CN105481631B - A kind of process for purification of pentadiene - Google Patents
A kind of process for purification of pentadiene Download PDFInfo
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- CN105481631B CN105481631B CN201410482519.8A CN201410482519A CN105481631B CN 105481631 B CN105481631 B CN 105481631B CN 201410482519 A CN201410482519 A CN 201410482519A CN 105481631 B CN105481631 B CN 105481631B
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- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical compound C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000000746 purification Methods 0.000 title abstract description 4
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims abstract description 54
- LPIQUOYDBNQMRZ-UHFFFAOYSA-N cyclopentene Chemical compound C1CC=CC1 LPIQUOYDBNQMRZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000605 extraction Methods 0.000 claims abstract description 35
- 238000000066 reactive distillation Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 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 claims abstract description 16
- 238000000895 extractive distillation Methods 0.000 claims abstract description 11
- 238000004821 distillation Methods 0.000 claims abstract description 6
- PMJHHCWVYXUKFD-UHFFFAOYSA-N piperylene Natural products CC=CC=C PMJHHCWVYXUKFD-UHFFFAOYSA-N 0.000 claims description 68
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 claims description 46
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 238000006471 dimerization reaction Methods 0.000 claims description 21
- 238000010992 reflux Methods 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000003795 desorption Methods 0.000 claims description 17
- 238000007670 refining Methods 0.000 claims description 17
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 abstract 3
- 239000000470 constituent Substances 0.000 abstract 2
- 239000000047 product Substances 0.000 description 20
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 16
- 238000000926 separation method Methods 0.000 description 12
- 239000000539 dimer Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000007086 side reaction Methods 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- QMMOXUPEWRXHJS-UHFFFAOYSA-N pentene-2 Natural products CCC=CC QMMOXUPEWRXHJS-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 150000001993 dienes Chemical class 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000005120 petroleum cracking Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical group CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- -1 wherein Chemical group 0.000 description 2
- YHQXBTXEYZIYOV-UHFFFAOYSA-N 3-methylbut-1-ene Chemical compound CC(C)C=C YHQXBTXEYZIYOV-UHFFFAOYSA-N 0.000 description 1
- 150000001345 alkine derivatives Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of process for purification of pentadiene.Methods described includes:(1) coarse piperyene enters in the middle part of reactive distillation column, and reacted distillation process includes the logistics of pentadiene, pentamethylene and cyclopentene from overhead extraction, and the logistics comprising dicyclopentadiene and heavy constituent is produced from bottom of towe；(2) the reactive distillation column overhead fraction comprising pentadiene, pentamethylene and cyclopentene that step (1) is obtained is introduced into extractive distillation column, extracting rectifying is carried out in the presence of extractant, comprising pentamethylene, cyclopentene component from overhead extraction, the solvent material rich in pentadiene from tower reactor extraction feeding desorber；(3) the extractive distillation column kettle material for obtaining step (2) sends into desorber, and tower top obtains the pentadiene product of high-purity.The present invention solves the shortcoming that dipolymer reactor accessory substance is more, heavy constituent can not be separated, common rectifying tower separating effect is not enough, and the pentadiene product purity finally given is high, high income.
Description
Technical Field
The invention relates to the field of carbon five separation of petroleum cracking, in particular to a method for refining piperylene.
Background
In the process of preparing ethylene by petroleum cracking, a considerable amount of C-V fraction is by-produced, wherein isoprene, cyclopentadiene, piperylene and the like are all important raw materials for organic chemical industry and fine chemical industry. At present, the separation process of cracking carbon five mainly comprises a full separation process mainly for separating isoprene and a simple separation process mainly for separating cyclopentadiene. The total separation process generally adopts a solvent extraction separation method to separate isoprene, cyclopentadiene, piperylene and the like, and solvents commonly used in the process include Acetonitrile (ACN), Dimethylformamide (DMF), N-methylpyrrolidone (NMP) and the like. The simple separation process generally adopts a thermal dimerization method to separate the dicyclopentadiene.
The main components of the piperylene-enriched mixed carbon five (hereinafter referred to as crude piperylene) obtained by the total separation process are piperylene, cyclopentene and cyclopentane, wherein the content of the piperylene is about 65-80 wt%, the total content of the cyclopentene and the cyclopentane is about 18-25 wt%, and the rest contains about 2% of cyclopentadiene and alkyne. Because the purity of the piperylene product is lower, usually less than 80%, the piperylene product can only be used for preparing piperylene resin, and the comprehensive utilization value is single. If the rubber can be further purified and refined to more than 99 percent, the rubber can be used as a raw material of synthetic rubber, and the value of the rubber is greatly improved.
Because the boiling points of the piperylene, the cyclopentene, the cyclopentane and the cyclopentadiene are very close, and various other impurities exist, the refining and purification of the piperylene cannot be realized by the common rectification technology. The purification can be achieved theoretically by precision rectification, but the rectification column requires a very high number of plates, requires a very large reflux ratio in operation, and is very uneconomical in industrial application.
CN101643379 proposes a method for preparing high-purity piperylene, which uses the by-product carbon five fraction of ethylene preparation by petroleum cracking as raw material, and the by-product carbon five fraction is polymerized in a polymerization tank, and then enters an extraction tower for extraction and separation, and the material mainly containing piperylene and an extracting agent obtained in the tower kettle finally enters a desorption tower for desorption and rectification, thus obtaining the high-purity piperylene product. The piperylene obtained by the process is more than or equal to 95 percent, but the dimerization reactor has more side reactions, the yield of the piperylene product is influenced, and meanwhile, the product still contains about 2 percent of heavy components.
CN 1445206 discloses a method for purifying and refining piperylene, wherein, piperylene raw material is rectified and separated to remove heavy components with more than six carbon atoms, materials at the top of the rectifying tower are extracted and rectified to remove light components, the purity of the purified piperylene is more than 95%, but the method can not separate cyclopentadiene from the product, and the product yield is lower, and is 60-75%.
In conclusion, the existing process has the problems of low pentadiene purity, low product recovery rate and the like.
Disclosure of Invention
The invention provides a method for refining piperylene, aiming at solving the problems in the method for refining piperylene in the prior art. The method not only solves the defects that the dimerization reactor has more byproducts and the produced heavy components cannot be separated, but also solves the defect that the separation effect of a common rectifying tower is insufficient, and the finally obtained piperylene product has high purity and high yield.
The invention aims to provide a method for refining piperylene.
The method comprises the following steps:
the coarse pentadiene is made into high-purity pentadiene product through reaction rectification and extraction rectification.
The method comprises the following steps:
(1) crude piperylene enters the middle part of a reactive distillation tower, and a material flow containing piperylene, cyclopentane and cyclopentene is extracted from the tower top in the reactive distillation process, and a material flow containing dicyclopentadiene and heavy components is extracted from the tower bottom;
the reactive distillation process is a process in which the reaction of dimerization of cyclopentadiene into dicyclopentadiene occurs in the distillation process;
(2) introducing the top fraction of the reactive distillation tower containing piperylene, cyclopentane and cyclopentene obtained in the step (1) into an extractive distillation tower, carrying out extractive distillation in the presence of an extraction solvent, extracting components containing cyclopentane and cyclopentene from the top of the tower, and extracting solvent materials rich in piperylene from the bottom of the tower and sending the solvent materials into a desorption tower;
the adopted extractant is dimethylformamide, N-methyl pyrrolidone or acetonitrile;
(3) and (3) feeding the tower bottom material of the extraction and rectification tower obtained in the step (2) into a desorption tower, obtaining a high-purity piperylene product at the tower top, and returning the extracting agent extracted from the tower bottom to the extraction and rectification tower for recycling.
Wherein,
the number of theoretical plates of the reactive distillation tower is 50-140, the operating pressure is 0.1-0.5 MPaG, the temperature of the top of the tower is 55-100 ℃, the temperature of a tower kettle is 80-130 ℃, and the reflux ratio is 2-15; preferably: the number of theoretical plates of the reactive distillation column is 60-120, the operating pressure is 0.15-0.4 MPaG, the temperature of the top of the column is 65-85 ℃, the temperature of the bottom of the column is 95-120 ℃, and the reflux ratio is 4-10; the designed residence time of each tower plate of the reactive distillation tower is 20-40 s; the reaction rectifying tower is preferably a plate rectifying tower;
the number of theoretical plates of the extractive distillation tower is 50-120, the operating pressure is 0-0.3 MPaG, the temperature of the top of the tower is 40-80 ℃, the temperature of a tower kettle is 100-170 ℃, and the reflux ratio is 1-10; preferably: the number of theoretical plates of the extraction rectifying tower is 60-100, the operating pressure is 0.02-0.15 MPaG, the tower top temperature is 45-60 ℃, the tower kettle temperature is 110-150 ℃, and the reflux ratio is 3-7;
the operating pressure of the desorption tower is 0.02-0.1 MPaG, the temperature of the tower kettle is 150-170 ℃, and the reflux ratio is 1-5.
In the step (2), the mass ratio of the extracting agent to the material entering the extraction and rectification tower is 3: 1-12: 1, and preferably 5: 1-10: 1.
The specific technical scheme is as follows:
a refining method of high-purity piperylene comprises the following steps:
(1) crude piperylene enters the middle part of a reactive distillation tower, a material flow containing piperylene, cyclopentane and cyclopentene is extracted from the tower top in the reactive distillation process, a material flow containing dicyclopentadiene and heavy components is extracted from the tower bottom, the reactive distillation tower is a plate-type distillation tower, the number of the theoretical plates is 50-140, the operating pressure is 0.1-0.5 MPaG, the tower top temperature is 55-100 ℃, the tower kettle temperature is 80-130 ℃, the reflux ratio is 2-15, and the reactive distillation process refers to the process of the reaction of dimerization of cyclopentadiene into dicyclopentadiene in the distillation process.
(2) Introducing the top fraction of the reactive distillation tower containing piperylene, cyclopentane and cyclopentene obtained in the step (1) into an extractive distillation tower, carrying out extractive distillation in the presence of an extraction solvent, extracting components containing cyclopentane and cyclopentene from the top of the tower, and extracting solvent materials rich in piperylene from the bottom of the tower and sending the solvent materials into a desorption tower. The number of theoretical plates of the extractive distillation tower is 50-120, the operating pressure is 0-0.3 MPaG, the temperature of the top of the tower is 40-80 ℃, the temperature of the bottom of the tower is 100-170 ℃, and the reflux ratio is 1-10. The mass ratio of the feeding of the extracting agent to the material entering the extraction and rectification tower is 3: 1-12: 1, and the adopted extracting agent is dimethylformamide, N-methylpyrrolidone or acetonitrile.
(3) And (3) feeding the tower bottom material of the extraction and rectification tower obtained in the step (2) into a desorption tower, obtaining a high-purity piperylene product at the tower top, and returning the extracting agent extracted from the tower bottom to the extraction and rectification tower for recycling.
In the step (1) of the method, the principle of reactive distillation is fully utilized, cyclopentadiene is subjected to dimerization reaction in the reactive distillation tower to generate dicyclopentadiene, and meanwhile, dicyclopentadiene is rapidly separated from other carbon five components by utilizing the boiling point difference, so that the aim of simultaneously carrying out reaction and separation is fulfilled.
C5The diolefins in the distillate are subjected to ① self-dimerization reaction, namely the self-dimerization reaction of diolefins such as cyclopentadiene, piperylene and isoprene into dimers, wherein the self-dimerization reaction of cyclopentadiene to dicyclopentadiene is a main reaction, the self-dimerization reaction of piperylene and isoprene to dimer is a side reaction, ② co-dimerization reaction is a side reaction, namely the co-dimerization reaction of cyclopentadiene and piperylene, cyclopentadiene and isoprene to form co-dimers, and ③ polymerization reaction, wherein the dimers and co-dimers formed by the self-dimerization and co-dimerization reactions further react with diolefins to form more than two polymers until polymers with larger molecular weight are formed.
The relative volatility of the C5 hydrocarbons in the presence of the different solvents is shown in table 1. It can be seen that cyclopentadiene and piperylene have close boiling points, have small relative volatility difference in the absence of solvent, are difficult to separate by ordinary rectification, while cyclopentadiene is more soluble in solvent than piperylene in the presence of solvent, and the components such as isopentene, cyclopentane and cyclopentene with high relative volatility can be removed by adopting a one-time extractive rectification method, but cyclopentadiene cannot be removed from piperylene products. CN101643379 adopts a dimerization reactor to remove most cyclopentadiene, but the polymerization reaction time is too long, 24-36 hours are needed, side reactions are more, and heavy components are not separated. CN 1445206 adopts a common rectifying tower to separate and remove heavy components with more than six carbon atoms, cyclopentadiene is not separated, if cyclopentadiene content in crude m-pentadiene is too high, product purity is reduced. Both the two processes restrict the further refining of piperylene, and the purity of piperylene cannot reach more than 99%.
TABLE 1 relative volatility of C5 hydrocarbons in the presence of different solvents
In the method, the reaction rectification function is fully utilized, and the dicyclopentadiene generated by the dimerization reaction of the cyclopentadiene moves to the tower bottom of the reaction rectification tower, so that the concentration of the cyclopentadiene at the tower top tends to be very low. Because the temperature of the rectifying section of the reactive distillation tower is lower relative to the temperature of the dimerization reactor, the retention time is shorter, and the pentadiene moves to the top of the tower, the occurrence of self-dimerization side reaction is effectively reduced, and the yield of the pentadiene product is improved. Meanwhile, the reactive distillation tower removes heavy components with more than six carbons and dimers generated by the reaction from the tower kettle, so that the purity of the piperylene product is improved.
In the method, the defects that the dimerization reactor has more byproducts and the produced heavy components cannot be separated are overcome, the defect that the separation effect of a common rectifying tower is insufficient is overcome, and the finally obtained piperylene product has high purity and high yield.
In order to dimerize cyclopentadiene to dicyclopentadiene in the column as much as possible and to reduce the formation of other dimers, it is necessary to select a plate-type rectification column having a suitable residence time and to use a plate favorable for the rectification of the reaction, for example, a high overflow weir or a vertical sieve plate column.
In conclusion, the reactive distillation method is adopted, the advantages of the dimerization reactor and the distillation tower in the prior art are combined, the process flow is simple, the operation is stable, and the industrialization is easy. The crude piperylene is purified and refined through the flow of reaction rectification and extraction rectification, the purity of the refined high-purity piperylene is more than 99%, and the yield of the product is more than 90%.
Drawings
FIG. 1 is a schematic flow diagram of a piperylene refining process of the present invention;
description of reference numerals:
1, a reaction rectifying tower; 2, an extraction rectifying tower; 3 a desorption tower; 4, coarse piperyene;
5 dicyclopentadiene and heavy components; 6 cyclopentane and cyclopentene; 7 extracting solvent;
8 high purity piperylene product
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
the crude piperylene enters a reaction rectifying tower, the reaction rectifying tower is 100 theoretical plates, the operation pressure is 0.25MPaG, the tower top temperature is 78.3 ℃, the tower kettle temperature is 115.3 ℃, and the reflux ratio is 8. Dicyclopentadiene and heavy components are separated at the bottom of the tower, and light components at the top of the tower enter the middle part of the extraction rectifying tower.
The extractant dimethyl formamide enters an extraction rectification tower from the top of the tower, the mass ratio of the extractant feeding to the material entering the extraction rectification tower is 8:1, the extraction rectification tower is 100 theoretical plates, the operation pressure is 0.02MPaG, the temperature at the top of the tower is 50.3 ℃, the temperature at the bottom of the tower is 123.3 ℃, and the reflux ratio is 6. Cyclopentane, cyclopentene, 2-pentene, isoamylene, isoprene and other substances with high relative volatility are separated from the top of the extraction and rectification tower, and the rich solvent absorbing piperylene enters a desorption tower for desorption.
The operating pressure of the desorption tower is 0.02MPaG, the temperature of the tower kettle is 161 ℃, and the reflux ratio is 2. The extractant obtained from the tower bottom returns to the extraction and rectification tower for recycling, the purity of the high-purity piperylene product obtained from the tower top is 99.5%, and the yield is 90.5%.
Example 2:
the crude piperylene enters a reaction rectifying tower, the reaction rectifying tower is 60 theoretical plates, the operation pressure is 0.15MPaG, the tower top temperature is 73.2 ℃, the tower kettle temperature is 103.3 ℃, and the reflux ratio is 5. Dicyclopentadiene and heavy components are separated at the bottom of the tower, and light components at the top of the tower enter the middle part of the extraction rectifying tower.
The extractant dimethyl formamide enters an extraction rectification tower from the top of the tower, the mass ratio of the extractant feeding to the material entering the extraction rectification tower is 6:1, the extraction rectification tower is 80 theoretical plates, the operation pressure is 0.1MPaG, the temperature at the top of the tower is 58.5 ℃, the temperature at the bottom of the tower is 140.3 ℃, and the reflux ratio is 6. Cyclopentane, cyclopentene, 2-pentene, isoamylene, isoprene and other substances with high relative volatility are separated from the top of the extraction and rectification tower, and the rich solvent absorbing piperylene enters a desorption tower for desorption.
The operating pressure of the desorption tower is 0.05MPaG, the temperature of the tower kettle is 168 ℃, and the reflux ratio is 1. The extractant obtained from the tower bottom returns to the extraction and rectification tower for recycling, the purity of the high-purity piperylene product obtained from the tower top is 99.1%, and the yield is 93.2%.
Claims (7)
1. A method for refining piperylene, the method comprising:
(1) crude piperylene enters the middle part of a reactive distillation tower, and a material flow containing piperylene, cyclopentane and cyclopentene is extracted from the tower top in the reactive distillation process, and a material flow containing dicyclopentadiene and heavy components is extracted from the tower bottom;
the reactive distillation process is a process in which the reaction of dimerization of cyclopentadiene into dicyclopentadiene occurs in the distillation process;
(2) introducing the top fraction of the reactive distillation tower containing piperylene, cyclopentane and cyclopentene obtained in the step (1) into an extractive distillation tower, carrying out extractive distillation in the presence of an extraction solvent, extracting components containing cyclopentane and cyclopentene from the top of the tower, and extracting solvent materials rich in piperylene from the bottom of the tower and sending the solvent materials into a desorption tower;
the adopted extractant is dimethylformamide, N-methyl pyrrolidone or acetonitrile;
(3) feeding the tower bottom material of the extraction and rectification tower obtained in the step (2) into a desorption tower, obtaining a high-purity piperylene product at the tower top, and returning the extracting agent extracted from the tower bottom to the extraction and rectification tower for recycling;
the number of theoretical plates of the reactive distillation tower is 50-140, the operating pressure is 0.1-0.5 MPaG, the temperature of the top of the tower is 55-100 ℃, the temperature of the bottom of the tower is 80-130 ℃, and the reflux ratio is 2-15.
2. A method of refining piperylene as defined in claim 1, wherein:
the number of theoretical plates of the extractive distillation tower is 50-120, the operating pressure is 0-0.3 MPaG, the temperature of the top of the tower is 40-80 ℃, the temperature of the bottom of the tower is 100-170 ℃, and the reflux ratio is 1-10.
3. A method of refining piperylene as defined in claim 1, wherein:
the reaction rectifying tower is a plate rectifying tower.
4. A method of refining piperylene as defined in claim 1, wherein:
in the step (2), the mass ratio of the extracting agent to the material entering the extraction and rectification tower is 3: 1-12: 1.
5. A process for refining piperylene as claimed in claim 4, wherein:
the mass ratio of the extracting agent to the material entering the extraction and rectification tower is 5: 1-10: 1.
6. A method of refining piperylene as defined in claim 2, wherein:
the number of theoretical plates of the reactive distillation column is 60-120, the operating pressure is 0.15-0.4 MPaG, the temperature of the top of the column is 65-85 ℃, the temperature of the bottom of the column is 95-120 ℃, and the reflux ratio is 4-10;
the number of theoretical plates of the extraction rectifying tower is 60-100, the operating pressure is 0.02-0.15 MPaG, the tower top temperature is 45-60 ℃, the tower kettle temperature is 110-150 ℃, and the reflux ratio is 3-7;
the operating pressure of the desorption tower is 0.02-0.1 MPaG, the temperature of the tower kettle is 150-170 ℃, and the reflux ratio is 1-5.
7. A process for refining piperylene as defined in claim 6, wherein:
the designed residence time of each tower plate of the reactive distillation tower is 20-40 s.
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|---|---|---|---|---|
| CN1412165A (en) * | 2001-10-12 | 2003-04-23 | 中国石油化工股份有限公司 | Separation method of cracked C5 fraction |
| CN1445206A (en) * | 2002-03-19 | 2003-10-01 | 中国石化上海石油化工股份有限公司 | Method for purifying and refining piperyene |
| CN101643379A (en) * | 2009-08-31 | 2010-02-10 | 山东玉皇化工有限公司 | Preparation method of high-purity 1,3-pentadiene |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW583178B (en) * | 2001-09-29 | 2004-04-11 | China Petrochemical Corp | Process for separating C5 cuts obtained from a petroleum cracking process |
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| CN1412165A (en) * | 2001-10-12 | 2003-04-23 | 中国石油化工股份有限公司 | Separation method of cracked C5 fraction |
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