CN112174768B - Method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation in dividing wall column - Google Patents

Method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation in dividing wall column Download PDF

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CN112174768B
CN112174768B CN202011014425.XA CN202011014425A CN112174768B CN 112174768 B CN112174768 B CN 112174768B CN 202011014425 A CN202011014425 A CN 202011014425A CN 112174768 B CN112174768 B CN 112174768B
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cyclopentane
dividing wall
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CN112174768A (en
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李国庆
卓楷升
仝保田
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Guangdong Chuanxun Technology Co ltd
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South China University of Technology SCUT
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    • C07C7/00Purification; Separation; Use of additives
    • C07C7/04Purification; Separation; Use of additives by distillation
    • C07C7/05Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
    • C07C7/08Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
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Abstract

The invention discloses a method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation in a bulkhead tower, belonging to the technical field of petrochemical industry. The technological process of the invention is improved on the basis of the original cyclopentane device and the technological process as follows: the original extraction rectifying tower and extractant recovery tower device is changed into a bulkhead extraction rectifying tower device, and the flow of other pipelines is not changed. Compared with the conventional separation process, the process flow can save energy by 27.4 percent, reduces equipment investment, has higher product purity and has obvious innovation significance.

Description

Method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation in dividing wall column
Technical Field
The invention belongs to the technical field of petrochemical industry, and particularly relates to a method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation in a dividing wall tower.
Background
The carbon five fraction obtained in the petroleum processing process mainly contains n-pentane, cyclopentane and 2, 2-dimethylbutane. Wherein the boiling point of cyclopentane is 49.3 ℃, the boiling point of 2, 2-dimethylbutane is 50 ℃, and the cyclopentane product with the mass fraction of 98.5 percent is difficult to obtain by ordinary rectification, so that the extraction and the rectification are more. The extractant was N, N-Dimethylformamide (DMF), boiling at 153 deg.C, which dissolves cyclopentane but is immiscible with 2, 2-dimethylbutane. The basic flow is that the raw material is pre-divided to obtain a mixture of cyclopentane and 2, 2-dimethylbutane, then the mixture enters an extraction and rectification tower, 2, 2-dimethylbutane is distilled off from the top, cyclopentane and an extractant are distilled off from the bottom and sent to an extractant recovery tower, the target product cyclopentane is obtained by separation, and the extractant is recycled.
Obviously, the process has long flow, high energy consumption and large equipment investment, and can obtain target products only by extracting and separating two towers, and whether the extraction and separation can be integrated into a bulkhead tower (DWC) or not, so as to realize single-tower three-component separation? This is the cause of the present invention.
Disclosure of Invention
The invention aims to solve the defects of long process flow, high energy consumption, large equipment investment, low purity of a target product cyclopentane and the like of the existing cyclopentane and 2, 2-dimethylbutane extractive distillation double-tower process, and provides a method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation in a dividing wall tower.
The invention is realized by the following technical scheme:
the present invention changes the original extraction and rectification tower and extractant recovering tower into bulkhead extraction and rectification tower, and has unchanged flow of other pipelines.
The inside of the dividing wall tower 14 is provided with a dividing wall plate 18 along the height direction, and the dividing wall plate 18 is a dividing wall plate which extends downwards from the top in the dividing wall tower 14 but is not contacted with the bottom of the dividing wall tower 14; the upper part of the cyclopentane discharging side of the partition wall tower 14 is closed and is not connected with the top space;
one side of the bulkhead tower 14 is a feeding side 15, an extracting agent and a feeding material enter from the feeding side 15 to realize the function of an extraction and rectification tower, the other side is an intermediate extraction side 16 of the cyclopentane, most of high-purity cyclopentane steam evaporated from the bottom of the bulkhead tower 14 is distilled off from the intermediate extraction side 16 to realize the rectification of a cyclopentane product; and a common stripping section 17 is arranged at the end part of a bulkhead tower bottom reboiler 25 of the bulkhead tower 14 to the bulkhead plate 18 and is mainly used for steaming out high-purity cyclopentane steam to realize the functions of an extractant regeneration section and a stripping section.
The method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation in a bulkhead column comprises the following steps:
extracting agent N, N-Dimethylformamide (DMF) and feeding material respectively enter from the upper part of a feeding side 15 of a dividing wall tower 14, relative volatility of cyclopentane and 2, 2-dimethylbutane is changed in the descending process of the extracting agent, most of cyclopentane flows to the bottom, 2-dimethylbutane is distilled from the feeding side 15 of the top of the dividing wall tower 14, and the mixture enters a feeding side overhead reflux tank 20 after being cooled by a feeding side overhead condenser 19 and is divided into two parts after being pressurized by a feeding side tower reflux pump 21: one part of the reflux liquid is returned to the bulkhead tower from the top of the bulkhead tower, and the other part of the reflux liquid is taken as a product 2, 2-dimethylbutane out of the tower;
the extractant N, N-dimethylformamide and the main component in the feeding material are cyclopentane which are mutually dissolved and then flow to the common stripping section 17, and the part at the bottom of the next door tower is contacted with steam generated after being heated by a reboiler 25 at the bottom of the next door tower, so that the cyclopentane is distilled out;
the high-purity cyclopentane vapor rises and enters both sides of the dividing wall tower 14, wherein the cyclopentane vapor at the feed side 15 is rapidly cooled by the descending mixed liquid and then returns to the bottom of the dividing wall tower, and the high-purity cyclopentane vapor evaporated from the middle extraction side 16 is evaporated at the top of the middle extraction side, is cooled by a middle extraction side tower top condenser 22 and enters a middle extraction side tower top reflux tank 23, and is divided into two parts after being pressurized by a middle extraction side tower reflux pump 24: namely, one part of the product is taken as reflux and enters the bulkhead tower from the top of the tower side, and the other part of the product is taken as a side product to extract cyclopentane;
the extractant N, N-dimethyl formamide (DMF) which descends to the bottom of the partition wall tower is heated by a reboiler 25 at the bottom of the partition wall tower, then the part of the extractant is returned to the bottom of the partition wall tower, the extractant discharged from the tower bottom is extracted from the bottom of the partition wall tower, then the pressure is increased by a solvent circulating pump 13, and the extractant is cooled by a solvent cooler 1 for recycling.
The dividing wall bottom reboiler 25 uses 1.0MPa steam as a heat source.
The raw material enters from the middle part of the feeding side 15 of the dividing wall tower 14, the position of the feeding plate is between the 25 th and 35 th plates from top to bottom on the feeding side 15 (the overhead condenser is the first plate, the number is sequentially from bottom to top, the same is carried out below), the feeding temperature is 40-50 ℃, the extractant enters from the upper part of the feeding side 15, and the position of the feeding plate is between the 3 rd and 6 th plates from top to bottom on the feeding side 15.
The temperature of the extracting agent is 60-70 ℃.
The operation pressure of the dividing wall tower is normal pressure or reduced pressure, and the solvent ratio is 11-16 (the operation ratio is preferably 11-12).
The overhead reflux ratio on the feed side is between 20 and 30 (with a preferred value of 22 to 25).
The overhead temperature of the feed side 15 is between 50 and 80 ℃; the reflux ratio of the middle extraction side tower top is between 0.5 and 1.5 (the optimal value is between 0.7 and 1); the temperature of the top of the middle extraction side tower is between 45 and 75 ℃, and the number of the middle extraction side theoretical plates is between 20 and 30.
The theoretical plates of the common stripping section 17 are 8-15 blocks, wherein the operation temperature of the tower bottom is between 150 ℃ and 200 ℃.
Compared with the prior art, the invention has the following advantages and effects:
1. the temperature of the reboiling and returning tower of the bulkhead tower rises to 154.8 ℃, the reboiling device at the bottom of the tower uses 1.0MPa steam, and the saturation temperature is 184.3 ℃, so that the heat exchange requirement can be met;
2. reboiling load at bulkhead bottom of column is 1034X 104kcal/h, reboiling load of the extractive distillation column is 559 multiplied by 104kcal/h, the reboiling load of the extraction agent recovery tower is 866 multiplied by 104kcal/h, total 1425 × 104kcal/h, decrease 391X 104kcal/h, the reduction amplitude reaches 27.4%;
3. the number of the theoretical plates of the extraction and rectification tower and the number of the theoretical plates of the extractant recovery tower are 86 and 36, the total number is 122, the number of the theoretical plates of the next-wall tower is 75, 47 blocks are reduced, the reduction amplitude reaches 38.5 percent, and the equipment investment can be effectively reduced;
4. the purity of the distilled product of the partition tower is higher than that of the products obtained by the extraction rectifying tower and the extractant recovery tower; therefore, compared with the conventional separation process, the method can save energy by 27.4 percent, reduce equipment investment and improve product purity.
Drawings
FIG. 1 is a process flow diagram of a comparative example of the present invention (existing extractive distillation column and extractant recovery column).
FIG. 2 is a process flow diagram of a dividing wall column according to an embodiment of the present invention.
The numbering in the figures is as follows:
1-a solvent cooler; 2-extractive distillation column; 3-an overhead condenser of the extractive distillation tower; 4-reflux tank at the top of the extractive distillation tower; 5-reflux pump of extractive distillation column; 6-extractive distillation tower bottom reboiler; 7-extractant recovery tower feed pump; 8-an extractant recovery column; 9-an extractant recovery tower top condenser; 10-an extractant recovery tower top reflux tank; 11-reflux pump of extractant recovery tower; 12-extractant recovery bottoms reboiler; 13-solvent circulation pump; 14-a divided wall column; 15-feed side; 16-the middle production side; 17-a common stripping section; 18-dividing wall panels; 19-feed side overhead condenser; 20-feed side overhead reflux drum; 21-feed side column reflux pump; 22-middle extraction side tower top condenser; 23-intermediate extraction side overhead reflux drum; 24-intermediate extraction side column reflux pump; 25-bulkhead bottoms reboiler.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Comparison example (prior art)
The comparative example is an existing extractive distillation column and an extracting agent recovery column, and the process flow diagram is shown in figure 1.
The specific process is as follows:
an extractant N, N-Dimethylformamide (DMF) and a feed material respectively enter from the upper part of an extraction rectifying tower 2, the relative volatility of cyclopentane and 2, 2-dimethylbutane is changed in the descending process of the extractant, most of cyclopentane flows to the bottom, 2-dimethylbutane is distilled from the top of the extraction rectifying tower, and the cyclopentane and the 2, 2-dimethylbutane enter a reflux tank 4 at the top of the extraction rectifying tower after being cooled by a condenser 3 at the top of the extraction rectifying tower and are pressurized by a reflux pump 5 of the extraction rectifying tower to be divided into two parts, one part is used as a reflux liquid to return into the tower from the top, and the other part is used as a product 2, 2-dimethylbutane to exit the tower; the extractant N, N-Dimethylformamide (DMF) and the main component in the feed are cyclopentane which are mutually dissolved and then flow to the bottom of the tower together. The reboiler 6 at the bottom of the extractive distillation tower uses 1.0MPa steam as a heat source. The mixture of the extractant and cyclopentane in the extraction and rectification tower is extracted from the bottom of the tower, and enters an extractant recovery tower 8 after being pressurized by an extractant recovery tower feed pump 7, high-purity cyclopentane steam rises and is evaporated at the top of the extractant recovery tower 8, and enters an extractant recovery tower top reflux tank 10 after being cooled by an extractant recovery tower top condenser 9, and is divided into two parts after being pressurized by an extractant recovery tower reflux pump 11, wherein one part is used as reflux and enters the tower from the tower side top, and the other part is used as a side line product to extract cyclopentane. The extractant discharged from the tower bottom is extracted from the tower bottom, pressurized by a solvent circulating pump 13 and then cooled by a solvent cooler 1 for recycling; the extractant recovery bottoms reboiler 12 used 1.0MPa steam as the heat source.
The embodiment of the invention is as follows:
extracting agent N, N-Dimethylformamide (DMF) and feeding material respectively enter from the upper part of a feeding side 15 of the tower, the relative volatility of cyclopentane and 2, 2-dimethylbutane is changed in the descending process of the extracting agent, most of cyclopentane flows to the bottom, 2-dimethylbutane is distilled from the top of the feeding side tower, the cyclopentane enters a feeding side tower top reflux tank 20 after being cooled by a feeding side tower top condenser 19, the cyclopentane is pressurized by a feeding side tower reflux pump 21 and then is divided into two parts, one part is used as reflux liquid to return to the tower from the top, and the other part is used as a product 2, 2-dimethylbutane to exit the tower; the extractant N, N-Dimethylformamide (DMF) and the main component cyclopentane in the feed material are mutually dissolved and then flow to the common stripping section 17, and the cyclopentane is distilled out by contacting with the steam generated after the bottom part of the column is heated by a bulkhead reboiler 25 at the bottom of the column. High-purity cyclopentane vapor rises and enters two sides of a partition wall tower, wherein the cyclopentane vapor at a feed side 15 is quickly cooled by descending mixed liquid and then returns to the bottom of the tower, the high-purity cyclopentane vapor distilled from a middle extraction side 16 is distilled at the top of the middle extraction side, is cooled by a middle extraction side tower top condenser 22 and enters a middle extraction side tower top reflux tank 23, the high-purity cyclopentane vapor is pressurized by a middle extraction side tower reflux pump 24 and then is divided into two parts, one part is taken as reflux and enters the tower from the top of the tower side, and the other part is taken as a side product to extract cyclopentane. The extractant N, N-Dimethylformamide (DMF) which falls to the bottom of the tower is heated by a reboiler 25 at the bottom of the partition wall tower, and then part of the extractant is returned to the bottom of the tower, and the extractant discharged from the bottom of the tower is extracted from the bottom of the tower, pressurized by a solvent circulating pump 13, and then cooled by a solvent cooler 1 for recycling; the dividing wall column bottom reboiler 25 uses 1.0MPa steam as a heat source.
The main operation of the comparative example and the examples is illustrated below with a certain 8 ten thousand ton/year cyclopentane installation under the same separation requirements and solvent ratio (98.5% by weight cyclopentane).
Table 1 below is a summary of the process parameters of the comparative examples and examples:
Figure BDA0002698578550000061
table 2 below is a summary of the product properties of the comparative examples and examples:
item Comparative example Examples
Flow rate of cyclopentane product, t/h 8.3 8.3
2, 2-dimethylbutane product flow, t/h 1.7 1.7
Purity,% wt, of cyclopentane product 98.5 99.3
Purity,% wt, of 2, 2-dimethylbutane product 86.7 90.4
From the above tables 1 and 2 it can be seen that the invention is comparable to the comparative examples:
1. the temperature of the reboiling and returning tower of the bulkhead tower rises to 154.8 ℃, the reboiling device at the bottom of the tower uses 1.0MPa steam, and the saturation temperature is 184.3 ℃, so that the heat exchange requirement can be met;
2. reboiling load at bulkhead bottom of column is 1034X 104kcal/h, reboiling load of the extractive distillation column is 559 multiplied by 104kcal/h, the reboiling load of the extraction agent recovery tower is 866 multiplied by 104kcal/h, total 1425 × 104kcal/h, decrease 391X 104kcal/h, the reduction amplitude reaches 27.4%;
3. the number of the theoretical plates of the extraction and rectification tower and the number of the theoretical plates of the extractant recovery tower are 86 and 36, the total number is 122, the number of the theoretical plates of the next-wall tower is 75, 47 blocks are reduced, the reduction amplitude reaches 38.5 percent, and the equipment investment can be effectively reduced;
4. the purity of the distilled product of the partition tower is higher than that of the products obtained by the extraction rectifying tower and the extractant recovery tower;
therefore, compared with the conventional separation flow, the embodiment can save energy by 27.4 percent, reduce equipment investment and improve product purity.
As described above, the present invention can be preferably realized.
The embodiments of the present invention are not limited to the above-described embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.

Claims (8)

1. The method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation in a bulkhead column is characterized by comprising the following steps:
extracting agent N, N-dimethylformamide and feeding material respectively enter from the upper part of a feeding side (15) of a dividing wall tower (14), the relative volatility of cyclopentane and 2, 2-dimethylbutane is changed in the descending process of the extracting agent, most of cyclopentane flows to the bottom, 2-dimethylbutane is distilled from the feeding side (15) of the top of the dividing wall tower (14), and after being cooled by a feeding side overhead condenser (19), the extracting agent N, N-dimethylformamide and the feeding material enter into a feeding side overhead reflux tank (20) and are pressurized by a feeding side tower reflux pump (21) to be divided into two parts: one part of the reflux liquid is returned to the bulkhead tower from the top of the bulkhead tower, and the other part of the reflux liquid is taken as a product 2, 2-dimethylbutane out of the tower;
the extractant N, N-dimethylformamide and the component in the feeding material are cyclopentane which are mutually dissolved and then flow to a common stripping section (17), and the part at the bottom of the next door tower is contacted with steam generated after being heated by a reboiler (25) at the bottom of the next door tower, so that the cyclopentane is distilled out;
high-purity cyclopentane vapor rises and enters two sides of a bulkhead tower (14), wherein the cyclopentane vapor at a feed side (15) is cooled by descending mixed liquid and then returns to the bottom of the bulkhead tower, the high-purity cyclopentane vapor distilled from a middle extraction side (16) is distilled at the top of the middle extraction side, is cooled by a middle extraction side tower top condenser (22) and enters a middle extraction side tower top reflux tank (23), and is pressurized by a middle extraction side tower reflux pump (24) and then divided into two parts: namely, one part of the product is taken as reflux and enters the bulkhead tower from the top of the tower side, and the other part of the product is taken as a side product to extract cyclopentane;
the extractant N, N-dimethylformamide which falls to the bottom of the dividing wall tower is heated by a reboiler (25) at the bottom of the dividing wall tower, and then is partially returned to the bottom of the dividing wall tower, and the extractant discharged from the tower bottom is extracted from the bottom of the dividing wall tower, pressurized by a solvent circulating pump (13), and cooled by a solvent cooler (1) for recycling;
the raw material enters from the middle part of a feeding side (15) of a bulkhead tower (14), the feeding temperature of a feeding plate between 25 th and 35 th plates from top to bottom at the feeding side (15) is 40-50 ℃, the extractant enters from the upper part of the feeding side (15), and the feeding plate is between 3 rd and 6 th plates from top to bottom at the feeding side (15);
a partition wall plate (18) is arranged in the partition wall tower (14) along the height direction, and the partition wall plate (18) is a partition wall which extends downwards from the top in the partition wall tower (14) but is not contacted with the bottom of the partition wall tower (14); the upper part of the cyclopentane discharging side of the partition wall tower (14) is closed and is not connected with the top space;
one side of the dividing wall tower (14) is a feeding side (15), an extracting agent and a feeding material enter from the feeding side (15) to realize the function of an extraction and rectification tower, the other side of the dividing wall tower is an intermediate extraction side (16) of cyclopentane, most of high-purity cyclopentane steam evaporated from the bottom of the dividing wall tower (14) is distilled from the intermediate extraction side (16), and the rectification of a cyclopentane product is realized; and a common stripping section (17) is arranged at the end part of a dividing wall tower bottom reboiler (25) of the dividing wall tower (14) to the dividing wall plate (18) and is used for steaming out high-purity cyclopentane steam to realize the functions of an extractant regeneration and a stripping section.
2. The method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation through the dividing wall column according to claim 1, characterized in that: the dividing wall bottom reboiler (25) uses 1.0MPa steam as a heat source.
3. The method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation through the dividing wall column according to claim 2, wherein the temperature of the extractant is 60-70 ℃.
4. The method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation through a dividing wall column according to claim 3, wherein the operating pressure of the dividing wall column is normal pressure or reduced pressure, and the solvent ratio is 11-16.
5. The method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation through a dividing wall column according to claim 4, wherein the overhead reflux ratio on the feed side is 20-30.
6. The process for the extractive rectification separation of cyclopentane and 2, 2-dimethylbutane according to claim 5, characterised in that the overhead temperature of the feed side (15) is between 50 and 80 ℃.
7. The method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation through a dividing wall column according to claim 6, characterized in that the mid-draw side-overhead reflux ratio is between 0.5 and 1.5.
8. The method for separating cyclopentane and 2, 2-dimethylbutane by extractive distillation through a dividing wall column according to claim 7, wherein the temperature of the top of the intermediate extraction side is 45-75 ℃, and the theoretical plate of the intermediate extraction side is 20-30.
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