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乙酸乙酯和乙腈萃取精馏模拟优化综述

时间：2020/10/15 9:10:22  作者：  来源：  查看：0  评论：0
内容摘要： 摘 要 乙酸乙酯和乙腈萃取精馏采用的溶剂具有沸点高、相对不易挥发,并与其他组分不易形成络合物的特点。随着萃取溶剂探索方法的发展、乙酸乙酯和乙腈萃取精馏系统的进一步优化及高效设备的采用提高了乙酸乙酯和乙腈萃取精馏系统的适用性、可控制性和操作性,使其与其他精密分离技...
摘 要
 
乙酸乙酯和乙腈萃取精馏采用的溶剂具有沸点高、相对不易挥发,并与其他组分不易形成络合物的特点。随着萃取溶剂探索方法的发展、乙酸乙酯和乙腈萃取精馏系统的进一步优化及高效设备的采用提高了乙酸乙酯和乙腈萃取精馏系统的适用性、可控制性和操作性,使其与其他精密分离技术和液液萃取技术相比,显示出了越来越明显的优越性。本文采用化工过程模拟软件Aspen Plus 11.1对乙酸乙酯-乙腈体系的萃取精馏过程进行了优化，结果表明，常压下，当萃取精馏塔的理论塔板数为36，萃取剂进口位置（从上向下数）为5，原料进口位置为29，回流比为3.8，萃取剂与原料液质量流量之比为6:1时，塔顶馏出物中乙酸乙酯的质量分数可达到99.90％ 。
 
关键词：乙酸乙酯-乙腈体系、萃取精馏、萃取剂、二甲基亚砜、Aspen Plus
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
Abstract
 
The solvent used in the extraction and distillation of ethyl acetate and acetonitrile has the characteristics of high boiling point, relatively less volatile and less complex with other components. With the development of extraction solvent exploration methods, the further optimization of ethyl acetate and acetonitrile extraction distillation system and the use of high efficiency equipment have improved the suitability, controllability and operability of ethyl acetate and acetonitrile extraction distillation system. Compared with other precision separation technology and liquid-liquid extraction technology, showing more and more obvious advantages. In this paper, the extraction process of ethyl acetate-acetonitrile system was optimized by chemical process simulation software Aspen Plus 11.1. The results showed that the theoretical plate number of extractive distillation column was 36, From the top down) is 5, the raw material inlet position is 29, the reflux ratio is 3.8, the ratio of the mass ratio of the extractant to the raw material is 6: 1, the mass fraction of the ethyl acetate in the overhead can reach 99.90 %.
 
Key words: ethyl acetate - acetonitrile system, extractive distillation, extractant, dimethyl sulfoxide, Aspen Plus
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 


1．引言

乙腈不仅是一种重要的化工原料，同时也是一种重要的有机溶剂，因其对无机以及有机化合物的优良溶解性而被广泛使用，在溶剂回收的过程中经常遇到乙腈和水的分离问题。
乙酸乙酯-乙腈体系是共沸物系，不能采用常规精馏方法进行分离。常压下，乙腈沸点为81.1℃，共沸物组成 85.8%（wt）。乙酸乙酯-乙腈体系的分离工艺主要有变压精馏、盐效萃取与精馏联合工艺、萃取精馏及渗透蒸发等。而萃取精馏特别适合于近沸点和共沸物体系。
本文采用原料废乙腈来自于2-甲基吡啶的生产过程所产生的乙腈和乙酸乙酯所形成混合物，其组成主要为乙酸乙酯和乙腈，分离的关键在于乙腈与乙酸乙酯的分离。该法采用二甲基亚砜作为溶剂对理论塔板数N、萃取剂进口位置N1（从上往下数，下同）、原料进口位置N2、溶剂比（即萃取剂与原料的流量之比）QS/QF、回流比R等操作参数进行了优化。萃取精馏过程为双塔流程，流程图如图1-1所示：
图1-1 萃取精馏模拟流程

2. 萃取精馏塔优化

2.1优化过程

拟优化的参数：塔板数N、萃取剂进口位置N1、原料进口位置N2、溶剂比QS/QF 、回流比R；目标函数均为塔顶产品组成XD。

2.1.1 理论塔板数的优化

以塔板数N（N≥2）为变量函数，以塔顶产品组成XD为目标函数进行优化。结果如图2-1所示。
 
图2-1 理论塔板数对塔顶组成的影响
由图2-1可知，当塔板数N≤34时，随着N的增加，塔顶产品的组成XD大体明显增加（除第4块板和第8块板外，因二者为物流进口位置）；当塔板数N≥35时，随着N的增加，塔顶产品的组成X虽有所增加，但变化甚微，X几乎保持在98.79%不变。由于增加塔板数对提高产品纯度没有太大的意义，此外，考虑到增加塔高不仅会提高设备成本，而且会增加能耗，权衡产品纯度要求与成本二者之间的关系，建议最佳的塔板数应选36。

2.1.2 萃取剂进料位置的优化

在上述优化的基础上，将塔板数N改设为36，以萃取剂进口位置N1为变量参数，以塔顶产品组成XD为目标函数，其他操作参数保持不变，进一步优化，结果如图2-2所示。
 
 
 
 
 
图2-2 溶剂进料位置对塔顶组成的影响
由图2-2可知，当萃取剂进口N1位于第5块板时，塔顶产品的组成XD达到最大值99.95%；随着N1的增大，X无明显变化，直至N1为13时；当N1≥13时，X 呈明显的下降趋势。由此可知，萃取剂的最佳进口位置为第5块板。

2.1.3 原料进料位置的优化

同理，将萃取剂进口位置N1改设为5，以原料进口位置N2为变量，以塔顶产品组成XD为目标函数，其他操作参数保持不变，继续进行优化，结果如图2-3所示:
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
 
图2-3 原料进料位置对塔顶组成的影响
    由图2-3可知：当原料进口位置N2≤20时，塔顶产品的组成XD随原料进口位置N2的增大呈明显的上升趋势；当N2≥30时，X明显下降。当20≤N2≤30时X几乎保持在99.80%不变。由此可知，原料的最佳进口位置为第29块板。

2.1.4 溶剂比的优化

在上述优化基础上，将原料进口位置N2改设为29，以萃取剂流量QS为变量，以塔顶产品乙酸乙酯组成XD为目标函数，其他操作参数保持不变，继续优化，结果如图2-4所示。
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
 
 
图2-4 溶剂进料量对塔顶组成的影响
由图2-4可知：当萃取剂流量QS≤600kg/hr时，随QS的增加，塔顶产品组成XD明显增大；当QS≥600kg/hr时，X增加幅度甚小，几乎保持在99.75%不变。考虑到萃取剂流量过大对提高塔顶产品纯度的意义不大，且造成萃取剂的后续回收工作量增大（萃取剂流量由于原料流量QF 为100kg/hr由生产量决定），故最佳溶剂比QS/QF应为6:1。

2.1.5 回流比的优化

在上述优化基础上，将萃取剂流量QS改设为600kg/hr ，以回流比R为变量，以塔顶产品乙酸乙酯组成XD为目标函数，其他操作参数保持不变，继续优化，结果如图2-5所示。
 
 
 
 
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
 
 
 
图2-5 塔顶产品组成随回流比的变化关系
    由图2-5可知，当回流比R在1.0-6.0之间时，塔顶产品组成XD基本保持最高值不变。因此将回流比定为3.8。2.2萃取精馏塔优化结果塔内气液相组成分布，温度分布分别见表2-1，表2-2和表2-3。
表2-1 萃取精馏塔内气相组成分布
塔板数  
乙酸乙酯
乙腈
二甲基亚砜       
1
0.9968
0.0032
2.36E-06
2
0.9987
0.0013
2.92E-05
3
0.9990
0.0006
0.0003
4
0.9966
0.0005
0.0028
5
0.9694
0.0004
0.0302
6
0.9691
0.0007
0.0301
7
0.9688
0.0010
0.0301
8
0.9684
0.0015
0.0301
9
0.9678
0.0020
0.0301
10
0.9671
0.0028
0.0301
11
0.9662
0.0038
0.0301
12
0.9649
0.0050
0.0301
13
0.9633
0.0067
0.0300
14
0.9612
0.0088
0.0300
15
0.9585
0.0116
0.0299
16
0.9549
0.0152
0.0299
17
0.9502
0.0100
0.0298
18
0.9440
0.0263
0.0297
19
0.9359
0.0345
0.0295
20
0.9251
0.0455
0.0294
21
0.9107
0.0601
0.0292
22
0.8914
0.0797
0.0289
23
0.8651
0.1062
0.0286
24
0.8292
0.1424
0.0284
25
0.7798
0.1919
0.0283
26
0.7126
0.2589
0.0285
27
0.6241
0.3465
0.0294
28
0.5177
0.4520
0.0303
29
0.4096
0.5653
0.0250
30
0.2667
0.7053
0.0279
31
0.1480
0.8213
0.0306
32
0.0727
0.8946
0.0326
33
0.0332
0.9324
0.0344
34
0.0145
0.9434
0.0422
35
0.0059
0.8893
0.1048
36
0.0016
0.5474
0.4509
 
萃取精馏塔内气相组成分布图如下：
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
图2-6  萃取精馏塔内气相组成分布
表2-2萃取精馏塔内液相组成分布
塔板数
乙酸乙酯
乙腈
二甲基亚砜
1
0.99877
0.0012
2.92E-05
2
0.99919
0.00055
0.0003
3
0.99618
0.0003
0.0036
4
0.9610
0.0002
0.0386
5
0.4037
0.0003
0.5960
6
0.4035
0.0004
0.5960
7
0.40332
0.0006
0.5960
8
0.4030
0.0009
0.5960
9
0.4027
0.0012
0.5960
10
0.4022
0.0017
0.5960
11
0.4017
0.0023
0.5960
12
0.4009
0.0030
0.5960
13
0.3999
0.0040
0.5960
14
0.3986
0.0053
0.5960
15
0.3969
0.0070
0.5959
16
0.3948
0.0093
0.5959
17
0.3919
0.0122
0.5959
18
0.3881
0.0160
0.5959
19
0.3829
0.0211
0.5958
20
0.3762
0.0279
0.5958
21
0.3671
0.0371
0.5958
22
0.3547
0.0494
0.5959
23
0.3377
0.0663
0.5959
24
0.3146
0.0893
0.5961
25
0.2832
0.1204
0.5963
26
0.2422
0.1613
0.5965
27
0.1934
0.2110
0.5955
28
0.1455
0.2668
0.5877
29
0.1170
0.3525
0.5305
30
0.0657
0.4068
0.5275
31
0.0326
0.4429
0.5244
32
0.0150
0.4621
0.5229
33
0.0066
0.4668
0.5266
34
0.0026
0.4335
0.5638
35
0.0007
0.2698
0.7295
36
9.95E-05
0.0768
0.9231
 
乙酸乙酯和乙腈萃取精馏模拟优化综述萃取精馏塔内液相组成分布图如下：
 
 
 
 
 
 
 
 
 
 
 
图2-7 萃取精馏塔内液相组成分布
表2-3萃取精馏塔温度分布
塔板数
温度（℃）
塔板数
温度（℃）
塔板数
温度（℃）
 
1
80.06
13
96.38
25
96.59
 
2
80.11
14
96.37
26
97.24
 
3
80.22
15
96.36
27
98.44
 
4
81.24
16
96.35
28
99.83
 
5
96.41
17
96.33
29
97.87
 
6
96.41
18
96.30
30
100.84
 
7
96.41
19
96.28
31
103.36
 
8
96.41
20
96.25
32
104.98
 
9
96.40
21
96.22
33
106.15
 
10
96.40
22
96.19
34
109.48
 
11
96.39
23
96.21
35
126.70
 
12
96.39
24
96.31
36
164.36
 
 
萃取精馏塔温度分布图如下
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
 
 
图2-7 萃取精馏塔温度分布图

3.溶剂回收塔的优化

3.1优化过程

 拟优化的参数：塔板数N’、萃取剂进口位置N1’、原料进口位置N2’、溶剂比QS’/QF’ 、回流比R’；目标函数均为塔顶产品组成XD。

3.1.1塔板数的优化

以塔板数N'（N'≥2）为变量函数，以塔顶产品组成XD'为目标函数进行优化。结果如图3-1所示。
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
图3-1理论塔板数对塔顶组成的影响
  由图3-1可知，当塔板数15≤N≤20时，随着N的增加，塔顶产品的组成X大体明显增加；当塔板数4≤N≤15时，随着N的增加，塔顶产品的组成X变化甚微，当N≥20时X几乎保持在99.84%不变。由于增加塔板数对于提高产品纯度没有太大的意义，此外，考虑到增加塔高不仅会提高设备成本，而且会增加能耗，权衡产品纯度要求与成本二者之间的关系，建议最佳的塔板数应选20。

3.1.2进料位置的优化

乙酸乙酯和乙腈萃取精馏模拟优化综述在上述优化的基础上，将塔板数N′改设为20，以原料进口位置N1′为变量参数，以塔顶产品组成XD′为目标函数，其他操作参数保持不变，进一步优化，结果如图3-2所示。
 
 
 
 
 
 
 
 
 
 
图3-2 进料位置对塔顶组成的影响
由图3-2可知：当原料进口位置3≤N2≤17时，塔顶产品的组成X′基本不发生变化，选用原料的进口位置为第10块板。

3.1.3回流比的优化

 在上述优化基础上，以回流比R′为变量，以塔顶产品乙腈组成X′为目标函数，其他操作参数保持不变，继续优化，结果如图3-3所示。由图3-3可知，当回流比R在1.0~20.0之间时，塔顶产品组成X基本保持最高值不变。因为回流比的增加直接导致成本地 增加，权衡利弊将回流比设为1.5。
 
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
 
图3-3 回流比对塔顶组成的影响

3.2 溶剂回收塔优化结果

塔内气液相组成分布，温度分布分别见表3-1，表3-2和表3-3。
表3-1回收塔内气相组成分布
塔板数
乙酸乙酯
乙腈
二甲基亚砜
1
0.0033
0.9967
1.96E-06
2
0.0013
0.9986
8.93E-05
3
0.0008
0.9967
0.0024
4
0.0007
0.9457
0.0536
5
0.0003
0.9461
0.0536
6
0.0001
0.9463
0.0536
7
4.53E-05
0.9464
0.0536
8
1.79E-05
0.9464
0.0536
9
7.09E-06
0.9464
0.0537
10
2.80E-06
0.9461
0.0539
11
1.11E-06
0.9447
0.0553
12
4.35E-07
0.9357
0.0643
13
1.63E-07
0.8816
0.1183
14
4.85E-08
0.6471
0.3529
15
8.50E-09
0.2624
0.7376
6
9.81E-10
0.0663
0.9337
17
9.84E-11
0.0142
0.9857
18
9.55E-12
0.0029
0.9970
19
9.17E-13
0.0006
0.9994
20
8.38E-14
0.0001
0.9999
 
回收塔内气相组成分布图如下：
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
 
 
图3-4 回收塔内气相组成分布图
 
表3-2回收塔内液相组成分布
塔板数
乙酸乙酯
乙腈
二甲基亚砜
1
0.0013
0.9986
8.93E-05
2
0.0005
0.9955
0.0040
3
0.0003
0.9045
0.0952
4
0.0001
0.3915
0.6084
5
4.74E-05
0.3916
0.6083
6
1.87E-05
0.3916
0.6083
7
7.42E-06
0.3916
0.6083
8
2.93E-06
0.3916
0.6083
9
1.16E-06
0.3915
0.6084
10
4.58E-07
0.3907
0.6092
11
1.79E-07
0.3856
0.6143
12
6.59E-08
0.3569
0.6431
13
1.89E-08
0.2515
0.7485
14
3.37E-09
0.1039
0.8961
15
4.14E-10
0.0280
0.9720
16
4.27E-11
0.0062
0.9938
17
4.18E-12
0.0013
0.9987
18
4.03E-13
0.0003
0.9997
19
3.87E-14
5.36E-05
0.9999
20
3.53E-15
9.87E-06
0.99999
 
回收塔内液相分布图如下：
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
 
 
图3-5 回收塔液相分布图
 
表3-3 回收塔各层温度分布
塔板数
温度（℃）
塔板数
温度（℃）
1
81.41
11
114.19
2
81.58
12
116.93
3
84.71
13
129.37
4
113.63
14
157.12
5
113.64
15
180.12
6
113.65
16
188.28
7
113.65
17
190.22
8
113.65
18
190.63
9
113.66
19
190.72
10
113.74
20
190.73
 
乙酸乙酯和乙腈萃取精馏模拟优化综述 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 

4 结论

   （1） 在常压下，二甲基亚枫作为萃取剂可以消除乙酸乙酯-乙腈共沸物系的共沸点，提高乙酸乙酯-乙腈体系的相对挥发度。
   （2）由优化结果可知：在常压下，以二甲基亚砜为萃取剂分离乙酸乙酯-乙腈时，优化的操作参数为：塔板数36，萃取剂进口位置为第5块板，原料进口位置为第29块板，溶剂比为6:1，回流比为3.8。优化后塔顶乙腈纯度可达99.67%。塔底二甲基亚砜的纯度可达99.99%。
（3）本优化过程可以为乙酸乙酯-乙腈的萃取精馏分离提供基础数据。
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 

附录1：

 BLOCK:  ED-T     MODEL: RADFRAC         
 -------------------------------
    INLETS   - F        STAGE  29
               S        STAGE   5
    OUTLETS  - D1       STAGE   1
               W1       STAGE  36
   PROPERTY OPTION SET:   WILSON    WILSON / IDEAL GAS                          
 
                      ***  MASS AND ENERGY BALANCE  ***
                                    IN              OUT        RELATIVE DIFF.
    TOTAL BALANCE
       MOLE(LBMOL/HR)            1543.24         1543.24        0.000000E+00
       MASS(LB/HR   )            116491.         116491.        0.249838E-15
       ENTHALPY(BTU/HR  )      -0.112106E+09   -0.982356E+08   -0.123728    
 
 
 
                         **********************
                         ****  INPUT DATA  ****
                         **********************
 
   ****   INPUT PARAMETERS   ****
 
    NUMBER OF STAGES                                        36
    ALGORITHM OPTION                                      STANDARD    
    ABSORBER OPTION                                       NO      
    INITIALIZATION OPTION                                 STANDARD    
    HYDRAULIC PARAMETER CALCULATIONS                      NO      
    INSIDE LOOP CONVERGENCE METHOD                        BROYDEN
    DESIGN SPECIFICATION METHOD                           NESTED  
    MAXIMUM NO. OF OUTSIDE LOOP ITERATIONS                 200
    MAXIMUM NO. OF INSIDE LOOP ITERATIONS                   10
    MAXIMUM NUMBER OF FLASH ITERATIONS                      50
    FLASH TOLERANCE                                          0.000100000
    OUTSIDE LOOP CONVERGENCE TOLERANCE                       0.000100000
 
   ****   COL-SPECS   ****
 
    MOLAR VAPOR DIST / TOTAL DIST                            0.0        
    MOLAR REFLUX RATIO                                       3.80000    
    MOLAR DISTILLATE RATE          LBMOL/HR                110.231      
 
   ****    PROFILES   ****
 
    P-SPEC          STAGE   1  PRES, PSI                    14.6959     
 
                          *******************
                          ****  RESULTS  ****
                          *******************
 
 
   ***   COMPONENT SPLIT FRACTIONS   ***
 
                             OUTLET STREAMS
                             --------------
                  D1           W1      
    COMPONENT:
    BENZE-01    .99878       .12244E-02
    ACETO-01    .12003E-02   .99880    
    DIMET-01    .20126E-05   1.0000    
 
 
   ***    SUMMARY OF KEY RESULTS    ***
 
    TOP STAGE TEMPERATURE          F                       176.126      
    BOTTOM STAGE TEMPERATURE       F                       323.649      
    TOP STAGE LIQUID FLOW          LBMOL/HR                418.878      
    BOTTOM STAGE LIQUID FLOW       LBMOL/HR              1,433.00       
    TOP STAGE VAPOR FLOW           LBMOL/HR                  0.0        
    BOTTOM STAGE VAPOR FLOW        LBMOL/HR                995.655      
    MOLAR REFLUX RATIO                                       3.80000    
    MOLAR BOILUP RATIO                                       0.69480    
    CONDENSER DUTY (W/O SUBCOOL)   BTU/HR           -7,007,580.         
    REBOILER DUTY                  BTU/HR                    0.208782+08
 
   ****   MAXIMUM FINAL RELATIVE ERRORS   ****
 
    DEW POINT                       0.28979E-03  STAGE= 27
    BUBBLE POINT                    0.30726E-03  STAGE= 22
    COMPONENT MASS BALANCE          0.35900E-05  STAGE= 11 COMP=DIMET-01
    ENERGY BALANCE                  0.12133E-03  STAGE= 27
 
 
   ****    PROFILES   ****
 
   **NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS
            FROM THE STAGE EXCLUDING ANY SIDE PRODUCT.  FOR THE FIRST STAGE,
            THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW.  FOR THE
            LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW.
 
                                          ENTHALPY
 STAGE TEMPERATURE   PRESSURE             BTU/LBMOL          HEAT DUTY
       F             PSI            LIQUID       VAPOR        BTU/HR  
 
   1   176.13        14.696        24535.       37771.      -.70076+07
   2   176.21        14.696        24510.       37779.                
   3   176.38        14.696        24203.       37763.                
   4   178.08        14.696        20720.       37572.                
   5   204.52        14.696       -38826.       35640.                
   6   204.52        14.696       -38828.       35639.                
  28   210.41        14.696       -39143.       33533.                
  29   207.01        14.696       -33412.       33390.                
  30   212.20        14.696       -33201.       32512.                
  32   219.42        14.696       -32736.       31226.                
  33   221.31        14.696       -32983.       30909.                
  34   226.16        14.696       -36046.       30334.                
  35   253.97        14.696       -51678.       25903.                
  36   323.65        14.696       -70439.      -3705.4       .20878+08
 
 STAGE     FLOW RATE                  FEED RATE               PRODUCT RATE
            LBMOL/HR                   LBMOL/HR                 LBMOL/HR
       LIQUID     VAPOR       LIQUID    VAPOR    MIXED      LIQUID    VAPOR
   1  418.9     0.0000E+00                                  110.2311          
   2  418.7      529.1                                                        
   3  416.7      528.9                                                        
   4  387.6      526.9                                                        
   5  2274.      497.9      1322.7735                                         
   6  2274.      1061.                                                        
  28  2296.      1063.                                                        
  29  2555.      1084.       220.4622                                         
  30  2576.      1122.                                                        
  32  2610.      1164.                                                        
  33  2610.      1177.                                                        
  34  2566.      1177.                                                        
  35  2429.      1133.                                                        
  36  1433.      995.7                                     1433.0047          
 
    ****  MASS FLOW PROFILES  ****
 
 STAGE     FLOW RATE                  FEED RATE               PRODUCT RATE
            LB/HR                      LB/HR                    LB/HR   
       LIQUID     VAPOR       LIQUID    VAPOR    MIXED      LIQUID    VAPOR
   1 0.3270E+05 0.0000E+00                                 8605.6516          
   2 0.3270E+05 0.4131E+05                                                    
   3 0.3254E+05 0.4131E+05                                                    
   4 0.3028E+05 0.4115E+05                                                    
   5 0.1776E+06 0.3888E+05  .10335+06                                         
   6 0.1776E+06 0.8285E+05                                                    
  28 0.1568E+06 0.6533E+05                                                    
  29 0.1662E+06 0.6204E+05  .13136+05                                         
  30 0.1623E+06 0.5831E+05                                                    
  32 0.1590E+06 0.5224E+05                                                    
  33 0.1585E+06 0.5115E+05                                                    
  34 0.1583E+06 0.5060E+05                                                    
  35 0.1641E+06 0.5045E+05                                                    
  36 0.1079E+06 0.5626E+05                                 .10789+06          
 
                         ****   MOLE-X-PROFILE     ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.99878       0.12003E-02   0.24151E-04
      2    0.99921       0.47565E-03   0.31016E-03
      3    0.99651       0.24987E-03   0.32413E-02
      4    0.96348       0.19254E-03   0.36323E-01
      5    0.40473       0.25220E-03   0.59501    
      6    0.40458       0.40361E-03   0.59502    
     28    0.14708       0.26589       0.58703    
     29    0.11826       0.35253       0.52921    
     30    0.66238E-01   0.40766       0.52610    
     32    0.14994E-01   0.46388       0.52113    
     33    0.65423E-02   0.46981       0.52364    
     34    0.26337E-02   0.44285       0.55452    
     35    0.73275E-03   0.28451       0.71476    
     36    0.94186E-04   0.76831E-01   0.92308    
 
                         ****   MOLE-Y-PROFILE     ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.99698       0.30227E-02   0.18746E-05
      2    0.99878       0.12003E-02   0.24151E-04
      3    0.99912       0.62666E-03   0.25056E-03
      4    0.99698       0.44870E-03   0.25682E-02
      5    0.97130       0.41566E-03   0.28286E-01
      6    0.97105       0.66513E-03   0.28281E-01
     28    0.52272       0.44897       0.28309E-01
     29    0.41318       0.56346       0.23360E-01
     30    0.26923       0.70478       0.25985E-01
     32    0.72978E-01   0.89676       0.30264E-01
     33    0.33136E-01   0.93512       0.31745E-01
     34    0.14390E-01   0.94808       0.37531E-01
     35    0.58467E-02   0.90594       0.88210E-01
     36    0.16518E-02   0.58340       0.41494    
 
                         ****   K-VALUES           ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.99820        2.5184       0.77623E-01
      2    0.99956        2.5235       0.77866E-01
      3     1.0026        2.5080       0.77303E-01
      4     1.0348        2.3305       0.70707E-01
      5     2.3999        1.6481       0.47537E-01
      6     2.4002        1.6479       0.47529E-01
     28     3.5555        1.6885       0.48218E-01
     29     3.4956        1.5983       0.44145E-01
     30     4.0662        1.7288       0.49403E-01
     32     4.8676        1.9332       0.58081E-01
     33     5.0650        1.9904       0.60627E-01
     34     5.4638        2.1409       0.67685E-01
     35     7.9791        3.1843       0.12341    
     36     17.538        7.5934       0.44952    
 
                         ****   MASS-X-PROFILE     ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.99934       0.63116E-03   0.24171E-04
      2    0.99944       0.25003E-03   0.31032E-03
      3    0.99663       0.13133E-03   0.32425E-02
      4    0.96356       0.10120E-03   0.36336E-01
      5    0.40472       0.13254E-03   0.59515    
      6    0.40459       0.21212E-03   0.59520    
     28    0.16828       0.15989       0.67183    
     29    0.14199       0.22244       0.63557    
     30    0.82107E-01   0.26557       0.65232    
     32    0.19222E-01   0.31253       0.66825    
     33    0.84173E-02   0.31768       0.67391    
     34    0.33336E-02   0.29459       0.70207    
     35    0.84690E-03   0.17282       0.82634    
     36    0.97724E-04   0.41895E-01   0.95801    
 
                         ****   MASS-Y-PROFILE     ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.99841       0.15909E-02   0.18778E-05
      2    0.99934       0.63116E-03   0.24171E-04
      3    0.99942       0.32944E-03   0.25070E-03
      4    0.99719       0.23586E-03   0.25695E-02
      5    0.97148       0.21849E-03   0.28299E-01
      6    0.97135       0.34967E-03   0.28297E-01
     28    0.66420       0.29982       0.35980E-01
     29    0.56394       0.40417       0.31892E-01
     30    0.40449       0.55647       0.39049E-01
     32    0.12702       0.82029       0.52690E-01
     33    0.59560E-01   0.88336       0.57076E-01
     34    0.26154E-01   0.90561       0.68234E-01
     35    0.10254E-01   0.83500       0.15474    
     36    0.22837E-02   0.42389       0.57383    
 
 

附录2：

 
 BLOCK:  SR-T     MODEL: RADFRAC         
 -------------------------------
    INLETS   - F2       STAGE   4
    OUTLETS  - D2       STAGE   1
               W2       STAGE  20
   PROPERTY OPTION SET:   WILSON    WILSON / IDEAL GAS                          
 
                      ***  MASS AND ENERGY BALANCE  ***
                                    IN              OUT        RELATIVE DIFF.
    TOTAL BALANCE
       MOLE(LBMOL/HR)            1433.00         1433.00        0.000000E+00
       MASS(LB/HR   )            107885.         107885.        0.310232E-14
       ENTHALPY(BTU/HR  )      -0.114453E+09   -0.984701E+08   -0.139644    
 
 
 
                         **********************
                         ****  INPUT DATA  ****
                         **********************
 
   ****   INPUT PARAMETERS   ****
 
    NUMBER OF STAGES                                        20
    ALGORITHM OPTION                                      STANDARD    
    ABSORBER OPTION                                       NO      
    INITIALIZATION OPTION                                 STANDARD    
    HYDRAULIC PARAMETER CALCULATIONS                      NO      
    INSIDE LOOP CONVERGENCE METHOD                        BROYDEN
    DESIGN SPECIFICATION METHOD                           NESTED  
    MAXIMUM NO. OF OUTSIDE LOOP ITERATIONS                  25
    MAXIMUM NO. OF INSIDE LOOP ITERATIONS                   10
    MAXIMUM NUMBER OF FLASH ITERATIONS                      50
    FLASH TOLERANCE                                          0.000100000
    OUTSIDE LOOP CONVERGENCE TOLERANCE                       0.000100000
 
   ****   COL-SPECS   ****
 
    MOLAR VAPOR DIST / TOTAL DIST                            0.0        
    MOLAR REFLUX RATIO                                       1.50000    
    MOLAR DISTILLATE RATE          LBMOL/HR                110.011      
 
   ****    PROFILES   ****
 
    P-SPEC          STAGE   1  PRES, PSI                    14.6959     
 
                          *******************
                          ****  RESULTS  ****
                          *******************
 
 
   ***   COMPONENT SPLIT FRACTIONS   ***
 
                             OUTLET STREAMS
                             --------------
                  D2           W2      
    COMPONENT:
    BENZE-01    1.0000       .33910E-09
    ACETO-01    .99790       .21005E-02
    DIMET-01    .61490E-05   .99999    
 
 
   ***    SUMMARY OF KEY RESULTS    ***
 
    TOP STAGE TEMPERATURE          F                       178.560      
    BOTTOM STAGE TEMPERATURE       F                       375.188      
    TOP STAGE LIQUID FLOW          LBMOL/HR                165.016      
    BOTTOM STAGE LIQUID FLOW       LBMOL/HR              1,322.99       
    TOP STAGE VAPOR FLOW           LBMOL/HR                  0.0        
    BOTTOM STAGE VAPOR FLOW        LBMOL/HR              1,033.79       
    MOLAR REFLUX RATIO                                       1.50000    
    MOLAR BOILUP RATIO                                       0.78140    
    CONDENSER DUTY (W/O SUBCOOL)   BTU/HR           -3,572,500.         
    REBOILER DUTY                  BTU/HR                    0.195552+08
 
   ****   MAXIMUM FINAL RELATIVE ERRORS   ****
 
    DEW POINT                       0.38401E-03  STAGE= 15
    BUBBLE POINT                    0.12425E-03  STAGE= 15
    COMPONENT MASS BALANCE          0.70475E-05  STAGE=  7 COMP=BENZE-01
    ENERGY BALANCE                  0.14709E-03  STAGE= 16
 
 
   ****    PROFILES   ****
 
   **NOTE** REPORTED VALUES FOR STAGE LIQUID AND VAPOR RATES ARE THE FLOWS
            FROM THE STAGE EXCLUDING ANY SIDE PRODUCT.  FOR THE FIRST STAGE,
            THE REPORTED VAPOR FLOW IS THE VAPOR DISTILLATE FLOW.  FOR THE
            LAST STAGE, THE REPORTED LIQUID FLOW IS THE LIQUID BOTTOMS FLOW.
 
                                          ENTHALPY
 STAGE TEMPERATURE   PRESSURE             BTU/LBMOL          HEAT DUTY
       F             PSI            LIQUID       VAPOR        BTU/HR  
 
   1   178.56        14.696        20173.       33175.      -.35725+07
   2   178.82        14.696        19820.       33163.                
   3   183.84        14.696        11221.       33035.                
   4   234.36        14.696       -41178.       29267.                
   5   234.38        14.696       -41176.       29264.                
  18   370.01        14.696       -75697.      -49928.                
  19   374.40        14.696       -76046.      -55935.                
  20   375.19        14.696       -76107.      -57053.       .19555+08
 
 STAGE     FLOW RATE                  FEED RATE               PRODUCT RATE
            LBMOL/HR                   LBMOL/HR                 LBMOL/HR
       LIQUID     VAPOR       LIQUID    VAPOR    MIXED      LIQUID    VAPOR
   1  165.0     0.0000E+00                                  110.0106          
   2  163.3      275.0                                                        
   3  142.5      273.3                                                        
   4  2257.      252.5      1433.0047                                         
   5  2257.      933.6                                                        
  18  2340.      947.6                                                        
  19  2357.      1017.                                                        
  20  1323.      1034.                                     1322.9940          
 
    ****  MASS FLOW PROFILES  ****
 
 STAGE     FLOW RATE                  FEED RATE               PRODUCT RATE
            LB/HR                      LB/HR                    LB/HR   
       LIQUID     VAPOR       LIQUID    VAPOR    MIXED      LIQUID    VAPOR
   1  6782.     0.0000E+00                                 4521.5169          
   2  6727.     0.1130E+05                                                    
   3  6314.     0.1125E+05                                                    
   4 0.1434E+06 0.1084E+05  .10789+06                                         
   5 0.1434E+06 0.4004E+05                                                    
  18 0.1823E+06 0.7123E+05                                                    
  19 0.1841E+06 0.7892E+05                                                    
  20 0.1034E+06 0.8069E+05                                 .10336+06          
 
                         ****   MOLE-X-PROFILE     ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.12253E-02   0.99870       0.73936E-04
      2    0.47998E-03   0.99603       0.34863E-02
      3    0.27903E-03   0.91244       0.87282E-01
      4    0.11232E-03   0.39332       0.60657    
      5    0.44099E-04   0.39340       0.60655    
     18    0.55216E-11   0.64048E-02   0.99360    
     19    0.44933E-12   0.11092E-02   0.99889    
     20    0.34550E-13   0.17480E-03   0.99983    
 
                         ****   MOLE-Y-PROFILE     ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.31095E-02   0.99689       0.15574E-05
      2    0.12253E-02   0.99870       0.73936E-04
      3    0.78002E-03   0.99711       0.21126E-02
      4    0.69124E-03   0.95002       0.49293E-01
      5    0.27148E-03   0.95042       0.49304E-01
     18    0.14970E-09   0.80128E-01   0.91987    
     19    0.12660E-10   0.14509E-01   0.98549    
     20    0.98015E-12   0.23049E-02   0.99770    
 
                         ****   K-VALUES           ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1     2.5377       0.99819       0.21064E-01
      2     2.5528        1.0027       0.21207E-01
      3     2.7954        1.0928       0.24205E-01
      4     6.1545        2.4154       0.81257E-01
      5     6.1562        2.4159       0.81281E-01
     18     27.112        12.511       0.92580    
     19     28.174        13.081       0.98659    
     20     28.369        13.186       0.99787    
 
                         ****   MASS-X-PROFILE     ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.23287E-02   0.99753       0.14056E-03
      2    0.91004E-03   0.99248       0.66118E-02
      3    0.49202E-03   0.84556       0.15395    
      4    0.13806E-03   0.25408       0.74578    
      5    0.54208E-04   0.25415       0.74580    
     18    0.55370E-11   0.33754E-02   0.99662    
     19    0.44944E-12   0.58307E-03   0.99942    
     20    0.34544E-13   0.91848E-04   0.99991    
 
                         ****   MASS-Y-PROFILE     ****
   STAGE     BENZE-01      ACETO-01      DIMET-01
      1    0.59000E-02   0.99410       0.29558E-05
      2    0.23287E-02   0.99753       0.14056E-03
      3    0.14803E-02   0.99451       0.40105E-02
      4    0.12585E-02   0.90898       0.89765E-01
      5    0.49442E-03   0.90969       0.89817E-01
     18    0.15558E-09   0.43764E-01   0.95624    
     19    0.12744E-10   0.76761E-02   0.99232    
     20    0.98095E-12   0.12123E-02   0.99879    
 
1 宋海华, 孙伟, 王秀丽, 王明涛. 萃取精馏溶剂选择的研究进展[J]. 化学工业与工程 , 2002,(01)
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3 刘建新, 肖翔. 萃取精馏技术与工业应用进展[J]. 现代化工 , 2004,(06)
4 崔现宝, 杨志才, 冯天扬. 萃取精馏及进展[J]. 化学工业与工程 , 2001,(04)
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6  Cines M R. Extractive Distillation. US Pat Appl 4 053 369. 1977
7 张志刚. 混合溶剂间歇萃取精馏的研究[D]天津大学 , 2004
8  Glanz S,Stichlmair J. Mixed integer optimization of combined solvent extraction and distillation processes
9  Jimenez L, Costa L J. Solvent selection for a reactive and extractive distillation process by headspace gas chromatography [J]. Sepatation Science and Technology, 2003,38(1):21—37.
10  Seiler M,Arlt W. Hyperbranched polymers: New selective solvents for extractive distillation and solvent extraction[J].
11  Shi Y H, Li W Q, Tu J L. Vapor - Liquid Equilibria for Dimethyl Carbonate - n - Butyl Acetate Binary System at 101. 325 kPa .Chinese J Chem Eng, 1999, 7(1) :83 .
12 杨志才,吴迪. 分批精馏过程设计计算方法的研究[J]石油化工设计, 1996,(02).
13 陈建宁,阮奇,陈佳彬,刘莉萍. 间歇精馏常规设计和优化设计的模型及算法[J]计算机与应用化学, 2004,(03).
14 李光兴,熊国玺. 糠醛萃取精馏分离甲醇-碳酸二甲酯二元共沸物研究[J]化学工程, 2000,(04).
 
 
 
致谢
本论文的完成，凝聚了我和导师以及其他许多可敬的老师和同学的心血。在此请接受我真诚的感谢！首先，感谢我的导师XX老师，他严谨细致，一丝不苟的作风一直是我学习的榜样；他循循善诱的教导和不拘一格的精神将使我铭记在心。在论文的选题、研究以及撰写过程中，杨老师给予了充分的指导、支持，并为我提供了良好的实验环境和实验条件，在我遇到困难时，杨老师总是给予我热情地鼓励和有益的启示，让我学到了许多以前没有学过得知识，掌握了科研的方法和程序，也获得了实践锻炼得机会。他严谨的工作态度，对我的严格要求以及为人处世的坦荡使我终身受益。感谢同学们在我遇到困难时给我不少鼓励和支持，从他们身上我学到了很多东西，和他们在一起的日子是快乐的时光。还有好多我无法一一列举姓名的师长和友人给了我指导和帮助，在此一并表示衷心的感谢！
   


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