Zn/NaHZSM-5沸石在C5～C8链烷烃芳构化反应中的催化性能

doi:10.11949/0438-1157.20190021

摘要/Abstract

摘要：

采用氨气程序升温脱附（NH₃-TPD）、紫外-可见光谱和小型固定床反应器，重点研究了碱金属钠离子和过渡金属锌离子改性对纳米H-ZSM-5沸石表面酸性及其催化C₅～C₈链烷烃芳构化反应性能的影响。结果表明，用碱金属钠离子改性能够有效地消除沸石表面的强酸中心，适当降低催化剂表面酸量，从而减少甲烷、乙烷和丙烷等低值副产物的生成，优化芳构化反应产物分布。适宜的Zn²⁺负载量为3%（质量分数），过高的Zn²⁺负载量会使产物中干气生成量增大，不利于芳烃收率的提高。C₅～C₈链烷烃芳构化的适宜反应温度为530℃。

关键词: 链烷烃, 芳构化, 纳米H-ZSM-5, 酸性, 碱金属离子改性

Abstract:

Ammonia gas temperature programmed desorption (NH₃-TPD), UV-visible spectroscopy and small fixed-bed reactor were used to study the surface acidity of nano-H-ZSM-5 zeolite modified by alkali metal sodium ion and transition metal zinc ion. The results showed that alkali metal ion Na⁺ modification can effectively eliminate the strong acid sites and reduce the acid amount of the zeolite, which consequently optimized the products distribution of aromatization process by suppressing the production of low-value by-products like methane, ethane or propane. The optimum Zn loading for aromatics production was 3% (mass), while further increasing Zn loadings resulted in high yield of dry gas. The suitable reaction temperature for C₅－C₈ alkanes aromatization was 530℃.

Key words: chain-alkanes, aromatization, nano-sized H-ZSM-5, acidity, alkali metal ion modification

中图分类号:

TQ 028.8

赵云, 刘春燕, 刘家旭, 贺宁, 郭洪臣. Zn/NaHZSM-5沸石在C₅～C₈链烷烃芳构化反应中的催化性能[J]. 化工学报, 2019, 70(6): 2182-2191.

Yun ZHAO, Chunyan LIU, Jiaxu LIU, Ning HE, Hongchen GUO. Catalytic performance of Zn/NaHZSM-5 zeolite for C₅－C₈ chain-alkanes aromatization[J]. CIESC Journal, 2019, 70(6): 2182-2191.

图/表 11

表1 重整抽余油的组成

Table 1 Composition of raffinate oil/%(mass)

组成	正构烷烃	异构烷烃	烯烃	环烷烃	芳烃	总和
C₄	0.01	0	0	0	0	0.01
C₅	3.66	1.46	0.12	3.41	0	8.65
C₆	12.43	30.65	2.35	1.77	0	47.20
C₇	6.59	25.40	0.25	0.67	0.27	33.18
C₈	1.67	8.01	0.01	0.56	0	10.25
C₉	0	0.71	0	0	0	0.71
总和	24.36	66.23	2.73	6.41	0.27	100

表2 Na+和Zn2+改性纳米H-ZSM-5沸石的相对酸量分布

Table 2 Relative acid amount of nano-sized H-ZSM-5 zeolites modified by Na+ and Zn2+

样品	弱酸	强酸	总酸
HZSM-5	0.72	0.28	1
Zn₃	0.75	0.24	0.99
Na_0.2	0.81	0.18	0.99
Na_0.8	0.95	0.05	1
Na_1.5	0.96	0.04	1
Na_2.0	0.92	0.01	0.93
Na_0.2Zn₃	0.86	0.12	0.98
Na_0.8Zn₃	0.87	0.10	0.97
Na_1.5Zn₃	0.86	0.09	0.95
Na_2.0Zn₃	0.80	0.07	0.87
Zn₃Na_0.2	0.78	0.11	0.89
Zn₃Na_0.8	0.76	0.08	0.84
Zn₃Na_1.5	0.74	0.05	0.79
Zn₃Na_2.0	0.64	0.04	0.68

图1 C5~C8链烷烃芳构化反应过程中甲烷、乙烷和丙烷等副产物的生成途径

Fig.1 Product pathway of methane, ethane or propane during aromatization process of C5－C8 chain-alkanes

表3 Na+、Zn2+改性纳米H-ZSM-5沸石上C5~C8链烷烃的芳构化反应产物分布

Table 3 Products distribution of aromatization of C5－C8 chain alkanes over

Item	HZSM-5	Zn₃	Na_0.8Zn₃	Na_1.5Zn₃	Na_2.0Zn₃	Zn₃Na_0.8	Zn₃Na_1.5	Zn₃Na_2.0
X	99.89	98.98	95.97	93.05	92.38	97.89	85.30	76.83
Y(A)	47.83	51.57	47.49	47.58	47.5	51.63	43.24	37.34
S(A)	47.88	52.10	49.48	51.13	51.42	52.74	50.69	48.60
S(C₁～C₂)	27.71	25.95	23.09	16.80	14.98	13.09	12.53	12.35
S(C₃⁰)	21.82	19.23	19.66	18.27	17.66	20.04	17.06	14.97
S(A)/[S(C₁～C₂) + S( $C 30$ )]	0.97	1.15	1.16	1.46	1.58	1.59	1.71	1.78
产物分布
甲烷	13.23	11.91	8.40	7.61	5.72	5.52	4.14	3.67
乙烷	14.27	13.48	13.32	7.15	7.06	6.18	5.01	3.90
乙烯	0.18	0.30	0.44	0.87	1.06	1.11	1.54	1.92
丙烷	21.80	19.03	18.87	17.00	16.31	19.62	14.55	11.50
丙烯	0.10	0.35	0.79	1.58	1.82	1.68	2.84	3.88
丁烷	2.07	1.60	4.49	8.79	9.81	8.98	9.89	7.57
丁烯	0.05	0.18	0.29	0.69	0.90	0.67	1.18	1.61
苯	7.18	10.30	8.24	7.04	6.36	6.72	4.66	3.45
甲苯	22.32	24.31	21.28	21.59	20.19	24.69	17.82	15.06
C₈芳烃	12.75	12.49	13.96	14.23	15.48	14.38	14.34	12.65
C₉₊芳烃	5.58	4.47	4.01	4.72	5.47	5.84	6.42	6.18
C₅₊非芳烃	0.48	1.58	5.90	8.74	9.83	4.60	17.62	28.60
总和	100	100	100	100	100	100	100	100

表3 Na+、Zn2+改性纳米H-ZSM-5沸石上C5~C8链烷烃的芳构化反应产物分布

Table 3 Products distribution of aromatization of C5－C8 chain alkanes over

Item	HZSM-5	Zn₃	Na_0.8Zn₃	Na_1.5Zn₃	Na_2.0Zn₃	Zn₃Na_0.8	Zn₃Na_1.5	Zn₃Na_2.0
X	99.89	98.98	95.97	93.05	92.38	97.89	85.30	76.83
Y(A)	47.83	51.57	47.49	47.58	47.5	51.63	43.24	37.34
S(A)	47.88	52.10	49.48	51.13	51.42	52.74	50.69	48.60
S(C₁～C₂)	27.71	25.95	23.09	16.80	14.98	13.09	12.53	12.35
S(C₃⁰)	21.82	19.23	19.66	18.27	17.66	20.04	17.06	14.97
S(A)/[S(C₁～C₂) + S( $C 30$ )]	0.97	1.15	1.16	1.46	1.58	1.59	1.71	1.78
产物分布
甲烷	13.23	11.91	8.40	7.61	5.72	5.52	4.14	3.67
乙烷	14.27	13.48	13.32	7.15	7.06	6.18	5.01	3.90
乙烯	0.18	0.30	0.44	0.87	1.06	1.11	1.54	1.92
丙烷	21.80	19.03	18.87	17.00	16.31	19.62	14.55	11.50
丙烯	0.10	0.35	0.79	1.58	1.82	1.68	2.84	3.88
丁烷	2.07	1.60	4.49	8.79	9.81	8.98	9.89	7.57
丁烯	0.05	0.18	0.29	0.69	0.90	0.67	1.18	1.61
苯	7.18	10.30	8.24	7.04	6.36	6.72	4.66	3.45
甲苯	22.32	24.31	21.28	21.59	20.19	24.69	17.82	15.06
C₈芳烃	12.75	12.49	13.96	14.23	15.48	14.38	14.34	12.65
C₉₊芳烃	5.58	4.47	4.01	4.72	5.47	5.84	6.42	6.18
C₅₊非芳烃	0.48	1.58	5.90	8.74	9.83	4.60	17.62	28.60
总和	100	100	100	100	100	100	100	100

图2 改性纳米H-ZSM-5沸石的反应性能与酸量的关联

Fig.2 Correlations between reaction performance and acid amount of modified nano-sized H-ZSM-5 zeolites

图3 不同Zn2+负载量改性纳米H-ZSM-5沸石的NH3-TPD结果

Fig.3 NH3-TPD profiles of modified nano-sized H-ZSM-5 with different Zn2+ loading

图4 不同Zn2+负载量改性纳米H-ZSM-5沸石的紫外可见谱图

Fig.4 UV-visible absorption spectra of modified nano-sized H-ZSM-5 with different Zn2+ loading

图5 改性纳米H-ZSM-5沸石（ZnyNa0.8）的反应性能与Zn2+负载量的关联

Fig.5 Correlation between reaction performance and Zn2+ loading of modified nano-sized H-ZSM-5 zeolite (ZnyNa0.8)

表4 不同Zn2+负载量纳米H-ZSM-5沸石上C5~C8链烷烃芳构化反应的产物分布

Table 4 Products distribution of aromatization of C5－C8 chain alkanes over modified nano-sized H-ZSM-5 zeolite with different Zn2+ loading/%(mass)

Item	Zn_1.5Na_0.8	Zn₃Na_0.8	Zn₆Na_0.8	Zn₉Na_0.8
X	95.28	97.89	95.33	94.85
Y(A)	46.95	51.63	44.78	44.16
S(A)	49.28	52.74	46.97	46.56
S(C₁~C₂)	12.98	13.09	18.16	18.70
S(C⁰₃)	22.09	20.04	18.46	18.22
S(A)/[S(C₁～C₂) + S( $C 30$ )]	1.40	1.59	1.28	1.26
产物分布
甲烷	5.10	5.52	6.47	6.35
乙烷	6.07	6.18	10.02	10.65
乙烯	1.20	1.11	0.82	0.74
丙烷	21.05	19.62	17.60	17.28
丙烯	1.79	1.68	1.60	1.66
丁烷	7.79	8.98	8.78	8.55
丁烯	0.58	0.67	0.64	0.71
苯	6.68	6.72	6.57	6.31
甲苯	21.21	24.69	18.87	18.11
C₈芳烃	13.42	14.38	14.43	14.91
C₉₊芳烃	5.64	5.84	4.91	4.83
C₅₊非芳烃	9.47	4.60	9.29	9.90
总和	100	100	100	100

表4 不同Zn2+负载量纳米H-ZSM-5沸石上C5~C8链烷烃芳构化反应的产物分布

Table 4 Products distribution of aromatization of C5－C8 chain alkanes over modified nano-sized H-ZSM-5 zeolite with different Zn2+ loading/%(mass)

Item	Zn_1.5Na_0.8	Zn₃Na_0.8	Zn₆Na_0.8	Zn₉Na_0.8
X	95.28	97.89	95.33	94.85
Y(A)	46.95	51.63	44.78	44.16
S(A)	49.28	52.74	46.97	46.56
S(C₁~C₂)	12.98	13.09	18.16	18.70
S(C⁰₃)	22.09	20.04	18.46	18.22
S(A)/[S(C₁～C₂) + S( $C 30$ )]	1.40	1.59	1.28	1.26
产物分布
甲烷	5.10	5.52	6.47	6.35
乙烷	6.07	6.18	10.02	10.65
乙烯	1.20	1.11	0.82	0.74
丙烷	21.05	19.62	17.60	17.28
丙烯	1.79	1.68	1.60	1.66
丁烷	7.79	8.98	8.78	8.55
丁烯	0.58	0.67	0.64	0.71
苯	6.68	6.72	6.57	6.31
甲苯	21.21	24.69	18.87	18.11
C₈芳烃	13.42	14.38	14.43	14.91
C₉₊芳烃	5.64	5.84	4.91	4.83
C₅₊非芳烃	9.47	4.60	9.29	9.90
总和	100	100	100	100

图6 改性纳米H-ZSM-5沸石（Zn3Na0.8）的反应性能与反应温度的关联

Fig.6 Correlation between reaction performance of modified nano-sized H-ZSM-5 (Zn3Na0.8) and reaction temperatures

表5 不同反应温度下改性纳米H-ZSM-5(Zn3Na0.8)沸石上C5~C8链烷烃芳构化反应的产物分布

Table 5 Products distribution of aromatization of C5－C8 chain alkanes over modified nano-sized H-ZSM-5 zeolite (Zn3Na0.8) at different temperatures/%(mass)

Item	490℃	510℃	530℃	550℃	570℃
X	93.25	94.59	97.89	98.02	98.44
Y(A)	47.58	47.05	51.63	51.11	51.92
S(A)	51.02	49.74	52.74	52.14	52.74
S(C₁~C₂)	9.93	11.62	13.09	17.27	18.53
S(C₃⁰)	24.28	23.85	20.04	17.92	16.63
S(A)/[S(C₁~C₂) + S( $C 30$ )]	1.49	1.40	1.59	1.48	1.50
产物分布
甲烷	3.90	4.89	5.52	7.01	7.66
乙烷	4.66	5.22	6.18	8.42	9.04
乙烯	0.70	0.88	1.11	1.50	1.54
丙烷	22.64	22.56	19.62	17.57	16.37
丙烯	1.17	1.35	1.68	2.33	2.41
丁烷	8.96	10.33	8.98	7.96	6.95
丁烯	0.43	0.48	0.67	0.98	0.72
苯	4.74	5.68	6.72	8.46	9.92
甲苯	20.52	21.49	24.69	23.70	23.42
C₈芳烃	15.19	14.30	14.38	14.06	14.10
C₉₊芳烃	7.13	5.58	5.84	4.89	4.48
C₅₊非芳烃	9.96	7.25	4.60	3.11	3.39
总和	100	100	100	100	100

表5 不同反应温度下改性纳米H-ZSM-5(Zn3Na0.8)沸石上C5~C8链烷烃芳构化反应的产物分布

Table 5 Products distribution of aromatization of C5－C8 chain alkanes over modified nano-sized H-ZSM-5 zeolite (Zn3Na0.8) at different temperatures/%(mass)

Item	490℃	510℃	530℃	550℃	570℃
X	93.25	94.59	97.89	98.02	98.44
Y(A)	47.58	47.05	51.63	51.11	51.92
S(A)	51.02	49.74	52.74	52.14	52.74
S(C₁~C₂)	9.93	11.62	13.09	17.27	18.53
S(C₃⁰)	24.28	23.85	20.04	17.92	16.63
S(A)/[S(C₁~C₂) + S( $C 30$ )]	1.49	1.40	1.59	1.48	1.50
产物分布
甲烷	3.90	4.89	5.52	7.01	7.66
乙烷	4.66	5.22	6.18	8.42	9.04
乙烯	0.70	0.88	1.11	1.50	1.54
丙烷	22.64	22.56	19.62	17.57	16.37
丙烯	1.17	1.35	1.68	2.33	2.41
丁烷	8.96	10.33	8.98	7.96	6.95
丁烯	0.43	0.48	0.67	0.98	0.72
苯	4.74	5.68	6.72	8.46	9.92
甲苯	20.52	21.49	24.69	23.70	23.42
C₈芳烃	15.19	14.30	14.38	14.06	14.10
C₉₊芳烃	7.13	5.58	5.84	4.89	4.48
C₅₊非芳烃	9.96	7.25	4.60	3.11	3.39
总和	100	100	100	100	100

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Zn/NaHZSM-5沸石在C₅～C₈链烷烃芳构化反应中的催化性能

Catalytic performance of Zn/NaHZSM-5 zeolite for C₅－C₈ chain-alkanes aromatization

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