NMR Characterization of Polymethylhydrosiloxane Synthesized using Dichloromethane and Diethyl Ether as Solvent for Vitreous Substitute

Nabillah Fa'diyyah Zahra, Diba Grace Auliya, Vira Fuji Arini, Fitrilawati Fitrilawati, Lusi Safriani, Risdiana Risdiana

Abstract

Polymethylhydrosiloxane (PMHS) can be synthesized from dichloromethylsilane (DCHS) by the hydrolysis-condensation method. In this synthesis method, a solvent is needed. Dichloromethane (DCM) or diethyl ether (DE) can be used as a solvent in the synthesis of PMHS. These two solvents greatly affect the physical properties of the resulting PMHS. Therefore, studies are needed to look at the characteristics and chemical content of the PMHS synthesized using these two solvents. In this research, we reported the characteristics and content studies of PMHS synthesized using different solvents, DCM and DE, using 1H-NMR and 13C-NMR. It was found that both samples had three peaks (Si-H, Si-CH3, and Si-CH3) on 1H-NMR measurement and one peak (Si-CH3) on 13C-NMR measurement. All of the peaks found were by the characteristics of PMHS and no other elements were found from solvents indicating that the PMHS samples had been successfully synthesized with a high degree of purity. In addition, the possibility of structures formed in the PMHS samples was also obtained.

Keywords

Dichloromethane; Diethyl Ether; NMR; PMHS; Vitreous Humour.

Full Text:

PDF

References

C. Alovisi, C. Panico, U. De Sanctis, and C. M. Eandi, “Vitreous Substitutes: Old and New Materials in Vitreoretinal Surgery,” J. Ophthalmol., vol. 2017, 2017, doi: 10.1155/2017/3172138. [2] S. Setiadji et al., “Optimization of polydimethylsiloxane synthesized parameters as vitreous humour substitutes,” Mater. Sci. Forum, vol. 966 MSF, pp. 189–193, 2019, doi: 10.4028/www.scientific.net/MSF.966.189. [3] K. E. Swindle and N. Ravi, “Recent advances in polymeric vitreous substitutes,” Expert Rev. Ophthalmol., vol. 2, no. 2, pp. 255–265, 2007, doi: 10.1586/17469899.2.2.255. [4] J. J. Chruściel, M. Fejdyś, and W. Fortuniak, “Synthesis, characterization and microstructure of new liquid poly(methylhydrosiloxanes) containing branching units SiO4/2,” Polymers (Basel)., vol. 10, no. 5, 2018, doi: 10.3390/polym10050484. [5] S. J. Lee, M. Goedert, M. T. Matyska, E. M. Ghandehari, M. Vijay, and J. J. Pesek, “Polymethylhydrosiloxane (PMHS) as a functional material for microfluidic chips,” J. Micromechanics Microengineering, vol. 18, no. 2, 2008, doi: 10.1088/0960-1317/18/2/025026. [6] M. S. Yadav, A. S. Singh, A. K. Agrahari, N. Mishra, and V. K. Tiwari, “Silicon industry waste polymethylhydrosiloxane-mediated benzotriazole ring cleavage: A practical and green synthesis of diverse benzothiazoles,” ACS Omega, vol. 4, no. 4, pp. 6681–6689, 2019, doi: 10.1021/acsomega.9b00343. [7] D. Seyferth, C. Prud’Homme, and G. H. Wiseman, “Cyclic Polysiloxanes from the Hydrolysis of Dichlorosilane,” Inorg. Chem., vol. 22, no. 15, pp. 2163–2167, 1983, doi: 10.1021/ic00157a014. [8] P. J. Flory, “Fundamental principles of condensation polymerization,” Chem. Rev., vol. 39, no. 1, pp. 137–197, 1946, doi: 10.1021/cr60122a003. [9] V. F. Arini, U. Fauziah, D. G. Auliya, S. Setiadji, Fitrilawati, and Risdiana, “Synthesis of low viscosity of polymethylhydrosiloxane using monomer of dichloromethylsilane,” J. Phys. Conf. Ser., vol. 2165, no. 1, pp. 2–8, 2022, doi: 10.1088/1742-6596/2165/1/012041. [10] R. Gunawan, A. Bayu, and D. Nandiyanto, “Indonesian Journal of Science & Technology How to Read and Interpret 1H-NMR and 13C-NMR Spectrums,” vol. 6, no. 2, pp. 267–298, 2021. [11] Fitrilawati et al., “Effect of KOH concentration on characteristics of polydimethylsiloxane synthesized by ring opening polymerization method,” J. Phys. Conf. Ser., vol. 1080, no. 1, 2018, doi: 10.1088/1742-6596/1080/1/012016.