISO 180-2000 test standard, the test conditions are 23 ℃ and 2mm injection notch;
ultraviolet ray resistance color difference: the PMMA test panels of the PMMA injection molded compositions were irradiated at a vertical distance of 10cm using UVC-LED disinfection lamps (30W, 254nm wavelength) for 40 hours, and color differences before and after UVC-LED irradiation were measured by CIE 1976 Lxab.
The test results of the examples are shown in Table 3, and the test results of the comparative examples are shown in Table 4.
Table 3 test results of examples
Table 4 test results of comparative examples
According to the test results of Table 3, PMMA compositions prepared in each example of the present invention have high toughness, and Izod notched impact strength of 5.6KJ/m or more 2 The ultraviolet ray resistance color difference is less than or equal to 2.0.
From examples 1 to 3, the PMMA material can be well toughened by adopting the toughening agent with methyl methacrylate as a shell and an organosilicon-acrylate copolymer as a core, and the core content is more than or equal to 30 wt%, and the PMMA composition has higher core contentThe better the toughness of the product. The toughening agent used in comparative example 1 was also a toughening agent with methyl methacrylate as the shell and an organosilicon-acrylate copolymer as the core, but the core content was too low, and the notched Izod impact strength of the PMMA composition was 5.4KJ/m 2 The requirement of complex product structure or assembly procedures such as screw driving and the like cannot be met. The toughening agents used in comparative examples 2 and 3 are toughening agents with non-core-shell structures, specifically ACR and MBS, and although the toughness of the PMMA composition can be improved to a certain extent, the ultraviolet resistance of the PMMA composition is very poor, and the color difference of the PMMA composition reaches 4.76 and 7.88 through a UVC-LED disinfection lamp.
According to the embodiment 1, the embodiment 4 and the embodiment 5, the average grain diameter of the nano silicon dioxide is less than or equal to 16nm, the nano silicon dioxide can have good synergistic effect with the toughening agent of the core-shell structure, and when the average grain diameter of the nano silicon dioxide is 7-12 nm, the synergistic effect with the toughening agent is better, and the toughness of the prepared PMMA composition is higher. Whereas comparative example 4 does not contain a toughening synergist, the PMMA composition has poorer system toughness.
Examples 1 and 6 to 13 use nano barium sulfate and nano titanium dioxide as ultraviolet blocking agents, so that ultraviolet resistance of the PMMA composition can be improved, and chromatic aberration after ultraviolet irradiation can be reduced. In contrast, comparative example 5 does not contain an ultraviolet blocking agent, comparative example 6 uses an organic ultraviolet absorber instead of the ultraviolet blocking agent of the present invention, and comparative example 7 uses nano zinc oxide instead of the ultraviolet blocking agent of the present invention, and thus good ultraviolet resistance cannot be achieved.
The ultraviolet blocking agent adopted in examples 10 to 13 is a mixture of nano barium sulfate and nano titanium dioxide, and it can be seen that lower ultraviolet chromatic aberration resistance can be realized by adopting the compound ultraviolet blocking agent compared with examples 1 and 6 to 8.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (8)
1. The ultraviolet-resistant high-toughness PMMA composition is characterized by comprising the following components in parts by weight:
75-85 parts of PMMA resin,
15-25 parts of a toughening agent,
0.1 to 0.5 part of toughening synergist,
0.5-3 parts of ultraviolet blocking agent,
0 to 0.5 part of an antioxidant,
0-1 parts of a lubricant;
the toughening agent is a toughening agent taking methyl methacrylate as a shell and an organosilicon-acrylate copolymer as a core, wherein the content of the organosilicon-acrylate copolymer is more than or equal to 30wt.%;
the toughening synergist is nano silicon dioxide, and the average particle size of the nano silicon dioxide is less than or equal to 16nm;
the ultraviolet blocking agent is nano barium sulfate and/or nano titanium dioxide, and the average particle size of the ultraviolet blocking agent is less than or equal to 100nm.
2. The ultraviolet-resistant high-toughness PMMA composition according to claim 1, wherein the average particle size of the nanosilica is 7-12 nm.
3. The ultraviolet-resistant high-toughness PMMA composition according to claim 1, wherein the ultraviolet blocking agent is a mixture of nano barium sulfate and nano titanium dioxide in a mass ratio of 1:1-9.
4. The ultraviolet light resistant, high toughness PMMA composition of claim 1, wherein the silicone-acrylate copolymer content of the toughening agent is 35 to 50 wt%.
5. The ultraviolet light resistant and high toughness PMMA composition according to claim 1, wherein the PMMA resin has a melt flow rate of 2-8 g/10min at 230 ℃ and 3.8 kg.
6. The method for preparing the ultraviolet light resistant and high-toughness PMMA composition according to any one of claims 1 to 5, which is characterized by comprising the following steps:
mixing PMMA resin, a toughening agent, a toughening synergist, an ultraviolet blocking agent, a lubricant and an antioxidant, adding the mixture into an extruder, and carrying out melt mixing, extrusion and granulation to obtain the ultraviolet-resistant and high-toughness PMMA composition.
7. The method according to claim 6, wherein the extruder is a twin screw extruder, the temperature of the head is 210-230 ℃, and the temperature of the barrel of the extruder is 220-230 ℃.
8. The use of the ultraviolet light resistant, high toughness PMMA composition of any one of claims 1 to 5 in the preparation of humidifiers, air conditioning housings, pet water feeders.
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| CN202211213773.9A CN115572449B (en) | 2022-09-30 | 2022-09-30 | Ultraviolet-resistant high-toughness PMMA (polymethyl methacrylate) composition and preparation method and application thereof |
| PCT/CN2023/120979 WO2024067453A1 (en) | 2022-09-30 | 2023-09-25 | Ultraviolet-resistant, highly tough pmma composition, preparation method therefor, and use thereof |
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| CN107189301A (en) * | 2017-05-25 | 2017-09-22 | 广东圆融新材料有限公司 | A kind of weather-proof PMMA AS plastic alloys and preparation method thereof |
| CN109517311A (en) * | 2018-11-20 | 2019-03-26 | 安徽江淮汽车集团股份有限公司 | A kind of PMMA composite material and preparation method |
| CN112724566A (en) * | 2020-12-15 | 2021-04-30 | 金发科技股份有限公司 | PMMA material and preparation method and application thereof |
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| WO2024067453A1 (en) | 2024-04-04 |
| CN115572449A (en) | 2023-01-06 |
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