CN115572449A - Ultraviolet-resistant and high-toughness PMMA (polymethyl methacrylate) composition as well as preparation method and application thereof - Google Patents
Ultraviolet-resistant and high-toughness PMMA (polymethyl methacrylate) composition as well as 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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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention discloses a PMMA composition with ultraviolet resistance and high toughness as well as a preparation method and application thereof. The PMMA composition comprises the following components in parts by weight: 75 to 85 parts of PMMA resin, 15 to 25 parts of toughening agent, 0.1 to 0.5 part of toughening synergistic agent, 0.5 to 3 parts of ultraviolet blocking agent, 0 to 0.5 part of antioxidant and 0 to 1 part of lubricant; the toughening agent is a toughening agent taking methyl methacrylate as a shell and organic silicon and acrylic ester as cores, and the core content 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 specific type of toughening agent is selected to cooperate with the nano silicon dioxide to form a toughening system, so that the toughness of the material is effectively improved, and meanwhile, the specific type of ultraviolet blocking agent is selected to improve the weather resistance of the material and further improve the toughness of the material under the synergistic action of the ultraviolet blocking agent and the toughening system.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a PMMA composition with ultraviolet resistance and high toughness as well as a preparation method and application thereof.
Background
With the diversified development of market demands, new bright spots appear in the LED industry, wherein the market of ultraviolet germicidal lamps rapidly rises. The ultraviolet germicidal lamp adopts UVC LED for disinfection, and can prevent some germs from being transmitted through air or transmitted through the surface of an object by virtue of UVC LED disinfection in public places such as hospitals, schools, nursery houses, cinemas, buses and offices. Further, UVC LEDs are increasingly used in small electric appliances such as humidifiers, air conditioners, pet water feeders, etc., which are used for air and water sterilization.
However, the traditional electrical appliance shell materials such as ABS, PC/ABS and ASA materials have poor weather resistance, and color difference is easy to occur under the action of short-wavelength ultraviolet rays. The PMMA material is one of materials with better weather resistance in thermoplastic materials, and the high weather resistance requirement of short-wave ultraviolet resistance is still difficult to meet. In addition, the PMMA material has poor notch impact strength, and cannot meet the requirements of complex workpiece structures or assembling procedures such as screwing and the like (generally, the notch impact strength is required to be more than or equal to 5.5KJ/m 2 )。
Therefore, there is a need to develop a PMMA composition having more resistance to ultraviolet rays and high toughness.
Disclosure of Invention
The invention provides the ultraviolet-resistant and high-toughness PMMA composition for overcoming the defects of poor weather resistance and poor toughness in the prior art, a toughening agent taking methyl methacrylate as a shell and organic silicon and acrylic ester as cores is selected to be cooperated with nano silicon dioxide as a toughening synergist, so that the toughness of a PMMA material is effectively improved by a formed toughening system, and meanwhile, a specific type of ultraviolet blocking agent is selected, so that the weather resistance of the material is improved, and the material toughness is further improved by the synergistic effect of the ultraviolet blocking agent and the toughening system.
Another object of the present invention is to provide a method for preparing the above PMMA composition.
Another object of the present invention is to provide the use of the PMMA composition described above.
In order to solve the technical problems, the invention adopts the technical scheme that:
the UV-resistant and high-toughness PMMA composition comprises the following components in parts by weight:
75 to 85 portions of PMMA resin,
15-25 parts of a toughening agent,
0.1 to 0.5 portion of toughening synergist,
0.5 to 3 portions of ultraviolet blocking agent,
0 to 0.5 portion of antioxidant,
0-1 part of a lubricant;
the toughening agent is a toughening agent taking methyl methacrylate as a shell and taking an organic silicon-acrylate copolymer as a core, wherein the content of the organic silicon-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 organic silicon-acrylate copolymer as a core, the toughening agent has good compatibility with PMMA resin, and the toughening agent can be uniformly dispersed in a PMMA system. Wherein, organosilicon has-Si-O-bond with flexibility and good thermal stability, and can form a plurality of obvious cavities in PMMA matrix. The inventors have found that acrylic ester "beads" are present in these voids, and the beads are uniformly dispersed and have a uniform size, forming a "core" in the core-shell structure. When the toughening agent is acted by external force, the core of the toughening agent is used as a stress concentration point to absorb energy and dissipate energy, and plays roles in generating silver lines and blocking further development of cracks, thereby improving the toughness of the material. In addition, the core-shell type toughening agent does not contain carbon-carbon double bonds, and the core-shell type toughening agent is not easy to cause yellowing due to the breakage of the carbon-carbon double bonds when subjected to UVC irradiation.
In the PMMA composition of the invention, the content of the core in the toughening agent cannot be too low, and the effective toughening effect cannot be achieved under the condition that the content of the core is less than 30 wt.%.
Preferably, the content of the organosilicon and the acrylate in the toughening agent is 35 to 50wt.%.
The nano silicon dioxide is used as the toughening synergist, and the nano silicon dioxide can play a certain filling role 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 synergistic toughening effect, and the toughness of the PMMA composition is further improved.
The nano barium sulfate and/or nano titanium dioxide are used as inorganic materials, can play a role in absorbing and blocking ultraviolet rays, reduce the negative effect of the ultraviolet rays on the PMMA composition to a certain extent, and simultaneously can play a role in nucleating the nano barium sulfate and the nano titanium dioxide to further reinforce a toughening system to form a synergistic effect.
Preferably, the average particle size of the nano silicon dioxide is less than or equal to 16nm.
More preferably, the average particle size of the nano silica is 7 to 12nm.
The average particle size of the nano-silica is in a proper range, and when the average particle size of the nano-silica is larger, the synergistic effect of the nano-silica and the organosilicon-acrylate copolymer component in the toughening agent is limited, so that the toughness of the PMMA composition is difficult to be improved in a synergistic manner, and the nucleation and toughening effect of the toughening agent can be damaged.
Preferably, the average particle size of the ultraviolet blocker 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 uv blocking agent is too large, its scattering effect on uv rays is reduced, and the toughness of the material is affected, resulting in a reduction in 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 both spherical structures, and have little influence on the mechanical properties of the material. Meanwhile, the filler powder has small particle size and high activity, can reflect and scatter ultraviolet rays and absorb the ultraviolet rays, thereby having stronger barrier capability to the ultraviolet rays, and the comprehensive performance of the filler powder is far superior to that of filler powder with a sheet 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 the materials can be improved by using the commonly used organic weather resisting agents (such as hindered amine light stabilizers and benzotriazole ultraviolet absorbers), the organic weather resisting agents only can act on the wavelength of more than 280nm and easily lose the efficacy under the irradiation of UV-C.
Preferably, the PMMA resin has the melt flow rate of 2 to 8g/10min under the conditions of 230 ℃ and 3.8 kg.
The melt flow rate was measured according to 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-based lubricant.
The PETS lubricant has the effect of high temperature resistance, so that the PMMA composition disclosed by the invention has better weather resistance.
The invention also provides a preparation method of the PMMA composition with ultraviolet resistance and high toughness, 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 performing 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 a nose is 210-230 ℃, and the temperature of a screw barrel of a machine body is 220-230 ℃.
The invention also protects the application of the PMMA composition with ultraviolet resistance and high toughness in preparing humidifiers, air-conditioning shells and water feeders for pets.
Compared with the prior art, the invention has the beneficial effects that:
the invention develops an ultraviolet-resistant high-toughness PMMA composition, a toughening agent taking methyl methacrylate as a shell and organic silicon and acrylic ester as cores is selected to cooperate with nano silicon dioxide as a toughening synergist, so that a formed toughening system effectively improves the toughness of a PMMA material, and meanwhile, a specific type of ultraviolet blocking agent is selected to improve the weather resistance of the material and further improve the toughness of the material under the synergistic action of the ultraviolet blocking agent and the toughening system.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The raw materials in the examples and comparative examples are commercially available;
PMMA resin-1, chimei CM-205, taiwan, melt flow rate of 2g/CM at 230 deg.C and 3.8kg 3 ；
PMMA resin-2, chimei CM-207, taiwan, melt flow rate of 8g/CM at 230 ℃ and 3.8kg 3 ；
Toughener-1, mitsubishi yang, S-2030, methyl methacrylate as shell, silicone-acrylate copolymer as core, core content 30wt.%;
flexibilizer-2, wenzhou longou plastic science, SL-1050, methyl methacrylate as a shell, silicone-acrylate copolymer as a core, core content 50wt.%;
toughening agent-3, shenzhen pascal new material, S203, methyl methacrylate as a shell, organosilicon-acrylate copolymer as a core, and the core content is 35wt.%;
toughening synergist-1, yingchuangdeguza, R974, nano silicon dioxide, average grain size is 12nm;
toughening synergist-2, yingchuangdinggusa, R974, nano silicon dioxide, with average particle size of 16nm;
toughening synergist-3, deshan Japan, QS-40, nano silicon dioxide, with average grain diameter of 7nm;
ultraviolet blocking agent-1, german island gold, nano barium sulfate, average particle size is 60nm;
ultraviolet blocking agent-2, zhongke jin Jiang, nanometer barium sulfate, with average particle diameter of 50nm;
ultraviolet blocking agent-3, yingchuangdeguza, AEROXIDE P25, nanometer titanium dioxide, the average particle size is 21nm;
ultraviolet blocking agent-4, ZHEJIANGZHITAI nanometer, VK-T25Q, nanometer titanium dioxide, with average particle diameter of 30nm;
antioxidants, antioxidant 168, commercially available;
lubricants, PETS-based lubricants, commercially available.
Toughening agent-4, wenzhou longou plastic science, SL-1020, methyl methacrylate as a shell, silicone-acrylate copolymer as a core, 20wt.% of core content;
ACR, commercially available, acrylate toughener;
MBS, commercially available, methyl methacrylate butadiene styrene toughener;
the nano zinc oxide with the average grain diameter of 30nm is sold in the market;
UV absorbers, UV-531, commercially available;
reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Examples 1 to 17
Examples 1 to 17 each provide a PMMA composition having the component contents shown in table 1, and the preparation method is as follows:
all the components are mixed according to the table 1 and then added into a double-screw extruder, the temperature of a machine head is 215 ℃, the temperature of a machine body screw cylinder is 225 ℃, and the PMMA composition is obtained by melt mixing, extrusion and granulation.
TABLE 1 component contents (parts by weight) of PMMA compositions of examples 1 to 17
| 10 | 11 | 12 | 13 | 14 | 15 | 16 | 17 | |
| PMMA resin-1 | 80 | 80 | 80 | 80 | 80 | 80 | 85 | 75 |
| Flexibilizer-1 | 20 | 20 | 20 | 20 | 25 | 15 | 20 | 20 |
| Toughening synergist-1 | 0.3 | 0.3 | 0.3 | 0.3 | 0.5 | 0.1 | 0.3 | 0.3 |
| Ultraviolet blocking agent-2 | 0.5 | 0.25 | 0.1 | 0.75 | 0.5 | 0.5 | 1.5 | 0.25 |
| Ultraviolet blocking agent-4 | 0.5 | 0.75 | 0.9 | 0.25 | 0.5 | 0.5 | 1.5 | 0.25 |
| Antioxidant agent | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.5 | 0 |
| Lubricant agent | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 1 | 0 |
Comparative examples 1 to 7
Comparative examples 1 to 7 each provide a PMMA composition having the following composition in the amounts shown in Table 2, and the preparation method is as follows:
all the components are mixed according to the table 2 and then added into a double-screw extruder, the temperature of a machine head is 215 ℃, the temperature of a machine body screw cylinder is 225 ℃, and the PMMA composition is obtained by melt mixing, extrusion and granulation.
TABLE 2 component contents (parts by weight) of comparative examples 1 to 7PMMA compositions
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | |
| PMMA resin-1 | 80 | 80 | 80 | 80 | 80 | 80 | 80 |
| Flexibilizer-1 | / | / | / | 20 | 20 | 20 | 20 |
| Flexibilizer-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 agent | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
| Lubricant agent | 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 the following property tests:
notched izod impact strength: according to ISO 180-2000 test standard, the test condition is injection molding gap of 2mm at 23 ℃;
ultraviolet ray resistance and color difference: the injection-molded PMMA test plaques of the PMMA composition were irradiated with a UVC-LED germicidal lamp (30W, 254nm wavelength) at a 10cm vertical distance for 40 hours and the color difference before and after UVC-LED irradiation was measured on the CIE 1976L a b standard.
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 the examples
Table 4 test results of comparative examples
According to the test results in Table 3, the PMMA compositions prepared in the examples of the present invention all had high toughness and notched Izod impact strength of 5.6KJ/m or more 2 And the ultraviolet resistance color difference is less than or equal to 2.0.
In examples 1 to 3, the toughening agent in which methyl methacrylate is used as a shell and the organosilicon-acrylate copolymer is used as a core is used, and when the core content is greater than or equal to 30wt.%, the PMMA material can be well toughened, and the higher the core content is, the better the toughness of the PMMA composition is. The toughening agent used in comparative example 1 was also a toughening agent in which methyl methacrylate was the shell and the silicone-acrylate copolymer was the core, but the core content was too low and the notched Izod impact strength of the PMMA composition was 5.4KJ/m 2 And the requirements of complex workpiece structures or assembling procedures such as screwing and the like cannot be met. The toughening agent used in comparative examples 2 and 3 is a non-core-shell structureThe structural toughening agents, specifically ACR and MBS can improve the toughness of the PMMA composition to a certain extent, but can cause the PMMA composition to have very poor ultraviolet resistance, and the color difference of the PMMA composition reaches 4.76 and 7.88 by a UVC-LED disinfection lamp.
In the embodiments 1, 4 and 5, the average particle size of the nano-silica is less than or equal to 16nm, which can play a good synergistic effect with the core-shell structure toughening agent, and when the average particle size of the nano-silica is 7-12 nm, the nano-silica has a better synergistic effect with the toughening agent, so that the prepared PMMA composition has higher toughness. And the comparative example 4 does not contain the toughening synergist, so that the system toughness of the PMMA composition is poor.
In examples 1 and 6 to 13, the use of nano barium sulfate and nano titanium dioxide as the ultraviolet blocking agent can improve the ultraviolet resistance of the PMMA composition and reduce the color difference after ultraviolet irradiation. The comparative example 5 does not contain the ultraviolet blocking agent, the comparative example 6 replaces the ultraviolet blocking agent of the invention with the organic ultraviolet absorber, and the comparative example 7 replaces the ultraviolet blocking agent of the invention with the nano zinc oxide, so that the good ultraviolet resistance can not be realized.
The ultraviolet blocking agents used in examples 10 to 13 are mixtures of nano barium sulfate and nano titanium dioxide, and it can be seen that the use of the compounded ultraviolet blocking agent can achieve lower ultraviolet resistance color difference compared to examples 1, 6 to 8.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The PMMA composition with ultraviolet resistance and high toughness is characterized by comprising the following components in parts by weight:
75 to 85 portions of PMMA resin,
15-25 parts of a toughening agent,
0.1 to 0.5 portion of toughening synergist,
0.5 to 3 portions of ultraviolet blocking agent,
0 to 0.5 portion of antioxidant,
0-1 part of lubricant;
the toughening agent is a toughening agent taking methyl methacrylate as a shell and taking organic silicon and acrylic ester as cores, wherein the content of the organic silicon and the acrylic ester 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.
2. The UV-resistant, high-toughness PMMA composition according to claim 1, characterized in that the nanosilica has an average particle size of 16nm or less.
3. UV-resistant, high-toughness PMMA composition according to claim 2, characterised in that the nanosilica has an average particle size ranging from 7 to 12nm.
4. The UV-resistant, high-toughness PMMA composition according to claim 1, characterized in that the UV blocker has an average particle size of 100nm or less.
5. The UV-resistant, high-toughness PMMA composition according to claim 1, characterized in that the UV blocker is a mixture of nano barium sulfate and nano titanium dioxide in a mass ratio of 1: 1-9.
6. UV-resistant, high-toughness PMMA composition according to claim 1, characterized in that the content of silicone and acrylate in the toughening agent ranges from 35 to 50wt.%.
7. The UV-resistant, high-toughness PMMA composition of claim 1, wherein the PMMA resin has a melt flow rate of 2-8 g/10min at 230 ℃ and 3.8 kg.
8. A method for preparing a UV-resistant, high-toughness PMMA composition as recited in any one of claims 1 through 7, which comprises the steps of:
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 performing melt mixing, extrusion and granulation to obtain the ultraviolet-resistant and high-toughness PMMA composition.
9. The method of claim 8, wherein the extruder is a twin screw extruder, the head temperature is 210 to 230 ℃, and the barrel temperature is 220 to 230 ℃.
10. Use of the uv-resistant, high-toughness PMMA composition according to any one of claims 1 to 7 for the preparation of humidifiers, air conditioning housings, water feeders for pets.
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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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| CN115572449B (en) * | 2022-09-30 | 2023-07-07 | 成都金发科技新材料有限公司 | Ultraviolet-resistant high-toughness PMMA (polymethyl methacrylate) composition and preparation method and application thereof |
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- 2022-09-30 CN CN202211213773.9A patent/CN115572449B/en active Active
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- 2023-09-25 WO PCT/CN2023/120979 patent/WO2024067453A1/en unknown
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024067453A1 (en) * | 2022-09-30 | 2024-04-04 | 成都金发科技新材料有限公司 | Ultraviolet-resistant, highly tough pmma composition, preparation method therefor, and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115572449B (en) | 2023-07-07 |
| WO2024067453A1 (en) | 2024-04-04 |
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