| The discovery of graphene,a naturally occurring two-dimensional polymer,has initiated the continued explorations into different kinds of two-dimensional materials.Until recently,there was a breakthrough in synthesis of two-dimensional polymer single-crystals with precise crystallographic structures and the preparation of its monolayers.Due to the crystallization process of two-dimensional polymer monomers that has an important influence on the photopolymerization and exfoliation of their monolayers.The dissolution equilibrium data could be guidance for process of crystallization.Hence,it is necessary to study deeply the solubility data of two-dimensional polymer monomers.(1)At first,the solubility of isomaltose was used to verify the reliability of the static gravimetric method,which were fitted by the model.The calculated values of Apelblat model were compared with the reported in the literature.According to results,the static gravimetric method used in this paper was relatively accuracy with small relative deviation.(2)Two-dimensional polymer monomer was prepared by one-step synthesis method.Some solvents were tried to dissolute the monomer,the experimental result indicated that dichloromethane was suitable as the positive solvent,and hexane was considered as a suitable anti-solvent.Secondly,The solubility of two-dimensional polymer monomers in dichloromethane + hexane was measured from(283.15 to 303.15)K by a gravimetric method at atmosphere pressure(P = 0.1 MPa).The experimental results were as followed: The solubility of monomers increased along with the temperature,but the overall change was small.The solubility of monomers increased along with the molar fraction of dichloromethane,especially when the molar fraction of dichloromethane was over 0.60.(3)Based on the trend of solubility data,we chose the antisolvent recrystallization to purify two-dimensional polymer monomers,and studied the induction period of crystallization.For further research on the variation of solubility of two-dimensional polymer monomers,the solubility data were correlated with the Apelblat equation,CNIBS/R-K equation,and the Apel-JA equation.The ARD and RMSD values of all the models were very small,but the correlation indexes were over 0.99,which showed that those models could gave satisfactory correlation results.The solubility data points which were not measured in the experiment can be calculated by these models.Finally,four light sources(sunlight,100 W tungsten filament lamp,150 W LED floodlight and ultraviolet lamp)were selected as reaction conditions,the FT-IR results showed that ultraviolet light was the most suitable light. |
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