CN116730791B - Continuous extraction process in carbon five separation - Google Patents
Continuous extraction process in carbon five separation Download PDFInfo
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- CN116730791B CN116730791B CN202311013024.6A CN202311013024A CN116730791B CN 116730791 B CN116730791 B CN 116730791B CN 202311013024 A CN202311013024 A CN 202311013024A CN 116730791 B CN116730791 B CN 116730791B
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- 238000000605 extraction Methods 0.000 title claims abstract description 120
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 41
- 238000000926 separation method Methods 0.000 title claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 82
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims abstract description 70
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000463 material Substances 0.000 claims abstract description 42
- 238000004064 recycling Methods 0.000 claims abstract description 28
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims abstract description 20
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 claims abstract description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 75
- 238000006471 dimerization reaction Methods 0.000 claims description 32
- 230000008929 regeneration Effects 0.000 claims description 30
- 238000011069 regeneration method Methods 0.000 claims description 30
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical group C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 claims description 26
- PMJHHCWVYXUKFD-UHFFFAOYSA-N piperylene Natural products CC=CC=C PMJHHCWVYXUKFD-UHFFFAOYSA-N 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 25
- 238000004821 distillation Methods 0.000 claims description 19
- 238000007670 refining Methods 0.000 claims description 19
- 238000010790 dilution Methods 0.000 claims description 16
- 239000012895 dilution Substances 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 10
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 claims description 6
- 239000000571 coke Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000011273 tar residue Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 22
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 238000000895 extractive distillation Methods 0.000 description 26
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 14
- 238000007865 diluting Methods 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 6
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 5
- 238000010533 azeotropic distillation Methods 0.000 description 4
- 230000000379 polymerizing effect Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003339 best practice Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A continuous extraction process in carbon five separation belongs to the technical field of carbon five separation. The method is characterized by comprising the following steps of: 1) The cracked carbon five fraction firstly enters a first extraction rectifying tower (1) and is subjected to continuous extraction rectification by directly utilizing DMF solvent, and pentane and pentene are separated from the top of the first extraction rectifying tower (1); the material at the bottom of the first extraction rectifying tower (1) enters a front analytical tower group to continuously separate DMF solvent; 2) Continuously extracting and rectifying materials continuously extracted from the top of the front analytical tower group in a second extraction and rectification tower (4) by using a carbon tetrachloride solvent, and continuously extracting isoprene from the top of the second extraction and rectification tower (4); and (3) continuously separating and recycling the carbon tetrachloride solvent by feeding the material at the bottom of the second extraction rectifying tower (4) into a rear analysis tower group. According to the invention, the carbon five fraction is separated by two-step continuous extraction, repeated rectification is not needed, and the energy consumption can be further reduced.
Description
Technical Field
A continuous extraction process in carbon five separation belongs to the technical field of carbon five separation.
Background
The content of diolefin in the cracked carbon five fraction varies, and the total content is between 40% and 60%, due to the difference of petroleum hydrocarbon cracking raw materials, cracking depth and separation degree. The extraction and rectification process is generally adopted to separate the carbon five, and the most commonly used process at present is the DMF method which is most applied. In the process of extracting and separating carbon five by using a DMF method, the carbon five fraction from which dicyclopentadiene and heavy components are removed is subjected to a separation process of a first extraction rectifying tower, a second extraction rectifying tower and a plurality of stripping towers to obtain products of polymerization-grade isoprene, m-pentadiene with certain purity, residual carbon five light components and the like; recycling DMF solvent, wherein a part of DMF solvent is extracted in the recycling process for regeneration and refining so as to maintain the purity of DMF solvent; separating dicyclopentadiene and heavy components to obtain dicyclopentadiene product. However, the traditional DMF method has longer process flow and high process requirement, and people have improved the method.
For example, chinese patent CN101302135B discloses a method for separating isoprene fraction by one-stage extractive distillation, which uses a distillation method to remove cyclopentadiene and an azeotropic distillation method to remove alkyne, and can obtain polymer grade isoprene product without secondary extraction, thereby omitting a second extraction unit and a solvent refining tower. However, in order to ensure the purity of the obtained isoprene, the method needs to carry out hydrofining, which reduces the yield of the isoprene and causes a certain degree of resource waste.
The applicant also discloses an improved process for extracting and separating isoprene by using a DMF method in patent CN115611698B, wherein the cracked carbon five fraction firstly enters an azeotropic distillation tower to carry out azeotropic distillation, a material A mainly containing isoprene is extracted from the top of the azeotropic distillation tower, and a solution mainly containing isoprene is extracted and distilled; separating solvent from the analysis tower, refining isoprene, and collecting polymerization grade isoprene; and (3) extracting a material mainly comprising cyclopentadiene from the tower kettle of the azeotropic rectifying tower 1, performing dimerization reaction, and performing secondary rectification on residual isoprene. The method realizes continuous isoprene acquisition during DMF extraction and separation. However, the applicant finds that in the application process, the method needs to be subjected to multi-step rectification, and still has the problem of high energy consumption.
Disclosure of Invention
The invention aims to solve the technical problems that: overcomes the defects of the prior art and provides a continuous extraction process in the separation of carbon five with lower energy consumption.
The technical scheme adopted for solving the technical problems is as follows: the continuous extraction process in the separation of the carbon five is characterized by comprising the following steps of:
1) The cracked carbon five fraction enters a first extraction rectifying tower to directly utilize DMF solvent for continuous extraction and rectification, and pentane and pentene are separated from the top of the first extraction rectifying tower; continuously separating DMF solvent from the material at the bottom of the first extraction rectifying tower in a front analytical tower group;
2) Continuously extracting and rectifying materials continuously extracted from the tower top of the front analytic tower group in a second extraction and rectification tower by using a carbon tetrachloride solvent, and continuously extracting isoprene from the tower top of the second extraction and rectification tower; and (3) continuously separating and recovering the carbon tetrachloride solvent by the material at the bottom of the second extraction rectifying tower after entering the post-resolving tower group.
According to the invention, the carbon five fraction is separated by two-step continuous extraction, the carbon five fraction is not subjected to rectification separation or/and dimerization in advance, instead, DMF (dimethyl formamide) extraction rectification is directly performed, pentane and pentene are separated, then carbon tetrachloride solvent is used for extraction rectification, isoprene is directly separated, and repeated rectification is not needed in the process, so that the energy consumption can be further reduced. The residual cyclopentadiene and piperylene are dimerized again, so that the polymerization volume is reduced. After dimerization, the dicyclopentadiene and the piperylene can be separated easily by distillation.
Preferably, in the continuous extraction process in the carbon five separation, the front analytical tower comprises an analytical tower a and an analytical tower b, the analytical tower a and the analytical tower b are operated in series, the material at the bottom of the first extraction rectifying tower enters the analytical tower a from the middle part, and DMF solvent extracted from the tower kettle of the analytical tower a is returned to the first extraction rectifying tower for recycling; the gas extracted from the top of the resolving tower a enters the lower part of the resolving tower b, the liquid part of the tower bottom of the resolving tower b enters from the top of the resolving tower a, and the material extracted from the top of the resolving tower b enters into the second extraction rectifying tower.
Preferably, in the continuous extraction process in the carbon five separation, the post-resolving tower group comprises a resolving tower e and a resolving tower f, the resolving tower e and the resolving tower f are operated in series, the material at the bottom of the second extraction rectifying tower enters the resolving tower e from the middle part, and the carbon tetrachloride solvent extracted from the tower bottom of the resolving tower e returns to the second extraction rectifying tower for recycling; the gas extracted from the top of the resolving tower e enters the lower part of the resolving tower f, the liquid part of the tower kettle of the resolving tower f enters from the top of the resolving tower e, and the material extracted from the top of the resolving tower f enters into a dimerization tank group to participate in dimerization reaction.
After polymerization, the solvent is separated by a series of analytical towers, and the solvent is recycled.
Preferably, the dimerization tank set at least comprises two dimerization tanks connected in parallel. The dimerization tanks connected in parallel are utilized for alternating polymerization and discharging, so that the continuous carbon five separation can be kept.
Preferably, the top extract part of the second extractive distillation column returns to the middle part of the second extractive distillation column through an external pipeline to participate in extractive distillation again. The invention utilizes the difference of solubility of isoprene, cyclopentadiene and the like in carbon tetrachloride to carry out extractive distillation, but the solubility of each component in carbon tetrachloride is not as great as that in DMF, so that part of the extract is required to return to the middle part of the second extractive distillation tower through an external pipeline to participate in extractive distillation again, thereby improving the purity of isoprene.
Preferably, the discharge hole of the dimerization tank group is connected with a distillation tower and a piperylene refining tower in sequence, DCPD is extracted from the tower bottom of the distillation tower, the tower top material of the distillation tower is transferred into the piperylene refining tower, and refined piperylene is extracted from the tower bottom of the piperylene refining tower.
Preferably, in the continuous extraction process in the carbon five separation, the reflux ratio of the first extraction rectifying tower is 7-10, the tower top temperature is 29-30 ℃, and the tower bottom temperature is 32-35 ℃. The first step of extraction and rectification is conventional operation, and only pentane and pentene are needed to be separated.
Preferably, in the continuous extraction process in the carbon five separation, the reflux ratio of the second extraction rectifying tower is 25-30, the tower top temperature is 30-34 ℃, and the tower bottom temperature is 38-42 ℃. In the process of extraction and rectification, isoprene, cyclopentadiene and the like have different solubilities in carbon tetrachloride for extraction and rectification, because the solubilities of each component in carbon tetrachloride are not as great as those of pentane and isoprene in DMF, the extraction process is controlled, more cyclopentadiene is brought back to the tower kettle by using carbon tetrachloride, more isoprene can be extracted from the top of the tower, and isoprene is efficiently separated by using the double difference of the solubilities and the boiling points.
Preferably, in the continuous extraction process in the carbon five separation, the liquid part of the tower bottom of the resolving tower b enters a first solvent regeneration tower, and DMF after impurity removal by the first solvent regeneration tower is returned to the first extraction rectifying tower for recycling.
Preferably, in the continuous extraction process in the carbon five separation, the liquid part of the tower bottom of the resolving tower f enters a solvent regeneration equipment set, the solvent regeneration equipment set comprises a second solvent regeneration tower and a Jiao Zhi dilution tower, and the second solvent regeneration tower removes the carbon tetrachloride solvent distilled from the tower top after the coke in the liquid and returns to the second extraction rectifying tower for recycling; the residue at the bottom of the second solvent regeneration tower is put into the Jiao Zhi dilution tower; adding water into a Jiao Zhi dilution tower for dilution, then evaporating carbon tetrachloride solvent at the top of the tower, and returning to a second extraction rectifying tower for recycling; jiao Zhi the tar residue is discharged from the tower bottom of the dilution tower.
Compared with the prior art, the continuous extraction process in the carbon five separation has the following beneficial effects: according to the invention, the carbon five fraction is separated by two-step continuous extraction, the carbon five fraction is not subjected to rectification separation or/and dimerization in advance, instead, DMF (dimethyl formamide) extraction rectification is directly performed, pentane and pentene are separated, then carbon tetrachloride solvent is used for extraction rectification, isoprene is directly separated, and repeated rectification is not needed in the process, so that the energy consumption can be further reduced. Only the rest cyclopentadiene and piperylene are dimerized, so that the polymerization volume is reduced, and the energy consumption of polymerization is reduced. After dimerization, the dicyclopentadiene and the piperylene can be separated easily by distillation.
Drawings
Fig. 1 is a schematic flow chart of a continuous extraction process in a carbon five separation of the present invention.
Wherein, 1, a first extraction rectifying tower 2, a resolving tower a3, a resolving tower b4, a second extraction rectifying tower 5, a resolving tower e6, a resolving tower f7, a dimerization tank 8, a distillation tower 9, a piperylene refining tower 10, a second solvent regenerating tower 11, a first solvent regenerating tower 12 and a coke diluting tower.
Detailed Description
The invention will be further described with reference to specific examples, of which example 1 is the best practice.
Example 1
1) The cracked carbon five fraction firstly enters a first extraction rectifying tower 1 to directly utilize DMF solvent for continuous extraction rectification, the reflux ratio of the first extraction rectifying tower 1 is controlled to be 8, the tower top temperature is 29 ℃, and the tower bottom temperature is 34 ℃; separating pentane and pentene from the top of the first extractive distillation column 1; the material at the bottom of the first extraction rectifying tower 1 enters a resolving tower a2 and a resolving tower b3 to be operated in series, the material at the bottom of the first extraction rectifying tower 1 enters the resolving tower a2 from the middle part, and DMF solvent extracted from the tower bottom of the resolving tower a2 is returned to the first extraction rectifying tower 1 for recycling; the gas extracted from the tower top of the resolving tower a2 enters the lower part of the resolving tower b3, the liquid part of the tower bottom of the resolving tower b3 enters from the tower top of the resolving tower a2, the liquid rest part of the tower bottom of the resolving tower b3 enters the first solvent regeneration tower 11, DMF after impurity removal by the first solvent regeneration tower 11 returns to the first extraction rectifying tower 1 for recycling, and the material extracted from the tower top of the resolving tower b3 enters the second extraction rectifying tower 4.
2) Continuously extracting and rectifying the second extractive distillation column 4 by using a carbon tetrachloride solvent, adjusting the reflux ratio of the second extractive distillation column 4 to be 28, and controlling the temperature of the top of the column to be 33 ℃ and the temperature of the bottom of the column to be 40 ℃; the part of the tower top extract of the second extractive distillation tower 4 returns to the middle part of the second extractive distillation tower 4 through an external pipeline to participate in extractive distillation again and continuously extract isoprene at the same time; the material at the bottom of the second extraction rectifying tower 4 enters a resolving tower e5 from the middle part, and the carbon tetrachloride solvent extracted from the tower kettle of the resolving tower e5 returns to the second extraction rectifying tower 4 for recycling; the gas extracted from the tower top of the resolving tower e5 enters the lower part of the resolving tower f6, the liquid part of the tower bottom of the resolving tower f6 enters from the tower top of the resolving tower e5, the liquid rest part of the tower bottom of the resolving tower f6 enters a No. two solvent regeneration tower 10, and the No. two solvent regeneration tower 10 evaporates carbon tetrachloride solvent from the tower top after removing the coke in the liquid and returns to the second extraction rectifying tower 4 for recycling; the residue at the bottom of the second solvent regeneration tower 10 is put into the Jiao Zhi dilution tower 12; jiao Zhi diluting the carbon tetrachloride solvent in the tower top after adding water into the diluting tower 12, and returning the carbon tetrachloride solvent to the second extraction rectifying tower 4 for recycling; jiao Zhi the tar residue is discharged from the tower bottom of the dilution tower 12; the materials extracted from the top of the analytic tower f6 enter a dimerization tank 7 to participate in dimerization reaction. While one group of dimerization tanks 7 is polymerizing, the material taken out from the top of the resolving tower f6 is discharged to another group of dimerization tanks 7 connected in parallel. The discharge port of the dimerization tank 7 is connected with a distillation tower 8 and a piperylene refining tower 9 in sequence, DCPD is extracted from the tower kettle of the distillation tower 8, the tower top material of the distillation tower 8 is transferred into the piperylene refining tower 9, and refined piperylene is extracted from the tower kettle of the piperylene refining tower 9.
Example 2
1) The cracked carbon five fraction firstly enters a first extraction rectifying tower 1 to directly utilize DMF solvent for continuous extraction rectification, the reflux ratio of the first extraction rectifying tower 1 is controlled to be 7, the tower top temperature is 29 ℃, and the tower bottom temperature is 32 ℃; separating pentane and pentene from the top of the first extractive distillation column 1; the material at the bottom of the first extraction rectifying tower 1 enters a resolving tower a2 and a resolving tower b3 to be operated in series, the material at the bottom of the first extraction rectifying tower 1 enters the resolving tower a2 from the middle part, and DMF solvent extracted from the tower bottom of the resolving tower a2 is returned to the first extraction rectifying tower 1 for recycling; the gas extracted from the tower top of the resolving tower a2 enters the lower part of the resolving tower b3, the liquid part of the tower bottom of the resolving tower b3 enters from the tower top of the resolving tower a2, the liquid rest part of the tower bottom of the resolving tower b3 enters the first solvent regeneration tower 11, DMF after impurity removal by the first solvent regeneration tower 11 returns to the first extraction rectifying tower 1 for recycling, and the material extracted from the tower top of the resolving tower b3 enters the second extraction rectifying tower 4.
2) Continuously extracting and rectifying the second extractive distillation column 4 by using a carbon tetrachloride solvent, adjusting the reflux ratio of the second extractive distillation column 4 to 25, and controlling the temperature of the top of the column to 30 and the temperature of the bottom of the column to 38 ℃; the part of the tower top extract of the second extractive distillation tower 4 returns to the middle part of the second extractive distillation tower 4 through an external pipeline to participate in extractive distillation again and continuously extract isoprene at the same time; the material at the bottom of the second extraction rectifying tower 4 enters a resolving tower e5 from the middle part, and the carbon tetrachloride solvent extracted from the tower kettle of the resolving tower e5 returns to the second extraction rectifying tower 4 for recycling; the gas extracted from the tower top of the resolving tower e5 enters the lower part of the resolving tower f6, the liquid part of the tower bottom of the resolving tower f6 enters from the tower top of the resolving tower e5, the liquid rest part of the tower bottom of the resolving tower f6 enters a No. two solvent regeneration tower 10, and the No. two solvent regeneration tower 10 evaporates carbon tetrachloride solvent from the tower top after removing the coke in the liquid and returns to the second extraction rectifying tower 4 for recycling; the residue at the bottom of the second solvent regeneration tower 10 is put into the Jiao Zhi dilution tower 12; jiao Zhi diluting the carbon tetrachloride solvent in the tower top after adding water into the diluting tower 12, and returning the carbon tetrachloride solvent to the second extraction rectifying tower 4 for recycling; jiao Zhi the tar residue is discharged from the tower bottom of the dilution tower 12; the materials extracted from the top of the analytic tower f6 enter a dimerization tank 7 to participate in dimerization reaction. While one group of dimerization tanks 7 is polymerizing, the material taken out from the top of the resolving tower f6 is discharged to another group of dimerization tanks 7 connected in parallel. The discharge port of the dimerization tank 7 is connected with a distillation tower 8 and a piperylene refining tower 9 in sequence, DCPD is extracted from the tower kettle of the distillation tower 8, the tower top material of the distillation tower 8 is transferred into the piperylene refining tower 9, and refined piperylene is extracted from the tower kettle of the piperylene refining tower 9.
Example 3
1) The cracked carbon five fraction firstly enters a first extraction rectifying tower 1 to directly utilize DMF solvent for continuous extraction rectification, the reflux ratio of the first extraction rectifying tower 1 is controlled to be 10, the tower top temperature is 30 ℃, and the tower bottom temperature is 35 ℃; separating pentane and pentene from the top of the first extractive distillation column 1; the material at the bottom of the first extraction rectifying tower 1 enters a resolving tower a2 and a resolving tower b3 to be operated in series, the material at the bottom of the first extraction rectifying tower 1 enters the resolving tower a2 from the middle part, and DMF solvent extracted from the tower bottom of the resolving tower a2 is returned to the first extraction rectifying tower 1 for recycling; the gas extracted from the tower top of the resolving tower a2 enters the lower part of the resolving tower b3, the liquid part of the tower bottom of the resolving tower b3 enters from the tower top of the resolving tower a2, the liquid rest part of the tower bottom of the resolving tower b3 enters the first solvent regeneration tower 11, DMF after impurity removal by the first solvent regeneration tower 11 returns to the first extraction rectifying tower 1 for recycling, and the material extracted from the tower top of the resolving tower b3 enters the second extraction rectifying tower 4.
2) The second extractive distillation column 4 is subjected to continuous extractive distillation by using carbon tetrachloride solvent, the reflux ratio of the second extractive distillation column 4 is adjusted to be 30, the temperature of the top of the column is 34 ℃, the temperature of the bottom of the column is 42 ℃, and the part of the top extract of the second extractive distillation column 4 returns to the middle part of the second extractive distillation column 4 through an external pipeline to participate in extractive distillation again and simultaneously continuously extract isoprene; the material at the bottom of the second extraction rectifying tower 4 enters a resolving tower e5 from the middle part, and the carbon tetrachloride solvent extracted from the tower kettle of the resolving tower e5 returns to the second extraction rectifying tower 4 for recycling; the gas extracted from the tower top of the resolving tower e5 enters the lower part of the resolving tower f6, the liquid part of the tower bottom of the resolving tower f6 enters from the tower top of the resolving tower e5, the liquid rest part of the tower bottom of the resolving tower f6 enters a No. two solvent regeneration tower 10, and the No. two solvent regeneration tower 10 evaporates carbon tetrachloride solvent from the tower top after removing the coke in the liquid and returns to the second extraction rectifying tower 4 for recycling; the residue at the bottom of the second solvent regeneration tower 10 is put into the Jiao Zhi dilution tower 12; jiao Zhi diluting the carbon tetrachloride solvent in the tower top after adding water into the diluting tower 12, and returning the carbon tetrachloride solvent to the second extraction rectifying tower 4 for recycling; jiao Zhi the tar residue is discharged from the tower bottom of the dilution tower 12; the materials extracted from the top of the analytic tower f6 enter a dimerization tank 7 to participate in dimerization reaction. While one group of dimerization tanks 7 is polymerizing, the material taken out from the top of the resolving tower f6 is discharged to another group of dimerization tanks 7 connected in parallel. The discharge port of the dimerization tank 7 is connected with a distillation tower 8 and a piperylene refining tower 9 in sequence, DCPD is extracted from the tower kettle of the distillation tower 8, the tower top material of the distillation tower 8 is transferred into the piperylene refining tower 9, and refined piperylene is extracted from the tower kettle of the piperylene refining tower 9.
The results of the product purity (impurity content) measurements of isoprene, DCPD and piperylene obtained in each example are shown in Table 1.
TABLE 1
。
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (7)
1. A continuous extraction process in the separation of carbon five, comprising the steps of:
1) The cracked carbon five fraction firstly enters a first extraction rectifying tower (1) and is subjected to continuous extraction rectification by directly utilizing DMF solvent, and pentane and pentene are separated from the top of the first extraction rectifying tower (1); the material at the bottom of the first extraction rectifying tower (1) enters a front analytical tower group to continuously separate DMF solvent;
2) Continuously extracting and rectifying materials continuously extracted from the top of the front analytical tower group in a second extraction and rectification tower (4) by using a carbon tetrachloride solvent, and continuously extracting isoprene from the top of the second extraction and rectification tower (4); the material at the bottom of the second extraction rectifying tower (4) enters a post-resolving tower group to continuously separate and recycle the carbon tetrachloride solvent;
the rear analytic tower group comprises an analytic tower e (5) and an analytic tower f (6), the analytic tower e (5) and the analytic tower f (6) are operated in series, the material at the bottom of the second extraction rectifying tower (4) enters the analytic tower e (5) from the middle part, and the carbon tetrachloride solvent extracted from the tower kettle of the analytic tower e (5) returns to the second extraction rectifying tower (4) for recycling; the gas extracted from the top of the analytic tower e (5) enters the lower part of the analytic tower f (6), the liquid part of the tower kettle of the analytic tower f (6) enters from the top of the analytic tower e (5), and the material extracted from the top of the analytic tower f (6) enters into a dimerization tank group to participate in dimerization reaction;
the reflux ratio of the first extraction rectifying tower (1) is 7-10, the tower top temperature is 29-30 ℃, and the tower bottom temperature is 32-35 ℃;
the reflux ratio of the second extraction rectifying tower (4) is 25-30, the tower top temperature is 30-34 ℃, and the tower bottom temperature is 38-42 ℃.
2. A continuous extraction process in carbon five separation according to claim 1, characterized in that: the front analytical tower comprises an analytical tower a (2) and an analytical tower b (3), wherein the analytical tower a (2) and the analytical tower b (3) are operated in series, materials at the bottom of the first extraction rectifying tower (1) enter the analytical tower a (2) from the middle part, and DMF solvent extracted from the tower kettle of the analytical tower a (2) is returned to the first extraction rectifying tower (1) for recycling; the gas extracted from the top of the resolving tower a (2) enters the lower part of the resolving tower b (3), the liquid part of the tower bottom of the resolving tower b (3) enters from the top of the resolving tower a (2), and the material extracted from the top of the resolving tower b (3) enters into the second extraction rectifying tower (4).
3. A continuous extraction process in carbon five separation according to claim 1, characterized in that: the dimerization tank group at least comprises two dimerization tanks (7) which are connected in parallel.
4. A continuous extraction process in carbon five separation according to claim 1, characterized in that: the part of the tower top extract of the second extraction rectifying tower (4) returns to the middle part of the second extraction rectifying tower (4) through an external pipeline to participate in extraction rectifying again.
5. A continuous extraction process in carbon five separation according to claim 1, characterized in that: and a discharge hole of the dimerization tank group is sequentially connected with a distillation tower (8) and a piperylene refining tower (9), DCPD is extracted from a tower kettle of the distillation tower (8), a tower top material of the distillation tower (8) is transferred into the piperylene refining tower (9), and refined piperylene is extracted from a tower kettle of the piperylene refining tower (9).
6. A continuous extraction process in carbon five separation according to claim 1, characterized in that: and the liquid part of the tower bottom of the resolving tower b (3) enters a first solvent regeneration tower (11), and DMF after impurity removal by the first solvent regeneration tower (11) is returned to the first extraction rectifying tower (1) for recycling.
7. A continuous extraction process in carbon five separation according to claim 1, characterized in that: the tower bottom liquid part of the resolving tower f (6) enters a solvent regeneration equipment set, the solvent regeneration equipment set comprises a second solvent regeneration tower (10) and a Jiao Zhi dilution tower (12), the second solvent regeneration tower (10) removes coke in the liquid, and carbon tetrachloride solvent is distilled out of the tower top and returned to the second extraction rectifying tower (4) for recycling; the residue at the bottom of the second solvent regeneration tower (10) is put into the Jiao Zhi dilution tower (12); adding water into a Jiao Zhi dilution tower (12) for dilution, evaporating carbon tetrachloride solvent at the top of the tower, and returning the carbon tetrachloride solvent to a second extraction rectifying tower (4) for recycling; jiao Zhi the tar residue is discharged from the tower bottom of the dilution tower (12).
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