2 kPa下均三甲苯-偏三甲苯与均三甲苯-邻甲乙苯体系二元汽液相平衡数据研究及精馏模拟

doi:10.11949/0438-1157.20210281

摘要/Abstract

摘要：

均三甲苯是一种重要的化工原料，通常存在于重整重芳烃中，其中均三甲苯与偏三甲苯、邻甲乙苯的分离较为困难。测定了2 kPa下均三甲苯(1)-偏三甲苯(2)、均三甲苯(1)-邻甲乙苯(3)两个体系的汽液相平衡数据，并分别采用NRTL和UNIQUAC活度系数模型对相平衡数据进行关联，回归获得二元交互参数，并进行了热力学一致性检验。结果表明，在2 kPa下，均三甲苯与邻甲乙苯无法通过普通精馏实现分离。通过对均三甲苯-偏三甲苯-邻甲乙苯体系进行烷基化反应，而后分别采用单塔减压精馏和双塔减压精馏对反应产物的分离进行精馏模拟，得出较优工艺为双塔连续减压精馏，两塔塔板数分别为50，回流比分别为7和8，此时均三甲苯纯度可达98%(质量)。该研究不仅补充了汽液相平衡数据库，也为低压下C₉体系的分离工艺设计提供参考。

关键词: 三甲苯, 汽液平衡, 分离, 活度系数, 流程模拟

Abstract:

1,3,5-trimethylbenzene is an important chemical raw material and usually exists in reformed heavy aromatics. It is difficult to separate 1,3,5-trimethylbenzene from 1,2,4-trimethylbenzene and 2-ethyltoluene in the C₉ aromatics mixture. The vapor-liquid equilibrium (VLE) data of 1,?3,?5-trimethylbenzene (1)?-1,?2,?4-trimethylbenzene (2) and 1,3,5-trimethylbenzene (1)-2-ethyltoluene (3) were measured at 2 kPa and then correlated by the activity coefficient models NRTL and UNIQUAC. The binary interaction parameters were obtained through regression. The thermodynamic consistency was checked as well. The results showed that 1,3,5-trimethylbenzene and 2-ethyltoluene could hardly be separated at 2 kPa by ordinary distillation. After the alkylation reaction of the ternary system (1,3,5-trimethylbenzene-1,2,4-trimethylbenzene-2-ethyltoluene), single-column and double-column distillation processes at low pressure were used to separate the reaction products by simulation, respectively. Compared to the single-column distillation process, the double-column one presented a better separation performance. The suitable separation parameters were obtained as follows: the number of stages in both columns was 50, and the reflux ratios were 7 and 8 respectively. The purity of 1,3,5-trimethylbenzene could reach 98%(mass) accordingly. This study not only fills in VLE database, but also provides a feasible method for the separation of C₉ aromatics at low pressure.

Key words: trimethylbenzene, vapor-liquid equilibria, separation, activity coefficient, process simulation

中图分类号:

TQ 013.1

徐健元, 吴艳阳, 徐菊美, 彭阳峰. 2 kPa下均三甲苯-偏三甲苯与均三甲苯-邻甲乙苯体系二元汽液相平衡数据研究及精馏模拟[J]. 化工学报, 2021, 72(9): 4504-4510.

Jianyuan XU, Yanyang WU, Jumei XU, Yangfeng PENG. Study on vapor-liquid equilibria and distillation simulation of 1,3,5-trimethylbenzene-1,2,4-trimethylbenzene and 1,3,5-trimethylbenzene-2-ethyltoluene at 2 kPa[J]. CIESC Journal, 2021, 72(9): 4504-4510.

图/表 10

表1 实验原料的沸点及Antoine常数

Table 1 Boiling points and Antoine constants of experimental materials

原料	沸点(2 kPa)/K^①	Antoine常数^②[18]			Antione常数适用的温度范围/K
原料	沸点(2 kPa)/K^①	A	B	C	Antione常数适用的温度范围/K
均三甲苯	329.41	7.07436	1569.622	209.578	322.15~466.15
偏三甲苯	332.43	7.04383	1573.267	208.564	325.15~471.15
邻甲乙苯	329.27	7.00314	1535.374	207.300	321.15~467.15

图1 改进的Rose汽液相平衡釜

Fig.1 Modified Rose vapor-liquid equilibrium still

表2 2 kPa下的汽液相平衡数据

Table 2 Vapor-liquid equilibria data at 2 kPa

T/K	$x 1$ ^①	$y 1$ ^②	$γ 1$	$γ 2$
均三甲苯(1)-偏三甲苯(2)
332.43	0.0000	0.0000	—	1.0000
332.05	0.0598	0.0759	1.1120	1.0016
331.79	0.1061	0.1329	1.1117	1.0014
331.52	0.1509	0.1875	1.1177	1.0013
331.32	0.1980	0.2404	1.1031	1.0011
331.05	0.2601	0.3076	1.0891	1.0026
330.88	0.3051	0.3547	1.0798	1.0035
330.67	0.3615	0.4096	1.0635	1.0099
330.53	0.4042	0.4507	1.0539	1.0140
330.42	0.4451	0.4872	1.0403	1.0221
330.20	0.5276	0.5623	1.0242	1.0362
329.99	0.6235	0.6485	1.0102	1.0553
329.85	0.6970	0.7155	1.0041	1.0689
329.72	0.7698	0.7830	1.0014	1.0802
329.64	0.8240	0.8345	1.0012	1.0819
329.54	0.8950	0.9016	1.0009	1.0838
329.47	0.9489	0.9523	1.0006	1.0834
329.41	1.0000	1.0000	1.0000	—
均三甲苯(1)-邻甲乙苯(3)
329.27	0.0000	0.0000	—	1.0000
329.28	0.0557	0.0554	1.0000	1.0000
329.29	0.1108	0.1104	1.0000	1.0000
329.29	0.1497	0.1493	1.0000	1.0000
329.30	0.2009	0.2002	1.0000	1.0000
329.31	0.2689	0.2680	1.0000	1.0000
329.31	0.3054	0.3044	1.0000	1.0000
329.32	0.3440	0.3425	1.0000	1.0000
329.33	0.4197	0.4181	1.0000	1.0000
329.34	0.4776	0.4758	1.0000	1.0000
329.35	0.5842	0.5825	1.0000	1.0000
329.37	0.6935	0.6924	1.0000	1.0000
329.38	0.7743	0.7737	1.0000	1.0000
329.39	0.8349	0.8345	1.0000	1.0000
329.40	0.8893	0.8890	1.0000	1.0000
329.40	0.9283	0.9280	1.0000	1.0000
329.41	1.0000	1.0000	1.0000	—

表2 2 kPa下的汽液相平衡数据

Table 2 Vapor-liquid equilibria data at 2 kPa

T/K	$x 1$ ^①	$y 1$ ^②	$γ 1$	$γ 2$
均三甲苯(1)-偏三甲苯(2)
332.43	0.0000	0.0000	—	1.0000
332.05	0.0598	0.0759	1.1120	1.0016
331.79	0.1061	0.1329	1.1117	1.0014
331.52	0.1509	0.1875	1.1177	1.0013
331.32	0.1980	0.2404	1.1031	1.0011
331.05	0.2601	0.3076	1.0891	1.0026
330.88	0.3051	0.3547	1.0798	1.0035
330.67	0.3615	0.4096	1.0635	1.0099
330.53	0.4042	0.4507	1.0539	1.0140
330.42	0.4451	0.4872	1.0403	1.0221
330.20	0.5276	0.5623	1.0242	1.0362
329.99	0.6235	0.6485	1.0102	1.0553
329.85	0.6970	0.7155	1.0041	1.0689
329.72	0.7698	0.7830	1.0014	1.0802
329.64	0.8240	0.8345	1.0012	1.0819
329.54	0.8950	0.9016	1.0009	1.0838
329.47	0.9489	0.9523	1.0006	1.0834
329.41	1.0000	1.0000	1.0000	—
均三甲苯(1)-邻甲乙苯(3)
329.27	0.0000	0.0000	—	1.0000
329.28	0.0557	0.0554	1.0000	1.0000
329.29	0.1108	0.1104	1.0000	1.0000
329.29	0.1497	0.1493	1.0000	1.0000
329.30	0.2009	0.2002	1.0000	1.0000
329.31	0.2689	0.2680	1.0000	1.0000
329.31	0.3054	0.3044	1.0000	1.0000
329.32	0.3440	0.3425	1.0000	1.0000
329.33	0.4197	0.4181	1.0000	1.0000
329.34	0.4776	0.4758	1.0000	1.0000
329.35	0.5842	0.5825	1.0000	1.0000
329.37	0.6935	0.6924	1.0000	1.0000
329.38	0.7743	0.7737	1.0000	1.0000
329.39	0.8349	0.8345	1.0000	1.0000
329.40	0.8893	0.8890	1.0000	1.0000
329.40	0.9283	0.9280	1.0000	1.0000
329.41	1.0000	1.0000	1.0000	—

图2 均三甲苯(1)-偏三甲苯(2)体系lnγ1γ2-x1图

Fig.2 lnγ1γ2-x1 for 1,3,5-trimethylbenzene (1) - 1,2,4-trimethylbenzene (2)

图3 均三甲苯(1)-邻甲乙苯(3)体系lnγ1γ3-x1图

Fig.3 lnγ1γ3-x1 for 1,3,5-trimethylbenzene (1) - 2-ethyltoluene (3)

表3 2 kPa下系统活度系数模型参数关联及回归偏差

Table 3 Activity coefficient parameters correlation and regression deviation at 2 kPa

模型	模型参数					AAD
模型	$a i j$	$a j i$	$b i j$	$b j i$	$c i j$	$? T$ /K	$? p$ /kPa	$? x 1$	$? y 1$
均三甲苯(1)-偏三甲苯(2)
NRTL	6.6444	-1.8407	-2160.15	613.62	0.3	0.020	4.73×10^-7	2.15×10^-5	0.0025
UNIQUAC	-3.8399	2.6059	1254.69	-856.9	—	0.020	4.76×10^-7	2.14×10^-5	0.0025
均三甲苯(1)-邻甲乙苯(3)
NRTL	-7.4030	7.7726	2411.95	-2533.05	0.3	0.003	1.04×10^-9	1.43×10^-5	0.0064
UNIQUAC	0.0884	-0.0830	-35.97	34.13	—	0.003	1.03×10^-9	1.43×10^-5	0.0064

表3 2 kPa下系统活度系数模型参数关联及回归偏差

Table 3 Activity coefficient parameters correlation and regression deviation at 2 kPa

模型	模型参数					AAD
模型	$a i j$	$a j i$	$b i j$	$b j i$	$c i j$	$? T$ /K	$? p$ /kPa	$? x 1$	$? y 1$
均三甲苯(1)-偏三甲苯(2)
NRTL	6.6444	-1.8407	-2160.15	613.62	0.3	0.020	4.73×10^-7	2.15×10^-5	0.0025
UNIQUAC	-3.8399	2.6059	1254.69	-856.9	—	0.020	4.76×10^-7	2.14×10^-5	0.0025
均三甲苯(1)-邻甲乙苯(3)
NRTL	-7.4030	7.7726	2411.95	-2533.05	0.3	0.003	1.04×10^-9	1.43×10^-5	0.0064
UNIQUAC	0.0884	-0.0830	-35.97	34.13	—	0.003	1.03×10^-9	1.43×10^-5	0.0064

图4 均三甲苯(1)-偏三甲苯(2)体系的模拟值(NRTL模型)与实验值对比

Fig.4 Comparison of the VLE data from experimental data and regression data by NRTL for the system of 1,3,5-trimethylbenzene (1) - 1,2,4-trimethylbenzene (2) at 2 kPa

图5 均三甲苯(1)-邻甲乙苯(3)体系的模拟值(NRTL模型)与实验值对比

Fig.5 Comparison of the VLE data from experimental data and regression data by NRTL for the system of 1,3,5-trimethylbenzene (1) - 2-ethyltoluene (3) at 2 kPa

图6 精馏模拟流程图

Fig.6 Diagram of distillation

表4 精馏塔参数

Table 4 Parameters of distillation columns

参数	单塔减压精馏	双塔连续减压精馏
参数	T11	T21	T22
塔顶压力/kPa	2	2	2
塔板数n	120	50	50
回流比R	12	7	8
塔顶采出率	0.70	0.65	0.60
再沸器热负荷Q_R/kW	97.4296	56.8002	37.1880

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