At the first stages of the research work, a copolymer of styrene and α methyl styrene was synthesized by the method of radical emulsion polymerization in an inert atmosphere of argon. The initiator was ammonium persulfate. The molar ratio of the initial monomers of styrene and α-methylstyrene was 70 : 30, respectively. It was found that copolymers synthesized under special controlled conditions have good values of permittivity and dielectric loss tangent. It should be noted that the choice of emulsifier directly affects the values of these indicators. It was previously shown that the most optimal emulsifier is potassium stearate, using which the best values of the dielectric constant and dielectric loss tangent were achieved. At the second stage of the research work, a number of copolymers were synthesized containing 4-methoxystyrene, 4 methyl styrene and α-methyl styrene in their structure. It was experimentally confirmed that the synthesis procedure may be applicable for the preparation of copolymers based on derivatives of styrene and α-methylstyrene. The resulting series of copolymers is highly soluble in methylene chloride; films of each copolymer sample of different thicknesses were obtained by casting from a solution. For this series of copolymer films, the dielectric constant and dielectric loss tangent were determined. It was found that the best values of permittivity and dielectric loss tangent are possessed by a sample of copolymer 4-methoxystyrene and α-methylstyrene. At the latest stage of the study, copolymers of styrene and 2,3,4,5,6-pentafluorostyrene, α-methylstyrene and 4-fluoro-α-methylstyrene, 2,3,4,5,6-pentafluorostyrene and 4-fluoro-α-methylstyrene were synthesized. These fluorine-containing derivatives of styrene and α-methylstyrene easily enough enter into the reaction of radical emulsion copolymerization. The copolymer yields are 53-76%, calculated on the weight of the starting monomers. The structure of a number of newly synthesized copolymers was confirmed by IR spectroscopy. In the future, it is planned to define the values of dielectric constant and dielectric loss tangent for these copolymer samples. It is planned to study the thermomechanical properties of the samples, since fluorine-containing polymers are a promising material for operation at elevated temperatures.
Three new copolymers based on fluorine-containing derivatives of styrene and α-methylstyrene were obtained. According to the results of the previous stages of the study, copolymers based on styrene derivatives have improved dielectric properties compared to polystyrene and a copolymer of styrene and α-methyl styrene. The dielectric constant ε and dielectric loss tangent tanδ were measured for the initial and synthesized samples of styrene – α-methyl styrene copolymer at Samara Electromechanical Plant OJ-SC (Samara city, Russia). All measurements of dielectric characteristics were carried out at an alternating current frequency of 10 GHz on a pressed copolymer tablet with a diameter of 10 and a thickness of 3 mm. During the experiment, a measuring stand was used, consisting of a high-frequency signal generator G4-83, an electronically counting frequency meter Ch3-54 with a frequency converter YaZCh-43, a measuring amplifier U2-4; low-frequency signal generator G3-109; measuring unit FKDG 418151.002. The results obtained indicate high values of the dielectric constant. For samples of copolymers of α-methylstyrene – 4-fluoro-α-methylstyrene and styrene – 4-fluoro-α-methylstyrene, values of 4.63 and 4.21, respectively, were obtained. These dielectric permittivity values are superior not only to samples previously obtained during the experiment, but also to some other compounds that are widely used in industry. In particular, the dielectric constant of lavsan, which is used in the manufacture of capacitors, is 3.1-3.3. The improved dielectric constant values are probably related to the high-quality composition of the copolymer. Samples of the copolymer containing 4-fluoro-α-methylstyrene are significantly superior to the copolymer with 2,3,4,5,6-pentafluorostyrene for this characteristic. The values of the dielectric loss tangent are in the range from 8.74∙10−4 to 37.4∙10−4. Given the dielectric characteristics of the synthesized copolymers, we can conclude that there are good prospects for the use of fluorine-containing styrene copolymers. The obtained values of permittivity and dielectric loss tangent indicate a good possible competitiveness of new materials based on new copolymers. In the future, it is planned to study a number of other physicochemical properties of these materials in order to obtain the most complete spectrum of their characteristics.
The paper describes the synthesis of three new copolymers based on styrene and α-methylstyrene derivatives by radical emulsion copolymerization in an aqueous medium in the presence of an ammonium persulfate initiator and potassium stearate emulsifier. In early study, it was found that copolymers based on methoxy derivatives of styrene have the advanced dielectric properties, as compared to polystyrene and a copolymer of styrene and α-methylstyrene. In addition, the latest scientific literature provides data on the biological activity of styrene copolymers. Thus, the synthesis and study of the properties of new copolymers based on styrene and α-methylstyrene creates a prospect for establishing materials with a unique set of properties differing from their previously studied analogues. The structure of synthesized copolymers is confirmed by IR spectroscopy. Along with this, the paper provides the curves of thermogravimetric analysis, data on dielectric constant and tangent of a dielectric loss angle. A hemolytic effect of copolymers is determined, which indicates biocompatibility and further research perspectives towards their suitability for medical use. A copolymer of sodium 4-styrenesulfonate and α-methylstyrene (the molar ratio of starting monomers is 7:3) is soluble in an aqueous medium, which makes it of higher priority in terms of further study into biological activity.
In the course of previous experiments, a technique was developed for the preparation of a copolymer of styrene and α-methylstyrene. This technique is an emulsion polymerization in the initiator of ammonium persulfate in an inert zone of direct current argon. It was found that the best emulsifier is potassium stearate. This substance can be explained by those copolymers that showed the best dielectric performance. In the course of the new experiment, a series of new copolymers of 4-methylstyrene-α-methylstyrene and 4-methoxystyrene-α-methyl-styrene was obtained in the molar ratios of the initial monomers of 8 : 3, 9 : 2 and 10 : 1 for both rows of copolymers. The outputs of the pure product for all compounds accounted for more than 60% in terms of the initial monomers. To further measure the value of the specific volume resistance of the material, films of each newly synthesized copolymer were obtained. Samples of the copolymers were dissolved in methylene chloride and applied to a smooth glass substrate. The choice of this solvent is due to its low toxicity and low boiling point. For the experiment were selected samples with a film thickness of 50 microns. Measurements of the specific volume resistance were carried out at the Research Institute "Girikond" (St. Petersburg) using an Agilent 4339B instrument. The operating voltage was 100 V. The measurement results showed that samples of 4-methoxystyrene-α-methylstyrene copolymer were several orders of magnitude superior to samples of 4-methylstyrene-α-methylstyrene copolymer. Most likely in this case such a difference in the indices of the specific volume resistance of the copolymer films is due to the nature of the functional groups of substituents in the copolymer. From the obtained measurement results it can be seen that the samples containing the methoxy group have a high resistance value compared to the samples containing a methyl group in their structure. In a series of samples of copolymer films, an increase in the specific volume resistivity index is observed with a decrease in the α-methylstyrene content in the copolymer structure. This dependence is observed for copolymers of 4-methylstyrene-α-methylstyrene and for 4-methoxystyrene-α-methylstyrene. The sample of 4-methoxystyrene-α-methylstyrene with a molar ratio of initial monomers of 10 : 1 has the highest value of specific volume resistance among all the obtained samples of copolymer films.
Two new copolymers of 4-methylstyrene and α-methylstyrene were obtained by the emulsion polymerization method according to the previously described and tested method in the course of the experiment in laboratory conditions. The molar ratio of the starting monomers of 4-methylstyrene and α-methylstyrene was 9: 2 and 10: 1, respectively, in each material sample. The structure of the copolymers obtained was confirmed by IR and 1H NMR spectroscopy. Under laboratory conditions, three prototypes of each copolymer film were obtained from the solution. A sample of the copolymer was dissolved in methylene chloride was applied on a smooth glass substrate. After complete evaporation of the solvent, the film was separated from the substrate. The thickness of the films for each copolymer sample was 20, 30, and 50 microns. In the course of further experimentation, these samples were examined for the values of dielectric constant and tangent of dielectric loss angle. The basis of this experiment used a resonant method of measurement. The presented method is based on the variation of conductivity due to a change in the electrical capacitance of the oscillating circuit. In this experiment, the magnitude of the electrical capacitance and the tangent of the dielectric loss angle were measured. Based on the value of the capacitance and the parameters of the film sample to be measured, it is possible to calculate the dielectric constant. From the data obtained it can be seen that with increasing film thickness, dielectric constant values decrease. However, the indicators of the tangent of dielectric loss angle increase. With an increase in the measurement frequency, a slight decrease in the dielectric constant is observed, and the value of the tangent of the dielectric loss angle decreases nonlinearly. In addition, it should be noted that the samples of 4-methylstyrene-α-methylstyrene copolymer films with a molar ratio of starting monomers of 10: 1 have a higher dielectric constant, along with lower values of the dielectric loss tangent. From this it follows that samples with a lower proportion of α-methylstyrene in their structure have better dielectric characteristics compared with their counterparts with a high content of α-methylstyrene.
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