Synthesis of hydrocarbon polymers by cationic polymerization and their thermal properties

Figures & data

Table 1. Reaction conversion and homopolymer physical characteristics.

	PInd^∗	PS^∗∗	Polylimonene^∗∗∗
Conversion (%)	81	92	7
M n (g/mol)	33 × 10^3	2.5 × 10^3	0.478 × 10^3
M w/M n	2.1	13.8	1.5
T g (°C)	207	99	−7
^∗[Ind] = 1.95 mol/L; ^∗∗[St] = 2.15 mol/L; ^∗∗∗[Lim] = 1.71 mol/L; [cat] = 2.42 × 10^−2 mol/L; temp. = −20 °C; time = 300 min.

Figure 1 (a) ¹³C NMR spectra of PInd and Ind-copolymers with St (poly(Ind-co-St)), Lim (poly(Ind-co-Lim)), and ENB (poly(Ind-co-ENB)) obtained using AlCl₃ without an electron donor in C₂H₄Cl₂ at −20 °C and (b) ¹H NMR spectra of the Ind-copolymers.

Figure 2 FTIR spectra of the homopolymers and Ind-copolymers with (a) St [(poly(Ind-co-St)/Ind:St MR = 0.9] and (b) Lim [(poly(Ind-co-Lim)/Ind:Lim MR = 1.4].

Figure 3 FTIR spectra of PInd and poly(Ind-co-ENB) (Ind:ENB MR = 1.0).

Figure 4 (a) UV–vis spectra of PInd (2) and Ind-copolymers: poly(Ind-co-St)/Ind:St MR = 0.9 (1), poly(Ind-co-Lim)/Ind:Lim MR = 1.4 (3), and poly(Ind-co-Nb)/Ind:ENB MR = 4.3 (4) and (b) UV–vis spectrum of Ind.

Figure 5 (a) Homopolymerization conversion and PInd molar mass (M _n) as function of monomer concentration. (b) Copolymerization conversion and poly(Ind-co-St) molar mass (M _n) as a function of catalyst concentration

Figure 6 SEC chromatogram curves of PInd (1) and Ind-copolymers: poly(Ind-co-St)/Ind:St MR = 3.3 (2), poly(Ind-co-ENB)/Ind:Nb MR = 4.3 (3), and poly(Ind-co-Lim)/Ind:Lim MR = 4.8 (4).

Table 2. Comonomer content and T _g values of the Ind-copolymer with St and Lim.

Ind-copolymer	Feed		Reaction conversion (%)	Comonomer content (mol%)	T g (°C)
	Comonomer (mol%)	Ind/comon (MR)
Ind-co-St1^∗	10	0.22/0.02	97	2	201
Ind-co-St2	20	0.19/0.06	95	16	189
Ind-co-St5	50	0.12/0.12	94	71	155
Ind-co-Lim1∗	10	0.22/0.02	27	1	201
Ind-co-Lim2	20	0.19/0.04	27	7	191
Ind-co-Lim5	50	0.12/0.12	16	23	139
^∗FTIR absorption bands: poly(Ind-co-St)/Ind = 1479 cm^−1, St = 1493 cm^−1; poly(Ind-co-Lim)/Ind = 3066 cm^−1, Lim = 881 cm^−1.

Figure 7 M _n (–▪–) and T _g (–▲–) values of the Ind-copolymers as a function of the comonomer concentration: (a) poly(Ind-co-St), (b) poly(Ind-co-ENB), and (c) poly(Ind-co-Lim).

Figure 8 DSC endothermic curves of PInd and Ind-copolymers: (a) poly(Ind-co-St)/Ind:St MR = 0.9 and poly(Ind-co-Nb)/Ind:ENB MR = 1.0; (b) poly(Ind-co-Lim)/Ind:Lim MR = 1.4.

Figure 9 (a) Thermogravimetric mass loss and (b) derivative curves of PInd (2) and Ind-copolymers: (1) poly(Ind-co-St)/Ind:St MR = 0.9, (3) poly(Ind-co-Lim)/Ind:Lim MR = 1.4, and (4) poly(Ind-co-Nb)/Ind:ENB MR = 1.0 (N₂ atm).