[C3mim][NTf2]/DEC/[Li][NTf2]体系的基础性质

doi:10.3866/PKU.WHXB201910067

摘要/Abstract

摘要：

本文通过传统方法合成了1-丙基-3-甲基咪唑双三氟甲基磺酸亚胺疏水型离子液体，在离子液体中加入碳酸二乙酯和双三氟甲基磺酸亚胺锂盐制备了八个体系。通过差式扫描量热仪考察了上述体系的热力学性质。考察了体系的半稳定态温度随着锂盐的加入后的变化情况，以及玻璃化温度随离子液体与碳酸二乙酯的比例的变化情况。测量结果并没有观测到体系的熔点温度，表明碳酸二乙酯和锂盐能够在较低的温度下溶解在离子液体中。系统研究了不同温度下八个体系的基础性质，如：锂离子([Li]⁺)自扩散系数随碳酸二乙酯浓度的变化规律，密度、粘度和电导率随温度的变化规律，利用Vogel Fulcher Tamman (VFT)，Final Vogel Fulcher Tamman (FVFT)和Arrhenius方程计算得到八个体系的粘度活化能、电导活化能等。在性质实验的基础上，通过分子动力学模拟讨论了[Li]⁺与[NTf₂]^-/碳酸二乙酯之间的相互作用情况，及碳酸二乙酯的引入对LiNTf₂/离子液体体系的微观结构影响，其中阴离子[NTf₂]^-通过氧原子与锂离子之间发生相互作用。通过径向分布函数和对[Li]⁺周围O原子的配位数的分析表明，碳酸二乙酯的引入，削弱了[Li]⁺与[NTf₂]^-之间的相互作用。因此，碳酸二乙酯的引入有利于[Li]⁺的扩散，该结论与实验结果相符。

关键词: 离子液体, 碳酸二乙酯, 双三氟甲基磺酸亚胺锂, 基础性质

Abstract:

The hydrophobic ionic liquid (IL) 1-propyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide ([C₃mim][NTf₂]) was synthesized according to traditional methods. By adding different amounts of diethyl carbonate (DEC) solvent and lithium bis[(trifluoromethyl)sulfonyl]imide ([Li][NTf₂]) salt to [C₃mim][NTf₂] IL, eight solution systems were prepared. First, the thermodynamic properties of the eight solution systems were characterized by differential scanning calorimetry (DSC). The semi-stable temperature of the system gradually disappeared with increasing lithium salt content, but the melting point temperature was not apparent in the experiment. These results indicate that DEC and lithium salts can dissolve in ILs within the tested temperature range. The basic properties of the eight systems, including thermodynamic and dynamic properties, were systematically studied at different temperatures. The variation in the self-diffusion coefficient of lithium ion ([Li]⁺) as a function of DEC concentration, density changes, viscosity, conductivity, and the viscosity/conductivity activation energy of the eight systems was calculated by the Vogel Fulcher Taman (VFT), Final Vogel Fulcher Taman (FVFT), and Arrhenius equations. The effect of temperature on the properties of the system was studied in detail. Within the temperature range measured herein, the deviation between the fitting equation and experimental value was small. Consequently, these equations were successfully used to calculate the properties of the system at various temperatures. All fitting parameters of the corresponding equations are provided herein. The viscosity for all systems decreased rapidly with increasing temperature, which increased the conductivity. Based on these experiments, the influence of DEC on the system microstructure was discussed in the context of the molecular dynamics simulation results. In particular, the interaction between [Li]⁺ and [NTf₂]^-/DEC was examined. In all solution systems, [NTf₂]^- coordinates to [Li]⁺ through only the O atom and not the N atom. Radial distribution function (RDF) analysis showed that the interaction between [Li]⁺ and [NTf₂]^- weakened with increasing DEC concentration. DEC molecules were observed in the first solvation layer of [Li]⁺ coordinating to [Li]⁺ through the carbonyl O atom. Although the interaction between [Li]⁺ and DEC was weakened, competition between [NTf₂]^- and DEC in the first solvation layer of [Li]⁺ was observed by the coordination number analysis of the O atom around [Li]⁺. Therefore, the introduction of DEC is beneficial for Li⁺ diffusion, which is consistent with the experimental results.

Key words: Ionic liquids, Diethyl carbonate, Lithium bis[(trifluoromethyl)sulfonyl]imide, Basic property

惠淑荣, 赵丽薇, 刘青山, 宋大勇. [C₃mim][NTf₂]/DEC/[Li][NTf₂]体系的基础性质[J]. 物理化学学报, 2020, 36(11), 1910067. doi: 10.3866/PKU.WHXB201910067

Shurong Hui, Liwei Zhao, Qingshan Liu, Dayong Song. Basic Properties of [C₃mim][NTf₂]/DEC/[Li][NTf₂] Systems[J]. Acta Physico-Chimica Sinica 2020, 36(11), 1910067. doi: 10.3866/PKU.WHXB201910067

链接本文: https://www.whxb.pku.edu.cn/CN/10.3866/PKU.WHXB201910067

https://www.whxb.pku.edu.cn/CN/Y2020/V36/I11/1910067

图/表 20

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Table 9

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Table 11

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Name	Purity (by mass)	MW	Source	T_m/K
[C₃mim][Cl]	≥0.99%	160.64	Lanzhou Institute of Chemical Physics, Lanzhou, China	≈ 333
[Li][NTf₂]	≥0.99%	287.09	Solvay Chemicals Co., LTD, Zhenjiang, China	≈ 407
[C₃mim][NTf₂]	≥0.99%	405.33	Synthesized	–
DEC	≥0.99%	118.13	Aladdin Industrial Inc. Shanghai, China	≈ 230

	Ratio	T_g/K	T_semi/K	η/(mPa·s)	σ/(mS·cm^-1)	10¹¹D_[Li]⁺/(m²·s^-1)
1	0.9769 mol·kg^-1 [Li][NTf₂]/(V(C₃mimNTf₂) : V(DEC) = 6 : 6)	171.25	–	18.21	4.32	3.928
2	V(C₃mimNTf₂) : V(DEC) = 6 : 6	151.69	223.43	5.194	10.00	–
3	1.1630 mol·kg^-1 [Li][NTf₂]/(V(C₃mimNTf₂) : V(DEC) = 6 : 4)	179.57	–	38.93	2.91	1.927
4	V(C₃mimNTf₂) : V(DEC) = 6 : 4	158.00	213.27	7.320	10.04	–
5	1.0408 mol·kg^-1 [Li][NTf₂]/(V(C₃mimNTf₂) : V(DEC) = 6 : 3)	180.27	–	45.43	2.87	1.176
6	V(C₃mimNTf₂) : V(DEC) = 6 : 3	160.98	211.35	9.647	9.59	–
7	1.0075 mol·kg^-1 [Li][NTf₂]/(V(C₃mimNTf₂) : V(DEC) = 6 : 0)	196.51	–	244.1	1.333	–
8	V(C₃mimNTf₂) : V(DEC) = 6 : 0	175.59	–	44.31	5.42	–

T/K	ρ/(g·cm^–3)
T/K	1	2	3	4	5	6	7	8
288.15	1.354014	1.245133	1.414378	1.287756	1.431885	1.320589	1.570253	1.484694
293.15	1.348608	1.239945	1.408932	1.282615	1.426470	1.315487	1.564899	1.479711
298.15	1.343203	1.234745	1.403495	1.277471	1.421075	1.310380	1.559525	1.474744
303.15	1.337790	1.229540	1.398082	1.272326	1.415697	1.305280	1.554157	1.469791
308.15	1.332376	1.224339	1.392673	1.267186	1.410333	1.300185	1.548802	1.464858
313.15	1.326968	1.219138	1.387274	1.26205	1.404975	1.295100	1.543474	1.459950
318.15	1.321566	1.213941	1.381881	1.256919	1.399622	1.290019	1.538174	1.455062
323.15	1.316167	1.208734	1.376498	1.251789	1.39429	1.284941	1.532900	1.450186
328.15	1.310775	1.203532	1.371121	1.246663	1.388963	1.279872	1.527654	1.445328
333.15	1.305379	1.198331	1.365749	1.241541	1.383643	1.27481	1.522432	1.440490
338.15	1.299981	1.193134	1.360383	1.236419	1.378333	1.269746	1.517233	1.435661
343.15	1.294590	1.187930	1.355025	1.231294	1.373028	1.264689	1.512054	1.430847
348.15	1.289199	1.182717	1.349668	1.226177	1.367733	1.259638	1.506902	1.426042

T/K	η/(mPa·s)
T/K	1	2	3	4	5	6	7	8
288.15	26.40	6.71	61.16	9.728	72.66	13.25	478.5	69.68
293.15	21.79	5.886	48.3	8.398	56.83	11.28	336.8	55.06
298.15	18.21	5.194	38.93	7.320	45.43	9.647	244.1	44.31
303.15	15.40	4.625	31.85	6.430	36.86	8.390	181.5	36.25
308.15	13.17	4.138	26.43	5.704	30.38	7.365	138.0	30.11
313.15	11.36	3.732	22.21	5.092	25.38	6.515	107.1	25.32
318.15	9.886	3.384	18.98	4.574	21.45	5.805	84.70	21.54
323.15	8.680	3.084	16.72	4.125	18.5	5.208	68.04	18.54
328.15	7.668	2.824	14.54	3.749	16.29	4.700	55.44	16.26
333.15	6.825	2.595	12.58	3.422	14.23	4.264	45.71	14.39
338.15	6.114	2.394	10.96	3.138	12.41	3.881	38.18	12.78
343.15	5.506	2.217	9.54	2.889	10.82	3.556	32.29	11.35
348.15	4.983	2.061	8.407	2.67	9.489	3.27	27.59	10.12

T/K	σ/(mS·cm^–1)
T/K	1	2	3	4	5	6	7	8
288.15	3.20	7.92	1.953	7.78	1.887	7.29	0.740	3.59
293.15	3.71	8.91	2.43	8.87	2.36	8.40	0.986	4.41
298.15	4.32	10.00	2.91	10.04	2.87	9.59	1.333	5.42
303.15	4.99	11.09	3.50	11.18	3.49	10.86	1.776	6.45
308.15	5.73	12.21	4.12	12.44	4.13	12.17	2.27	7.65
313.15	6.48	13.36	4.85	13.81	4.82	13.56	2.84	8.99
318.15	7.28	14.56	5.56	15.19	5.56	15.00	3.43	10.44
323.15	8.12	15.79	6.28	16.64	6.47	16.52	4.16	11.90
328.15	8.98	17.07	7.18	18.17	7.36	18.12	4.98	13.51
333.15	9.92	18.40	8.05	19.68	8.34	19.72	5.93	15.33
338.15	10.93	19.76	9.05	21.3	9.31	21.3	6.92	17.07
343.15	11.90	21.2	9.99	22.9	10.37	23.1	8.01	19.07
348.15	12.96	22.6	10.99	24.5	11.54	24.9	9.23	21.2

[C₃mim][NTf₂]/DEC/[Li][NTf₂]体系的基础性质

Basic Properties of [C₃mim][NTf₂]/DEC/[Li][NTf₂] Systems

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T/K	ρ/(g·cm^-3)
T/K	Exp.	Lit.
293.15	1.479711	1.47939 ¹⁴ (0.0217), 1.47932 ¹⁵ (0.0264)
298.15	1.474744	1.47444 ¹⁴ (0.0206), 1.47424 ¹⁵ (0.0342)
303.15	1.469791	1.46950 ¹⁴ (0.0198), 1.46940 ¹⁵ (0.0266), 1.47114¹⁶(-0.0918)
308.15	1.464858	1.46458 ¹⁴ (0.0190), 1.46443 ¹⁵ (0.0292), 1.46683¹⁶(-0.1346)
313.15	1.459950	1.45967 ¹⁴ (0.0192), 1.45944 ¹⁵ (0.0349), 1.46207¹⁶(-0.1452)
318.15	1.455062	1.45478 ¹⁴ (0.0194), 1.45463 ¹⁵ (0.0297), 1.45705¹⁶(-0.1366)
323.15	1.450186	1.44991 ¹⁴ (0.0190), 1.44973 ¹⁵ (0.0314), 1.45166¹⁶(-0.1016)
328.15	1.445328	1.44506 ¹⁴ (0.0185)
333.15	1.440490	1.44023 ¹⁴ (0.0180), 1.44012 ¹⁶ (0.0257)
338.15	1.435661	1.43542 ¹⁴ (0.0168),
343.15	1.430847	1.43062¹⁴(0.0159)
T/K	η/(mPa·s)		σ/(mS·cm^-1)
T/K	Exp.	Lit.	Exp.	Lit.
293.15	55.06	54.19¹⁰(1.58)	4.41	3.55¹⁵(19.50)
298.15	44.31	43.7¹⁴(1.38), 43.94¹⁰(0.84)	5.42	4.35¹⁵(19.74)
303.15	36.25	35.68¹⁴(1.57), 35.92¹⁰(0.91)	6.45	5.21¹⁵(19.22)
308.15	30.11	29.51¹⁴(1.99), 30.00¹⁵(0.37)	7.65	6.11¹⁵(20.13)
313.15	25.32	24.77¹⁴(2.17), 25.32¹⁵(0.00)	8.99	7.10¹⁵(21.02)
318.15	21.54	21.01¹⁴(2.46), 21.58¹⁵(-0.19)	10.44	8.13¹⁵(22.13)
323.15	18.54	18.04¹⁴(2.70), 18.82¹⁵(-1.51)	11.90	9.23¹⁵(22.44)
328.15	16.26	15.59¹⁴(4.12)
333.15	14.39	13.63¹⁴(5.28)
338.15	12.78	12.02¹⁴(5.95)
343.15	11.35	10.66 ¹⁴ (6.08)

Property	1	2	3	4	5	6	7	8
ρ/(g·cm^-3)
A	1.66529	1.54490	1.72495	1.58346	1.73976	1.61325	1.87451	1.76609
10⁴B	-10.80	-10.40	-10.80	-10.30	-10.70	-10.20	-10.60	-9.77
R	0.99999	0.99999	0.99999	0.99999	0.99999	0.99999	0.99994	0.99996
VFT equation
η/(mPa·s)
η₀/(mPa·s)	0.1056	0.0959	0.1839	0.1133	0.2258	0.1516	0.1437	0.2973
B/K	765.9	663.0	691.7	653.5	650.7	591.0	896.0	600.2
10³E_η/eV	66.1	57.2	59.7	56.4	56.1	51.0	77.3	51.8
T₀/K	149.4	132.1	169.0	141.4	175.5	156.0	177.7	178.2
R	0.99999	0.99999	0.99982	0.99999	0.99993	0.99998	0.99999	0.99998
σ/(mS·cm^-1)
σ₀/(mS·cm^-1)	332.51	362.11	304.76	433.42	405.52	440.76	827.03	791.37
B/K	643.9	609.5	582.6	602.7	635.2	577.6	751.5	661.6
10³E_σ/eV	55.6	52.6	50.3	52.0	54.8	49.8	64.8	57.1
T₀/K	149.7	128.5	172.7	138.3	169.8	147.3	181.0	165.5
R	0.99996	0.99995	0.99980	0.99997	0.99994	0.99997	0.99993	0.99994

T/K	10⁴α/K^-1
T/K	1	2	3	4	5	6	7	8
288.15	7.98	8.35	7.64	8.00	7.47	7.72	6.75	6.58
293.15	8.01	8.39	7.67	8.03	7.50	7.75	6.77	6.60
298.15	8.04	8.42	7.70	8.06	7.53	7.78	6.80	6.63
303.15	8.07	8.46	7.72	8.10	7.56	7.81	6.82	6.65
308.15	8.11	8.49	7.75	8.13	7.59	7.85	6.84	6.67
313.15	8.14	8.53	7.79	8.16	7.62	7.88	6.87	6.69
318.15	8.17	8.57	7.82	8.19	7.64	7.91	6.89	6.72
323.15	8.21	8.60	7.85	8.23	7.67	7.94	6.91	6.74
328.15	8.24	8.64	7.88	8.26	7.70	7.97	6.94	6.76
333.15	8.27	8.68	7.91	8.30	7.73	8.00	6.96	6.78
338.15	8.31	8.72	7.94	8.33	7.76	8.03	6.99	6.81
343.15	8.34	8.75	7.97	8.37	7.79	8.07	7.01	6.83
348.15	8.38	8.79	8.00	8.40	7.82	8.10	7.03	6.85

1000T^–1/K^–1	lnη/(mPa·s)
1000T^–1/K^–1	1	2	3	4	5	6	7	8
3.4704	3.2735	1.9036	4.1135	2.2750	4.2858	2.5840	6.1707	4.2439
3.4112	3.0813	1.7726	3.8774	2.1280	4.0401	2.4230	5.8195	4.0084
3.354	2.9021	1.6475	3.6618	1.9906	3.8162	2.2666	5.4975	3.7912
3.2987	2.7344	1.5315	3.4610	1.8610	3.6071	2.1270	5.2013	3.5904
3.2452	2.5779	1.4202	3.2745	1.7412	3.4138	1.9967	4.9273	3.4049
3.1934	2.4301	1.3169	3.1005	1.6277	3.2340	1.8741	4.6738	3.2316
3.1432	2.2911	1.2191	2.9434	1.5204	3.0657	1.7587	4.4391	3.0699
3.0945	2.1610	1.1262	2.8166	1.4171	2.9178	1.6502	4.2201	2.9199
3.0474	2.0371	1.0382	2.6769	1.3215	2.7906	1.5476	4.0153	2.7887
3.0016	1.9206	0.9536	2.5321	1.2302	2.6554	1.4502	3.8223	2.6665
2.9573	1.8106	0.8730	2.3943	1.1436	2.5185	1.3561	3.6423	2.5479
2.9142	1.7058	0.7962	2.2555	1.0609	2.3814	1.2686	3.4748	2.4292
2.8723	1.6060	0.7232	2.1291	0.9821	2.2501	1.1848	3.3175	2.3145

1000T^–1/K^–1	lnσ/(mS·cm^–1)
1000T^–1/K^–1	1	2	3	4	5	6	7	8
3.4704	1.1632	2.0694	0.6694	2.0516	0.6350	1.9865	-0.3011	1.2782
3.4112	1.3110	2.1872	0.8879	2.1827	0.8587	2.1282	-0.0141	1.4839
3.3540	1.4633	2.3026	1.0682	2.3066	1.0543	2.2607	0.2874	1.6901
3.2987	1.6074	2.4060	1.2528	2.4141	1.2499	2.3851	0.5744	1.8641
3.2452	1.7457	2.5023	1.4159	2.5209	1.4183	2.4990	0.8198	2.0347
3.1934	1.8687	2.5923	1.5790	2.6254	1.5728	2.6071	1.0438	2.1961
3.1432	1.9851	2.6783	1.7156	2.7206	1.7156	2.7081	1.2326	2.3456
3.0945	2.0943	2.7594	1.8374	2.8118	1.8672	2.8046	1.4255	2.4765
3.0474	2.1950	2.8373	1.9713	2.8998	1.9961	2.8970	1.6054	2.6034
3.0016	2.2946	2.9124	2.0857	2.9796	2.1211	2.9816	1.7800	2.7298
2.9573	2.3915	2.9837	2.2028	3.0587	2.2311	3.0587	1.9344	2.8373
2.9142	2.4765	3.0540	2.3016	3.1311	2.3389	3.1398	2.0807	2.9481
2.8723	2.5619	3.1179	2.3970	3.1987	2.4458	3.2149	2.2225	3.0540

System	[Li][NTf₂]	[C₃mim][NTf₂]	DEC	ρ_c/(g·cm^-3)	ρ_e/(g·cm^-3)	δ%
1	100	152	344	1.36573	1.34320	-1.68
3	100	148	222	1.41818	1.40350	-1.05
5	100	178	201	1.43260	1.42108	-0.81
7	100	245	0	1.54756	1.55953	0.77

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