CN110218408B - Optically transparent polymethyl methacrylate/polycarbonate composite and preparation method thereof - Google Patents
Optically transparent polymethyl methacrylate/polycarbonate composite and preparation method thereof Download PDFInfo
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- 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
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Abstract
本发明公开一种光学透明的聚甲基丙烯酸甲酯/聚碳酸酯复合物及其制备方法本发明材料为聚甲基丙烯酸甲酯、聚碳酸酯和阳离子为金属的有机盐的共混物，质量比为60～90：40～10：0.2～3。本发明将阳离子为金属的有机盐加入极大地提高了聚甲基丙烯酸甲酯和聚碳酸酯之间的相容性，极大地改善了材料的透光性能，使材料的透光率大于90％，雾度低于10％，折射率大于1.49，材料光学透明。
The invention discloses an optically transparent polymethyl methacrylate/polycarbonate composite and a preparation method thereof. The material of the invention is a blend of polymethyl methacrylate, polycarbonate and an organic salt whose cation is a metal. The mass ratio is 60-90:40-10:0.2-3. The invention greatly improves the compatibility between polymethyl methacrylate and polycarbonate by adding the organic salt whose cation is metal, greatly improves the light transmittance of the material, and makes the light transmittance of the material greater than 90% , the haze is less than 10%, the refractive index is greater than 1.49, and the material is optically transparent.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, relates to an optically transparent polymethyl methacrylate/polycarbonate blend and a preparation method thereof, and particularly relates to an optically transparent polymethyl methacrylate/polycarbonate compound obtained by compatibilization of polymethyl methacrylate and polycarbonate through organic salt and a preparation method thereof
Background
Polymethyl methacrylate (PMMA, polymethyl methacrylate for short) is an important thermoplastic which is developed earlier, and chemists of Rome-Haas company in Germany in 1927 heat methyl methacrylate between two glass plates, so that the methyl methacrylate is subjected to polymerization reaction, and the polymethyl methacrylate with high transparency and good performance is obtained. In 1931, the company foundries produced PMMA, which was first used in the aircraft industry to replace celluloid plastics for aircraft canopy and windshield applications. The light transmittance of the polymethyl methacrylate under visible light is up to 92-94%, the birefringence and Abbe number are small, the surface glossiness is high, the weather resistance and the impact resistance are good, the price is low, the preparation process is simple, and the forming and processing are easy. It is because of these excellent properties that polymethyl methacrylate has wide applications in the fields of vehicles, building materials, optical instruments, household appliances, and the like.
Polycarbonate (PC for short) is an amorphous, odorless, tasteless, nontoxic and transparent thermoplastic polymer, has good mechanical strength, heat resistance, ultraviolet radiation resistance and electric resistance comprehensive performance, high impact resistance, small creep property, stable product size, easy reinforcement, no toxicity, sanitation, coloring, good cost performance, chemical modification and physical modification potential, and is an important engineering plastic variety with excellent comprehensive performance and extremely wide application. Since the first publication of polycarbonate condensates in 1988 and the first development of polycarbonates with thermoplastic and high melting point by the Bayer company in Germany in 1953, and the industrialization of polycarbonates since the first polycarbonate patent in the same year and after 1958, polycarbonates have gained importance as a very important engineering plastic in the world plastic market.
Polymer blending is a method to achieve new materials with different properties. Among these materials, polymethyl methacrylate (PMMA) has been widely used as a transparent acrylic material because of its sufficient optical transparency and low density. PMMA has the characteristics of good light transmission, high surface hardness and the like, but the toughness is poor. On the other hand, Polycarbonate (PC) has excellent toughness and a high refractive index, but has a low surface hardness. Therefore, the transparent composite material prepared by blending PC and PMMA is expected to realize the complementation of the properties of the PC and the PMMA, and has important significance. However, the PMMA/PC blends prepared are problematic, and PC and PMMA are known to be incompatible, which we believe is due to the difference in refractive index between PC and PMMA, as well as the lack of compatibility of the two. This requires compatibilization to reduce the size of the dispersed phase and to produce transparent blends.
Aiming at the problems, a scheme for improving the compatibility of PMMA and PC and enabling the blended material to be optically transparent is innovatively provided through a large number of experiments. Organic salt (preferably Li-TFSI) with metal cation is compounded and modified with PMMA/PC, and the Li-TFSI is found to promote ester exchange between PC and PAR and improve the compatibility and transparency of the material.
Disclosure of Invention
The object of the present invention is to provide an optically transparent polymethyl methacrylate/polycarbonate blend which has excellent light transmission and a high refractive index.
The purpose of the invention is realized by the following technical scheme:
an optically transparent polymethyl methacrylate/polycarbonate composite material is a blend of polymethyl methacrylate, polycarbonate and organic salt, wherein the mass ratio of the polymethyl methacrylate to the polycarbonate to the organic salt is (60-90): 40-10: 0.2 to 3.
The organic salt cation is a metal cation, specifically a lithium ion, a magnesium ion, a calcium ion or other metal cations;
the organic salt anion is (CF)3SO2)2N-、PF6 -、BF4 -Or CF3CO2-；
Preferably, the metal cation organic salt is lithium bis (trifluoromethanesulfonyl) imide (Li-TFSI).
Preferably, in the above aspect, the mass ratio of the polymethyl methacrylate to the polycarbonate to the Li-TFSI is 90: 10: 0.375.
in order to obtain the effect, the technical means adopted by the invention comprises the following steps:
respectively drying polymethyl methacrylate and polycarbonate in vacuum at 80-120 ℃ for 24-48 h;
step (2), mixing the dried polymethyl methacrylate, polycarbonate and organic salt according to a mass ratio of 60-90: 40-10: 0.2-3, adding the mixture into a melting and mixing device, and melting and mixing at 250-300 ℃ to obtain a mixture;
the melting and mixing equipment is an internal mixer and a double-screw extruder;
if the dried polymethyl methacrylate, the polycarbonate and the organic salt are added into an internal mixer for melt mixing, the rotor speed of the internal mixer is 40-60 rpm/min during mixing, and the melt mixing is 3-20 min;
if the dried polymethyl methacrylate, the polycarbonate and the organic salt are added into a double-screw extruder for melt mixing, the screw speed of the screw extruder is 15-20 rpm/min during feeding, and the screw speed is increased to 45-75 rpm/min during extrusion;
and (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the optically transparent polymethyl methacrylate/polycarbonate blend.
The invention has the beneficial effects that:
the invention adds the organic salt (preferably Li-TFSI) with metal as cation into the composite material of polymethyl methacrylate and polycarbonate, and has the advantages that: (1) the method is simple to operate and small in addition amount, and the PMMA/PC blend is changed from incompatibility into complete compatibility through small addition amount, so that the material has optical transparency, and the method has not been reported before; (2) in addition, the addition of the organic salt (preferably Li-TFSI) with metal cation greatly improves the refractive index of the polymethyl methacrylate, and can meet more application fields on the basis of actual requirements. (3) Especially when the content of PMMA is far greater than that of PC, the PMMA is changed from incompatibility into complete compatibility through an organic salt (preferably Li-TFSI) with metal cation, and the material has optical transparency and is remarkable in creativity. (4) The invention only needs common melting and mixing equipment, and the industrial preparation is simple.
The invention innovatively modifies the polymethyl methacrylate/polycarbonate composite material by using the organic salt (preferably Li-TFSI) with metal as the cation successfully, which is shown in the following steps: the addition of the organic salt greatly improves the compatibility between the polymethyl methacrylate and the polycarbonate, greatly improves the light transmittance of the material, enables the light transmittance of the material to be more than 90%, the haze to be lower than 10%, the refractive index to be more than 1.49, and enables the material to be optically transparent.
The polymethyl methacrylate/polycarbonate composite material greatly improves the transparency of the blend, and can be widely applied to the fields of automobile industry, buildings, electronic and electric appliances and the like.
Drawings
FIG. 1(a) is a sample view of a material prepared in comparative example 1;
FIG. 1(b) is a sample plot of the material prepared in example 1;
FIG. 2(a) is a sample diagram of the material prepared in comparative example 2;
fig. 2(b) is a sample diagram of the material prepared in example 2.
Detailed Description
The invention is further analyzed with reference to the following figures and specific examples.
Comparative example 1.
Respectively drying polymethyl methacrylate and polycarbonate for 24 hours in vacuum at the temperature of 80-120 ℃;
and (2) adding 54g of dried polymethyl methacrylate and 6g of dried polycarbonate into an internal mixer, carrying out melt blending at 250 ℃, and carrying out melt mixing for 10min at the rotating speed of 50 rpm/min.
And (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the polymethyl methacrylate/polycarbonate blend.
The mass ratio of polymethyl methacrylate to polycarbonate in the polymethyl methacrylate/polycarbonate blend prepared in comparative example 1 was 90: 10.
comparative example 2
Respectively drying polymethyl methacrylate and polycarbonate for 24 hours in vacuum at the temperature of 80-120 ℃;
and (2) adding 48g of dried polymethyl methacrylate and 12g of dried polycarbonate into an internal mixer, carrying out melt blending at 250 ℃, and carrying out melt mixing for 10min at the rotating speed of 50 rpm/min.
And (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the polymethyl methacrylate/polycarbonate blend.
The mass ratio of polymethyl methacrylate to polycarbonate in the polymethyl methacrylate/polycarbonate blend prepared in comparative example 2 was 80: 20.
comparative example 3.
Respectively carrying out vacuum drying on polycarbonate and polymethyl methacrylate at 80-120 ℃ for 24-48 h;
and (2) adding 42g of dried polymethyl methacrylate and 18g of dried polycarbonate into an internal mixer, and carrying out melt blending at 230-260 ℃, wherein the rotor speed of the internal mixer is 45-75 rpm, and the melt blending is carried out for 5-15 min.
And (3) discharging the blend from the internal mixer, and cooling to normal temperature to obtain the compound.
The mass ratio of the polymethyl methacrylate to the polycarbonate in the polymer composite prepared in comparative example 3 was 70: 30.
example 1
Respectively drying polymethyl methacrylate and polycarbonate at 80-120 ℃ for 24h in vacuum (Li-TFSI does not need drying);
and (2) adding 54g of dried polymethyl methacrylate, 6g of dried polycarbonate and 0.225g of Li-TFSI into an internal mixer, carrying out melt blending at 250 ℃, and carrying out melt mixing at the rotating speed of 50rpm/min for 10 min.
And (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the polymethyl methacrylate/polycarbonate composite material.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the Li-TFSI in the polymethyl methacrylate/polycarbonate composite material prepared in example 1 is 90: 10: 0.375.
example 2
Respectively drying polymethyl methacrylate and polycarbonate at 80-120 ℃ for 24h in vacuum (Li-TFSI does not need drying);
and (2) adding 48g of dried polymethyl methacrylate, 12g of dried polycarbonate and 0.45g of Li-TFSI into an internal mixer, melting and blending at 250 ℃, and melting and mixing for 10min at the rotating speed of 50 rpm/min.
And (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the polymethyl methacrylate/polycarbonate composite material.
The mass ratio of the polymethyl methacrylate to the polycarbonate to the Li-TFSI in the polymethyl methacrylate/polycarbonate composite material prepared in example 2 was 80: 20: 0.75.
example 3.
Respectively carrying out vacuum drying on polycarbonate and polymethyl methacrylate at the temperature of 80-120 ℃ for 24h (Li-TFSI does not need drying);
and (2) adding 42g of dried polymethyl methacrylate, 18g of dried polycarbonate and 0.45gLi-TFSI into an internal mixer, and carrying out melt blending at 230-260 ℃ with the rotor speed of the internal mixer being 45-75 rpm for 10-25 min.
And (3) discharging the blend from the internal mixer, and cooling to normal temperature to obtain the high-light-transmittance compound.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the lithium salt in the polymer composite prepared in example 3 was 70: 30: 0.75.
the materials prepared in comparative examples 1 to 3 and examples 1 to 3 were subjected to the transmittance-haze test under the following conditions: the sample was pressed into a 0.3mm sheet.
The materials prepared in comparative examples 1 to 3 and examples 1 to 3 were subjected to a refractive index test under the following test conditions: the sample was pressed into a 0.3mm sheet.
TABLE 1 light transmittance and haze of materials prepared in comparative examples 1-2 and examples 1-2
TABLE 2 refractive indices of neat PMMA and materials prepared in examples 1-2
| Sample (I) | Refractive index (n) |
| Pure PMMA | 1.4923 |
| Example 1 | 1.5039 |
| Example 2 | 1.5102 |
The transparency results of the composite materials are shown in FIGS. 1-2. The specific data of the light transmittance-haze test and the refractive index test are shown in tables 1 and 2, the binary melt blend of the polymethyl methacrylate and the polycarbonate is completely incompatible, the light transmittance of the material is as low as 60 percent, the haze is as high as 90 percent, and the material is macroscopically represented as an opaque white pearlescent material. After Li-TFSI is added, the compatibility of the material is greatly improved, the light transmittance is higher than 90%, the haze is lower than 6%, the refractive index is improved to a certain extent compared with that of pure PMMA, and the material is a colorless and transparent composite material in macroscopic appearance. The addition of Li-TFSI is proved to greatly improve the compatibility between PMMA/PC, greatly improve the transparent performance of the composite material and meet the standard of optical transparent materials required by the industry.
Example 4
Respectively drying polymethyl methacrylate and polycarbonate at 80-120 ℃ for 24h in vacuum (Li-TFSI does not need drying);
and (2) adding 54g of dried polycarbonate, 6g of dried polymethyl methacrylate and 0.3g of Li-TFSI into an internal mixer, carrying out melt blending at 250 ℃, and carrying out melt mixing at the rotating speed of 50rpm/min for 10 min.
And (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the optically transparent polymethyl methacrylate/polycarbonate compound.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the Li-TFSI in the polymethyl methacrylate/polycarbonate composite prepared in example 4 was 90: 10: 0.5.
example 5.
Respectively drying polymethyl methacrylate and polycarbonate at 80-120 ℃ for 24h in vacuum (Li-TFSI does not need drying);
and (2) adding 54g of dried polymethyl methacrylate, 6g of dried polycarbonate and 0.45g of Li-TFSI into an internal mixer, melting and blending at 250 ℃, and melting and mixing for 20min at the rotating speed of 50 rpm/min.
And (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the optically transparent polymethyl methacrylate/polycarbonate compound.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the Li-TFSI in the polymethyl methacrylate/polycarbonate composite prepared in example 5 was 90: 10: 0.75.
example 6.
Respectively drying polymethyl methacrylate and polycarbonate at 80-120 ℃ for 24h in vacuum (Li-TFSI does not need drying);
and (2) adding 48g of dried polymethyl methacrylate, 12g of dried polycarbonate and 0.6g of Li-TFSI into an internal mixer, melting and blending at 250 ℃, and melting and mixing for 10min at the rotating speed of 50 rpm/min.
And (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the optically transparent polymethyl methacrylate/polycarbonate compound.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the Li-TFSI in the polymethyl methacrylate/polycarbonate composite prepared in example 6 was 80: 20: 1.
example 7.
Respectively drying polymethyl methacrylate and polycarbonate at 80-120 ℃ for 24h in vacuum (Li-TFSI does not need drying);
and (2) adding 42g of dried polymethyl methacrylate, 18g of dried polycarbonate and 0.45g of Li-TFSI into an internal mixer, melting and blending at 250 ℃, and melting and mixing for 20min at the rotating speed of 50 rpm/min.
And (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the optically transparent polymethyl methacrylate/polycarbonate compound.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the Li-TFSI in the polymethyl methacrylate/polycarbonate composite prepared in example 7 was 70: 30: 0.75.
example 8.
Respectively drying polymethyl methacrylate and polycarbonate at 80-120 ℃ for 48h in vacuum (Li-TFSI does not need drying);
adding 36g of dried polymethyl methacrylate, 24g of dried polycarbonate and 0.9g of Li-TFSI into a double-screw extruder, and carrying out melt mixing at 280 ℃, wherein the screw speed of the double-screw extruder is 20rpm/min during feeding, and the screw speed is increased to 50rpm/min during extrusion to obtain a mixture;
and (3) discharging the mixture from the double-screw extruder equipment, and cooling to normal temperature to obtain the polymethyl methacrylate/polycarbonate compound.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the Li-TFSI in the polymethyl methacrylate/polycarbonate composite prepared in example 8 was 60: 40: 1.5.
the polymethyl methacrylate/polycarbonate composite prepared in the above examples 4 to 8 has a light transmittance of more than 90% and a haze of less than 6%, and a refractive index higher than that of pure PMMA, and is a colorless and transparent composite material in macroscopic view.
Example 9
Respectively carrying out vacuum drying on polymethyl methacrylate and polycarbonate at the temperature of 80-120 ℃ for 48h (Ca-TFSI does not need drying);
adding 36g of dried polymethyl methacrylate, 24g of dried polycarbonate and 1.8g of Ca-TFSI into a double-screw extruder, carrying out melt mixing at 280 ℃, wherein the screw speed of the double-screw extruder is 20rpm/min during feeding, and the screw speed is increased to 50rpm/min during extrusion to obtain a mixture;
and (3) discharging the mixture from the double-screw extruder equipment, and cooling to normal temperature to obtain the polymethyl methacrylate/polycarbonate compound.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the Ca-TFSI in the polymethyl methacrylate/polycarbonate composite prepared in example 8 was 60: 40: 3.
example 10
Respectively carrying out vacuum drying on polymethyl methacrylate and polycarbonate at the temperature of 80-120 ℃ for 48h (Mg-TFSI does not need to be dried);
adding 36g of dried polymethyl methacrylate, 24g of dried polycarbonate and 0.9g of Mg-TFSI into a double-screw extruder, carrying out melt mixing at 280 ℃, wherein the screw speed of the double-screw extruder is 20rpm/min during feeding, and the screw speed is increased to 50rpm/min during extrusion to obtain a mixture;
and (3) discharging the mixture from the double-screw extruder equipment, and cooling to normal temperature to obtain the polymethyl methacrylate/polycarbonate compound.
The mass ratio of the polymethyl methacrylate, the polycarbonate and the Mg-TFSI in the polymethyl methacrylate/polycarbonate composite prepared in example 8 is 60: 40: 1.5.
the above embodiments are not intended to limit the present invention, and the present invention is not limited to the above embodiments, and all embodiments are within the scope of the present invention as long as the requirements of the present invention are met.
Claims (5)
1. An optically transparent polymethyl methacrylate/polycarbonate composite material is a blend and is characterized by comprising polymethyl methacrylate, polycarbonate and organic salt, wherein the mass ratio of the polymethyl methacrylate to the polycarbonate is 60-90: 40-10: 0.2 to 3;
the organic salt is lithium bis (trifluoromethanesulfonyl) imide.
2. The optically transparent polymethylmethacrylate/polycarbonate composite material of claim 1 wherein the mass ratio of polymethylmethacrylate, polycarbonate and Li-TFSI is 90: 10: 0.375.
3. a method of preparing an optically transparent polymethylmethacrylate/polycarbonate composite material according to any of claims 1 to 2, characterized in that the method comprises the steps of:
respectively drying polymethyl methacrylate and polycarbonate in vacuum at 80-120 ℃ for 24-48 h;
adding the dried polymethyl methacrylate, polycarbonate and organic salt into a melt mixing device according to the mass ratio, and carrying out melt mixing at the temperature of 250-300 ℃ to obtain a mixture;
and (3) discharging the mixture from the melting and mixing equipment, and cooling to normal temperature to obtain the optically transparent polymethyl methacrylate/polycarbonate composite material.
4. The method according to claim 3, wherein the dried polymethylmethacrylate, the polycarbonate and the organic salt are added to an internal mixer for melt-kneading, and the rotor speed of the internal mixer is 40 to 60rpm/min, and the melt-kneading is performed for 3 to 20 min.
5. The method according to claim 3, wherein the dried polymethylmethacrylate, the polycarbonate and the organic salt are added to a twin-screw extruder for melt-kneading, the screw speed of the screw extruder during feeding is 15 to 20rpm/min, and the screw speed is increased to 45 to 75rpm/min during extrusion.
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| "Development of ion conducting ionic liquid-based gel polymer electrolytemembrane PMMA/BMPyr.TFSI - With improved electrical, optical, thermaland structural properties";Safna Hussan K.P et al.;《Solid State Ionics》;20170912;第166–175页 * |
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