CN101289363B - Process for preparing 1-amylene by separating C5 distillate of petroleum - Google Patents
Process for preparing 1-amylene by separating C5 distillate of petroleum Download PDFInfo
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- CN101289363B CN101289363B CN 200710039675 CN200710039675A CN101289363B CN 101289363 B CN101289363 B CN 101289363B CN 200710039675 CN200710039675 CN 200710039675 CN 200710039675 A CN200710039675 A CN 200710039675A CN 101289363 B CN101289363 B CN 101289363B
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Abstract
The invention discloses a method which is used for preparing 1-pentene by separating petroleum C5 fraction and takes raffinate petroleum C5 fraction obtained after separating diolefin and isoamylene by extracting as raw materials. The process comprises that the raw materials are distilled and separated so as to remove heavy components, the materials richly containing 1-pentene are obtained in a column top, and the materials with heavy components are discharged from the column bottom; the materials in the column top obtained in the process 1 are extracted and distilled, the extractant is N and N-dimethylformamide, the feeding weight ratio of the raw materials and the extractant is 1:5 to 1:12, C5 saturated hydrocarbon materials are discharged from the column top, and materials richly containing 1-pentene and the extractant are obtained in the column bottom; the materials in the column bottom obtained in the process 2 are distilled so as to recycle the extractant, the crude product of 1-pentene are obtained from the column top, the extractant is obtained in the column bottom, and the extractant can be recycled; and the crude product of 1-pentene obtained in the process 3 is distilled and refined so asto remove light components, the materials in the column bottom are taken and a refined product of 1-pentene is obtained. By processing at a much deeper degree, the method of the invention solves a technical problem that 1-pentene in C5 fraction can not be utilized by the prior art.
Description
Technical field
The present invention relates to the separation method of Petrocarbon 5 distillate, particularly separated the method for producing the 1-amylene by technological processs such as rectifying, extracting rectifyings by the Petrocarbon 5 distillate.
Background technology
The a considerable amount of C5 fractions of process by-product of petroleum cracking ethene processed, its amount is about 10% of ethylene yield, is the effective way that improves the ethylene production economic benefit to the comprehensive utilization of C5 fraction.The comprehensive utilization of C5 fraction at present is mainly extracting to be carried out in C5 fraction separate, and obtains being worth diolefin and the isopentene such as higher m-pentadiene, isoprene and dicyclopentadiene.Separate the remaining Petrocarbon five cut materials of taking out of diolefin and isopentene through extracting and accounted for 10～15% of C5 fraction raw material.The component boiling point of taking out remaining oil C5 fraction is very approaching, its separation difficulty, and the oil that generally only acts as a fuel uses.Take out remaining Petrocarbon five cut materials for this, existing deep processing and utilization is to obtain the mixture of pentane and iso-pentane by full hydrogenation, introduces as Chinese patent ZL02145057.9, ZL02145056.0.The mixture of pentane, pentane and iso-pentane can be used as whipping agent, extraction agent, green refrigerant and organic solvent etc., and the method has further improved the utility value of taking out remaining oil C5 fraction.But, in fact take out and contain 30～40% the amylene of having an appointment in remaining Petrocarbon five cut materials and (comprise 1-amylene and 2-amylene, both ratios are about 1: 2), and the amylene higher industrial chemicals that is using value, be the important monomer that polymer modification and complicated organometallics synthesize, medicine is synthetic as the 1-amylene, its price is also far above pentane and iso-pentane.The defective of full hydrogenation technique is to make amylene to be utilized.
Summary of the invention
The invention provides a kind of method produce the 1-amylene of being separated by the Petrocarbon 5 distillate, it is by carrying out the more processing of the degree of depth to the oil C5 fraction, can't utilize this technical problem of 1-amylene in C5 fraction to solve prior art.
Below the detailed technical scheme of the present invention:
A kind of method produce the 1-amylene of being separated by the Petrocarbon 5 distillate, the method have been separated take extracting and have been taken out remaining oil C5 fraction as raw material after diolefin and isopentene, and its process comprises:
1) raw material carries out rectifying separation to remove heavy constituent, and tower top temperature is 26～32 ℃, and the tower reactor temperature is 35～45 ℃, and working pressure is normal pressure, and reflux ratio is 20～50, is got the material of enrichment 1-amylene by tower top, and tower reactor is discharged the heavy constituent material;
2) the tower top material of process 1 carries out extracting rectifying, extraction agent is N, dinethylformamide, material is 1: 5～1: 12 with the feed weight ratio of extraction agent, the extractant feed temperature is 20～45 ℃, tower top temperature is 25～36 ℃, the tower reactor temperature is 60～120 ℃, and working pressure is normal pressure, and reflux ratio is 1～6, tower top is discharged carbon five stable hydrocarbon materials, and tower reactor gets the material of enrichment 1-amylene and extraction agent;
3) the tower reactor material of process 2 carries out rectifying to reclaim extraction agent, and tower top temperature is 26～32 ℃, and the tower reactor temperature is 110～150 ℃, and working pressure is normal pressure, and reflux ratio is 1～6, and tower top gets the thick product of 1-amylene, and tower reactor gets extraction agent, the extraction agent recycled;
4) the thick product of 1-amylene that obtains of process 3 carries out that rectified purified tower top temperature is 25～29 ℃ to remove light constituent, and the tower reactor temperature is 35～45 ℃, working pressure is normal pressure, reflux ratio is 20～50, and tower top is discharged the light constituent material, gets the tower reactor material and gets 1-amylene purified product.
The described tower top temperature of said process 1 is preferably 27～30 ℃, and the tower reactor temperature is preferably 38～42 ℃, and reflux ratio is preferably 30～40;
It is 1: 6～1: 10 that the feed weight of the described material of process 2 and extraction agent cans be compared to most, and the extractant feed temperature is preferably 30～40 ℃, and the tower reactor temperature is preferably 65～110 ℃, and reflux ratio is preferably 1～4;
The described tower top temperature of process 3 is preferably 27～30 ℃, and the tower reactor temperature is preferably 120～140 ℃, and reflux ratio is preferably 1～4;
The described tower reactor temperature of process 4 is preferably 38～42 ℃, and reflux ratio is preferably 30～40.
Key of the present invention is to have selected a kind of suitable technique, effectively to isolate 1-amylene product from take out remaining oil C5 fraction.Whole technological process mainly comprises four parts, wherein:
The purpose of process 1 is the heavy constituent that first cuts away in raw material, and its amount accounts for 60% of raw material, and component mainly comprises Skellysolve A, 2-amylene and a small amount of isopentene.The atmospheric boiling point of these heavy constituent materials and 1-amylene are comparatively approaching, therefore adopt precise distillation.Rectifying tower can adopt packing tower, and theoretical plate number is at least 40, generally can be no more than 100, is advisable with 40～80, and it is comparatively suitable near the position of tower reactor that the opening for feed of raw material is arranged in stripping section.
The purpose of process 2 is remaining saturated alkanes in the tower top material that obtains of removal process 1, mainly comprises iso-pentane.Because iso-pentane is difficult to be separated with the 1-amylene with the method for rectifying, therefore adopt extracting rectifying.The key of process 2 is the selection of extraction agent and the selection of processing condition.Extractive distillation column can adopt packing tower, and theoretical plate number is advisable with 30～60.The same with most of extraction rectification techniques, extraction agent is preferably by the top charging of tower, and material preferably by in stripping section near the position charging of tower reactor.
Process 3 is simple rectifying, its objective is to realize separating of extraction agent and carbon five materials, because both atmospheric boiling points are poor larger, can realize both separation fully by the simple rectifying once the step.The extraction agent that reclaims can return to the abstraction distillation system recycled.Rectifying tower can adopt packing tower, and theoretical plate number is advisable with 15～30, material preferably by in stripping section near the position charging of tower reactor.
Process 4 is also precise distillation, its objective is that the thick product of 1-amylene that process 3 is obtained makes with extra care, and isolates light constituent impurity.Rectifying tower can adopt packing tower, and theoretical plate number is at least 40, generally can be no more than 100, is advisable with 40～80, and it is comparatively suitable near the position of tower reactor that the opening for feed of raw material is arranged in stripping section.
Positive effect of the present invention is to take out by further raising the working depth of remaining Petrocarbon five cut materials, has obtained higher carbon five products of economic worth, and the more perfect comprehensive utilization means of C 5 fraction are exhausted the waste that has reduced possibly petroleum resources.
Below further describe details of the present invention by specific embodiment.In embodiment, 1-amylene product yield is defined as:
The remaining oil C5 fraction fraction raw material chief component of taking out that each embodiment uses sees Table 1.
Table 1.
| Component | Content (% by weight) |
| The 1-amylene | 18.2 |
| The 2-amylene | 27.6 |
| Skellysolve A | 42.3 |
| Iso-pentane | 5.8 |
| Isopentene | 4.2 |
| Isosorbide-5-Nitrae-pentadiene | 1.2 |
| The materials such as other hydro carbons | Surplus |
Embodiment
[embodiment 1～10]
Separate by following process forming remaining Petrocarbon five feedstock of taking out as listed in table 1:
1) raw material carries out rectifying separation to remove heavy constituent, and rectifying tower is packing tower, and theoretical plate number is 50, and raw material is by the position charging of the 40th column plate, and input speed is 1.0kg/h.Working pressure is normal pressure, and it is 2 listed that other rectification process condition sees Table.Got the material of enrichment 1-amylene by tower top, tower reactor is discharged the heavy constituent material;
2) the tower top material of process 1 carries out extracting rectifying, and extraction agent is DMF.Extractive distillation column is packing tower, and theoretical plate number is 40, and material is by the position charging of the 32nd column plate, and extraction agent is by the position charging of the 4th column plate.Working pressure is normal pressure, and it is 3 listed that other extraction rectification technique condition sees Table.Tower top is discharged carbon five stable hydrocarbon materials, and tower reactor gets the material of enrichment 1-amylene and extraction agent;
3) the tower reactor material of process 2 carries out rectifying to reclaim extraction agent, and rectifying tower is packing tower, and theoretical plate number is 20, and raw material is by the position charging of the 16th column plate.Working pressure is normal pressure, and it is 4 listed that other rectification process condition sees Table.Tower top gets the thick product of 1-amylene, and tower reactor gets extraction agent, and extraction agent returns to the abstraction distillation system recycled;
4) the thick product of 1-amylene that obtains of process 3 carries out that rectified purified rectifying tower is packing tower to remove light constituent, and theoretical plate number is 50, and raw material is by the position charging of the 40th column plate.Working pressure is normal pressure, and it is 5 listed that other rectification process condition sees Table.Tower top is discharged the light constituent material, gets the tower reactor material and gets 1-amylene purified product.
It is 6 listed that product yield, the product purity of each embodiment 1-amylene sees Table.
Table 2.
| ? | Tower top temperature (℃) | The tower reactor temperature (℃) | Reflux ratio |
| Embodiment 1 | 26 | 35 | 50 |
| Embodiment 2 | 27 | 36 | 38 |
| Embodiment 3 | 29 | 38 | 40 |
| Embodiment 4 | 29 | 38 | 20 |
| Embodiment 5 | 30 | 39 | 30 |
| Embodiment 6 | 30 | 39 | 34 |
| Embodiment 7 | 30 | 40 | 32 |
| Embodiment 8 | 28 | 41 | 45 |
| Embodiment 9 | 30 | 42 | 36 |
| Embodiment 10 | 32 | 45 | 25 |
[0034]Table 3.
| ? | Material/extraction agent (feed weight ratio) | The extractant feed temperature (℃) | Tower top temperature (℃) | The tower reactor temperature (℃) | Reflux ratio |
| Embodiment 1 | 1:12 | 45 | 25 | 120 | 6 |
| Embodiment 2 | 1:10 | 42 | 27 | 110 | 3 |
| Embodiment 3 | 1:9 | 39 | 28 | 92 | 4 |
| Embodiment 4 | 1:8.5 | 35 | 28 | 87 | 2 |
| Embodiment 5 | 1:6.5 | 38 | 29 | 67 | 3 |
| Embodiment 6 | 1:8 | 39 | 29 | 81 | 3 |
| Embodiment 7 | 1:7 | 36 | 29 | 73 | 2 |
| Embodiment 8 | 1:7.5 | 40 | 27 | 76 | 4 |
| Embodiment 9 | 1:5 | 30 | 32 | 60 | 2 |
| Embodiment 10 | 1:6 | 20 | 36 | 65 | 1 |
Table 4.
| ? | Tower top temperature (℃) | The tower reactor temperature (℃) | Reflux ratio |
| Embodiment 1 | 26 | 110 | 6 |
| Embodiment 2 | 27 | 140 | 4 |
| Embodiment 3 | 29 | 138 | 2 |
| Embodiment 4 | 29 | 135 | 3 |
| Embodiment 5 | 30 | 137 | 2 |
| Embodiment 6 | 29 | 139 | 2 |
| Embodiment 7 | 29 | 145 | 2 |
| Embodiment 8 | 27 | 130 | 3 |
| Embodiment 9 | 30 | 120 | 1 |
| Embodiment 10 | 32 | 150 | 1 |
[0038]Table 5.
| ? | Tower top temperature (℃) | The tower reactor temperature (℃) | Reflux ratio |
| Embodiment 1 | 25 | 35 | 50 |
| Embodiment 2 | 26 | 37 | 36 |
| Embodiment 3 | 27 | 38 | 30 |
| Embodiment 4 | 28 | 38 | 32 |
| Embodiment 5 | 28 | 39 | 38 |
| Embodiment 6 | 29 | 39 | 28 |
| Embodiment 7 | 28 | 40 | 35 |
| Embodiment 8 | 27 | 41 | 20 |
| Embodiment 9 | 29 | 42 | 34 |
| Embodiment 10 | 29 | 45 | 40 |
Table 6.
| ? | 1-amylene product yield (%) | 1-amylene product purity (%) |
| Embodiment 1 | 77.2 | 96.6 |
| Embodiment 2 | 77.5 | 96.5 |
| Embodiment 3 | 79.9 | 97.1 |
| Embodiment 4 | 80.5 | 97.3 |
| Embodiment 5 | 81.0 | 97.2 |
| Embodiment 6 | 80.8 | 97.5 |
| Embodiment 7 | 81.3 | 97.4 |
| Embodiment 8 | 78.2 | 97.0 |
| Embodiment 9 | 82.2 | 96.7 |
| Embodiment 10 | 80.2 | 96.8 |
Claims (5)
1. method of being separated to produce the 1-amylene by the Petrocarbon 5 distillate, the method have been separated take extracting and have been taken out remaining oil C5 fraction as raw material after diolefin and isopentene, and its process comprises:
1) raw material carries out rectifying separation to remove heavy constituent, and tower top temperature is 26～32 ℃, and the tower reactor temperature is 35～45 ℃, and working pressure is normal pressure, and reflux ratio is 20～50, is got the material of enrichment 1-amylene by tower top, and tower reactor is discharged the heavy constituent material;
2) the tower top material of process 1 carries out extracting rectifying, extraction agent is N, dinethylformamide, material is 1: 5～1: 12 with the feed weight ratio of extraction agent, the extractant feed temperature is 20～45 ℃, tower top temperature is 25～36 ℃, the tower reactor temperature is 60～120 ℃, and working pressure is normal pressure, and reflux ratio is 1～6, tower top is discharged carbon five stable hydrocarbon materials, and tower reactor gets the material of enrichment 1-amylene and extraction agent;
3) the tower reactor material of process 2 carries out rectifying to reclaim extraction agent, and tower top temperature is 26～32 ℃, and the tower reactor temperature is 110～150 ℃, and working pressure is normal pressure, and reflux ratio is 1～6, and tower top gets the thick product of 1-amylene, and tower reactor gets extraction agent, the extraction agent recycled;
4) the thick product of 1-amylene that obtains of process 3 carries out that rectified purified tower top temperature is 25～29 ℃ to remove light constituent, and the tower reactor temperature is 35～45 ℃, working pressure is normal pressure, reflux ratio is 20～50, and tower top is discharged the light constituent material, gets the tower reactor material and gets 1-amylene purified product.
2. the method for producing the 1-amylene of being separated by the Petrocarbon 5 distillate according to claim 1, is characterized in that the described tower top temperature of process 1 is 27～30 ℃, and the tower reactor temperature is 38～42 ℃, and reflux ratio is 30～40.
3. the method produce the 1-amylene of being separated by the Petrocarbon 5 distillate according to claim 1, it is characterized in that the described material of process 2 and the feed weight ratio of extraction agent are 1: 6～1: 10, the extractant feed temperature is 30～40 ℃, and the tower reactor temperature is 65～110 ℃, and reflux ratio is 1～4.
4. the method for producing the 1-amylene of being separated by the Petrocarbon 5 distillate according to claim 1, is characterized in that the described tower top temperature of process 3 is 27～30 ℃, and the tower reactor temperature is 120～140 ℃, and reflux ratio is 1～4.
5. the method for producing the 1-amylene of being separated by the Petrocarbon 5 distillate according to claim 1, is characterized in that the described tower reactor temperature of process 4 is 38～42 ℃, and reflux ratio is 30～40.
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| CN103333042B (en) * | 2013-07-24 | 2015-09-23 | 上海派尔科化工材料有限公司 | A kind of preparation method of amylene |
| CN103333041B (en) * | 2013-07-24 | 2015-09-23 | 上海派尔科化工材料有限公司 | A kind of preparation method of positive amylene |
| CN104557410B (en) * | 2013-10-11 | 2017-09-29 | 中国石油化工股份有限公司 | A kind of method of the amylene of high-purity 1 |
| CN104557407B (en) * | 2013-10-11 | 2017-10-27 | 中国石油化工股份有限公司 | A kind of 2 pentene isomerization is the method for 1 amylene |
| CN104557409B (en) * | 2013-10-11 | 2018-03-20 | 中国石油化工股份有限公司 | The method of the amylene of high-purity 1 |
| CN104370678B (en) * | 2014-11-15 | 2015-12-30 | 太原理工大学 | Alkene method of comprehensive utilization in a kind of F-T synthesis light ends oil |
| CN105061128B (en) * | 2015-07-31 | 2016-08-10 | 濮阳市新豫石油化工有限责任公司 | A kind of the most poly-C5 of oil extracts dechlorination method |
| CN109305877A (en) * | 2017-07-26 | 2019-02-05 | 抚顺伊科思新材料有限公司 | Thick light dydrocarbon produces high alkene light dydrocarbon, pentane, isopentane and pentamethylene method |
| CN112341306B (en) * | 2019-08-06 | 2024-01-19 | 内蒙古伊泰煤基新材料研究院有限公司 | Eluent and method for separating alkane and alkene by simulated moving bed |
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| CN1160035A (en) * | 1996-03-20 | 1997-09-24 | 中国石油化工总公司 | Method for separation of petroleum cracking C5 fraction by liquid phase feeding extraction rectification |
| CN1796341A (en) * | 2004-12-24 | 2006-07-05 | 中国石化上海石油化工股份有限公司 | Refining separation method for coarse piperyene |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4348260A (en) * | 1979-12-06 | 1982-09-07 | Nippon Zeon Co., Ltd. | Method for inhibiting polymerization of conjugated dienes |
| CN1160035A (en) * | 1996-03-20 | 1997-09-24 | 中国石油化工总公司 | Method for separation of petroleum cracking C5 fraction by liquid phase feeding extraction rectification |
| CN1796341A (en) * | 2004-12-24 | 2006-07-05 | 中国石化上海石油化工股份有限公司 | Refining separation method for coarse piperyene |
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