混合热力学促进剂对水合物法分离回收瓦斯的影响

doi:10.16085/j.issn.1000-6613.2024-0024

摘要/Abstract

摘要：

水合物法在分离瓦斯混合气体方面具有清洁、高效、安全的优势，为突破水合物储气效率的瓶颈问题，在磁力搅拌体系中考察了水合物法分离30% CH₄/70% N₂混合气（摩尔分数）的动力学规律与储气效率。四氢呋喃（THF）、环戊烷（CP）与四丁基溴化铵（TBAB）、四丁基氟化铵（TBAF）二元混合体系作为水合物形成热力学促进剂，0.06% L-色氨酸（Trp）作为动力学促进剂。结果表明：与THF或CP单一添加的实验体系相比，THF-TBAF或CP-TBAB、CP-TBAF体系均能延续水合物形成、提高储气量、降低形成速率，其中CP-TBAF改善效果最为明显，3h内的储气量提高了1.33倍，而水合物初期形成速率下降3倍以上。THF-TBAB-Trp、THF-TBAF-Trp体系增大了N₂在水合物相的储集量，使CH₄/N₂的分离效果低于THF-Trp体系；CP与TBAB或TBAF在瓦斯水合分离过程中具有耦合促进作用，CP-TBAF使水合物储气量、分离因子、CH₄回收率等关键指标全面提升，其中平均CH₄回收率最高可达68.5%，CP-TBAF组合为突破瓦斯水合分离效率提供了参考。

关键词: 混合热力学促进剂, 水合物, 甲烷回收率, 动力学, 分离浓度

Abstract:

The advantage of separation gas mixture via hydrate method includes clean, efficient and safe. We examined the synergistic effect of sII hydrate promoters, semi-cage hydrate promoters and amino acids on hydrate formation of 30% CH₄/70% N₂ mixture with magnetic stirring to solve the problem of gas storage capacity, involving four thermodynamic promoters [tetrahydrofuran (THF), cyclopentane (CP), tetrabutylammonium bromide (TBAB) and tetrabutylammonium fluoride (TBAF)], with a 0.06% Tryptophan (Trp) as kinetic promotor added in every experiments system of hydrate formation. The results of the study showed that THF-TBAF, CP-TBAB and CP-TBAF systems continued the growth of hydrate and enhanced the gas uptake comparing the THF or CP as the single thermodynamic promotor system. However, the hydrate growth rate was decreased for adding semi-cage thermodynamic promoters. The average gas consumption in CP-TBAF system was the highest among the mixed promotors systems and increased by 1.33 times within 3 hours. Meanwhile, the normalized gas uptake rate was decreased by more 3 times. The N₂ entering the hydrate phase in THF-TBAB-Trp and THF-TBAF-Trp system was so more that separation effect was lower than THF-Trp system. CP and TBAB/TBAF mixture had the synergistic effect on the process of separation CH₄/N₂via hydrate technology for CH₄ of stronger selectivity. The improving effect on hydration separation mixed gas in CP-TBAF system was optimal. The gas consumption, separation factor and CH₄ recovery rate in CP system were boosted for adding TBAF. The average CH₄ recovery rate was up to 68.5%. The CP-TBAF combination provided a reference for improving the efficiency of coal mine gas hydration separation.

Key words: mixed thermodynamic promoter, hydrate, methane recovery, kinetics, separation concentration

中图分类号:

TD712

张强, 孙楠, 郑俊杰, 吴强, 刘传海, 李元吉. 混合热力学促进剂对水合物法分离回收瓦斯的影响[J]. 化工进展, 2025, 44(1): 192-201.

ZHANG Qiang, SUN Nan, ZHENG Junjie, WU Qiang, LIU Chuanhai, LI Yuanji. Effect of mixed thermodynamic promoters on kinetic and recovery study of hydration separation coal mine gas[J]. Chemical Industry and Engineering Progress, 2025, 44(1): 192-201.

图/表 11

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摘要

混合热力学促进剂体系	相平衡条件		∆p/MPa
混合热力学促进剂体系	p_eq/MPa	T/K	∆p/MPa
(30%CH₄/70%N₂)THF-TBAB	0.57	282.87	2.43
(30%CH₄/70%N₂)THF-TBAF	0.57	282.9	2.43
(30%CH₄/70%N₂)CP-TBAB	0.47	283.8	2.53
(30%CH₄/70%N₂)CP-TBAF	0.42	284.49	2.58

混合热力学促进剂体系	相平衡条件		∆p/MPa
混合热力学促进剂体系	p_eq/MPa	T/K	∆p/MPa
(30%CH₄/70%N₂)THF-TBAB	0.57	282.87	2.43
(30%CH₄/70%N₂)THF-TBAF	0.57	282.9	2.43
(30%CH₄/70%N₂)CP-TBAB	0.47	283.8	2.53
(30%CH₄/70%N₂)CP-TBAF	0.42	284.49	2.58

实验编号	添加剂及摩尔分数	诱导时间 IT/min	t₉₀/min	IT时刻气体消耗量/mmol·mol^-1	IT+3h时刻气体消耗量/mmol·mol^-1	初始水合物生长速率NR₃₀/mmol·mol^-1·h^-1	水合物相中CH₄摩尔分数/%	分离因子	CH₄回收率/%
A-1	THF(5.56%)-Trp(0.06%)	2.70	54.67	0.19	26.00	0.68	54.68	6.61	67.65
A-2		1.30	55.00	0.16	25.23	0.65	53.50	6.01	66.36
A-3		1.70	40.67	0.08	30.05	0.79	49.12	4.80	67.08
均值		1.9(±0.72)	50.11(±8.18)	0.14(±0.06)	27.09(±2.59)	0.71(±0.07)	52.43(±2.93)	5.81(±0.92)	67.03(±0.65)
A-4	THF(5.56%)-TBAB(0.3%)-Trp(0.06%)	2.30	476.00	0.02	17.50	0.21	40.72	2.23	50.96
A-5		2.30	450.67	0.02	17.46	0.20	43.25	2.63	52.68
A-6		4.00	479.00	0.06	17.79	0.19	44.61	2.82	51.56
均值		2.87(±0.98)	468.56(±15.56)	0.03(±0.02)	17.58(±0.18)	0.2(±0.01)	42.86(±1.97)	2.56(±0.3)	51.73(±0.87)
A-7	THF(5.56%)-TBAF(0.3%)-Trp(0.06%)	11.00	277.00	0.04	24.65	0.15	37.25	1.89	56.68
A-8		16.70	271.67	0.05	29.36	0.30	37.02	1.97	61.55
A-9		16.70	209.00	0.02	31.17	0.19	36.75	1.91	60.93
均值		14.8(±3.29)	252.56(±37.82)	0.04(±0.02)	28.39(±3.37)	0.21(±0.08)	37.01(±0.25)	1.92(±0.04)	59.72(±2.65)
B-1	CP(5.56%)-Trp(0.06%)	16.30	61.67	0.03	9.56	0.29	77.57	12.62	39.18
B-2		14.70	65.00	0.01	12.06	0.21	65.97	6.91	40.36
B-3		12.00	68.33	0.06	10.65	0.17	72.63	10.02	42.40
均值		14.33(±2.17)	65(±3.33)	0.03(±0.03)	10.76(±1.25)	0.22(±0.06)	72.06(±5.82)	9.85(±2.86)	40.65(±1.63)
B-4	CP(5.56%)-TBAB(0.3%)-Trp(0.06%)	36.70	384.33	0.01	10.77	0.05	64.04	9.32	62.10
B-5		27.00	409.33	0.02	10.59	0.06	63.26	9.23	63.32
B-6		29.30	436.00	0.02	9.93	0.03	62.04	8.81	63.97
均值		31.00(±5.07)	409.89(±25.84)	0.02(±0.01)	10.43(±0.44)	0.05(±0.02)	63.11(±1.01)	9.12(±0.27)	63.13(±0.95)
B-7	CP(5.56%)-TBAF(0.3%)-Trp(0.06%)	11.00	423.00	0.01	15.11	0.00	70.32	15.25	68.23
B-8		16.70	641.00	0.02	16.45	0.14	65.32	12.36	70.12
B-9		16.70	467.67	0.01	10.62	0.06	63.36	10.24	67.15
均值		14.8(±3.29)	510.56(±115.15)	0.01(±0.01)	14.06(±3.05)	0.07(±0.07)	66.33(±3.59)	12.62(±2.51)	68.5(±1.50)
C	纯水	—	—	—	—	—	—	—	—

实验编号	添加剂及摩尔分数	诱导时间 IT/min	t₉₀/min	IT时刻气体消耗量/mmol·mol^-1	IT+3h时刻气体消耗量/mmol·mol^-1	初始水合物生长速率NR₃₀/mmol·mol^-1·h^-1	水合物相中CH₄摩尔分数/%	分离因子	CH₄回收率/%
A-1	THF(5.56%)-Trp(0.06%)	2.70	54.67	0.19	26.00	0.68	54.68	6.61	67.65
A-2		1.30	55.00	0.16	25.23	0.65	53.50	6.01	66.36
A-3		1.70	40.67	0.08	30.05	0.79	49.12	4.80	67.08
均值		1.9(±0.72)	50.11(±8.18)	0.14(±0.06)	27.09(±2.59)	0.71(±0.07)	52.43(±2.93)	5.81(±0.92)	67.03(±0.65)
A-4	THF(5.56%)-TBAB(0.3%)-Trp(0.06%)	2.30	476.00	0.02	17.50	0.21	40.72	2.23	50.96
A-5		2.30	450.67	0.02	17.46	0.20	43.25	2.63	52.68
A-6		4.00	479.00	0.06	17.79	0.19	44.61	2.82	51.56
均值		2.87(±0.98)	468.56(±15.56)	0.03(±0.02)	17.58(±0.18)	0.2(±0.01)	42.86(±1.97)	2.56(±0.3)	51.73(±0.87)
A-7	THF(5.56%)-TBAF(0.3%)-Trp(0.06%)	11.00	277.00	0.04	24.65	0.15	37.25	1.89	56.68
A-8		16.70	271.67	0.05	29.36	0.30	37.02	1.97	61.55
A-9		16.70	209.00	0.02	31.17	0.19	36.75	1.91	60.93
均值		14.8(±3.29)	252.56(±37.82)	0.04(±0.02)	28.39(±3.37)	0.21(±0.08)	37.01(±0.25)	1.92(±0.04)	59.72(±2.65)
B-1	CP(5.56%)-Trp(0.06%)	16.30	61.67	0.03	9.56	0.29	77.57	12.62	39.18
B-2		14.70	65.00	0.01	12.06	0.21	65.97	6.91	40.36
B-3		12.00	68.33	0.06	10.65	0.17	72.63	10.02	42.40
均值		14.33(±2.17)	65(±3.33)	0.03(±0.03)	10.76(±1.25)	0.22(±0.06)	72.06(±5.82)	9.85(±2.86)	40.65(±1.63)
B-4	CP(5.56%)-TBAB(0.3%)-Trp(0.06%)	36.70	384.33	0.01	10.77	0.05	64.04	9.32	62.10
B-5		27.00	409.33	0.02	10.59	0.06	63.26	9.23	63.32
B-6		29.30	436.00	0.02	9.93	0.03	62.04	8.81	63.97
均值		31.00(±5.07)	409.89(±25.84)	0.02(±0.01)	10.43(±0.44)	0.05(±0.02)	63.11(±1.01)	9.12(±0.27)	63.13(±0.95)
B-7	CP(5.56%)-TBAF(0.3%)-Trp(0.06%)	11.00	423.00	0.01	15.11	0.00	70.32	15.25	68.23
B-8		16.70	641.00	0.02	16.45	0.14	65.32	12.36	70.12
B-9		16.70	467.67	0.01	10.62	0.06	63.36	10.24	67.15
均值		14.8(±3.29)	510.56(±115.15)	0.01(±0.01)	14.06(±3.05)	0.07(±0.07)	66.33(±3.59)	12.62(±2.51)	68.5(±1.50)
C	纯水	—	—	—	—	—	—	—	—

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