CN104418694B - Method for preparing high-purity piperylene by acetonitrile method - Google Patents
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 38
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical group C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 title abstract description 10
- PMJHHCWVYXUKFD-UHFFFAOYSA-N piperylene Natural products CC=CC=C PMJHHCWVYXUKFD-UHFFFAOYSA-N 0.000 title abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 65
- 238000000605 extraction Methods 0.000 claims abstract description 48
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 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 13
- 238000006471 dimerization reaction Methods 0.000 claims abstract description 8
- 238000005336 cracking Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000010992 reflux Methods 0.000 claims description 15
- 238000006116 polymerization reaction Methods 0.000 claims description 13
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical compound CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 claims description 10
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 5
- 239000000470 constituent Substances 0.000 claims description 5
- 150000001941 cyclopentenes Chemical class 0.000 claims description 5
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 5
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- OHBTULDTCSOWOY-UHFFFAOYSA-N [C].C=C Chemical compound [C].C=C OHBTULDTCSOWOY-UHFFFAOYSA-N 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 238000005406 washing Methods 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract description 2
- 239000005977 Ethylene Substances 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 2
- 239000012141 concentrate Substances 0.000 abstract 1
- 238000012719 thermal polymerization Methods 0.000 abstract 1
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical group CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 10
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PMJHHCWVYXUKFD-PLNGDYQASA-N (3z)-penta-1,3-diene Chemical compound C\C=C/C=C PMJHHCWVYXUKFD-PLNGDYQASA-N 0.000 description 2
- QMMOXUPEWRXHJS-HWKANZROSA-N (e)-pent-2-ene Chemical group CC\C=C\C QMMOXUPEWRXHJS-HWKANZROSA-N 0.000 description 2
- QMMOXUPEWRXHJS-HYXAFXHYSA-N (z)-pent-2-ene Chemical group CC\C=C/C QMMOXUPEWRXHJS-HYXAFXHYSA-N 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 1
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- -1 be in cracked Chemical compound 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing high-purity piperylene by an acetonitrile method; it uses the pentadiene concentrate obtained in the course of ethylene cracking carbon five separation as raw material, and makes it pass through thermal polymerization still thermal dimerization, and makes it enter into heavy component removing tower to remove dicyclopentadiene, and the material obtained from tower top is passed into light component removing tower to remove light component, and the material obtained from tower bottom is passed into primary extraction rectification tower to make extraction separation, and the material obtained from tower bottom and mainly uses pentadiene and extracting agent is passed into primary resolution tower to make resolution rectification, and the material obtained from tower top is passed into secondary extraction rectification tower to make rectification, and the crude pentadiene obtained from tower top is passed into water-washing tower to remove acetonitrile and water, so that the high-purity pentadiene with purity above 98% can be obtained, and the dicyclopentadiene with purity above 60% can be produced.
Description
Technical field
The invention belongs to chemical technology field, particularly a kind of acetonitrile method prepares the method for high purity (>=98%) m-pentadiene.
Background technology
Along with the fast development of ethylene industry, the source of cracked, C 5 fraction is also increasingly abundant, its output is different because of the difference of cracking stock, generally to account for 10% ~ 20%, containing a large amount of diolefine and monoolefine in cracked, C 5 fraction, olefin(e) centent accounts for 85% ~ 95% of C 5 fraction, that wherein content is more is isoprene (IP), cyclopentadiene/dicyclopentadiene (CDP/DCPD) and m-pentadiene (PIP), its content is respectively at 15 ~ 23% (massfractions, lower same), 14 ~ 17% and about 13 ~ 25% fluctuations, three accounts for 40% ~ 55% of C 5 fraction.These diolefins are owing to having special molecular structure, and chemical property is active, and can synthesize many important high value added products, be the precious resources of chemical utilization.
M-pentadiene also claims 1,3-pentadiene (PD), be in cracked, C 5 fraction content higher, apply one of more component, when taking extraction fractional distillation separating isoprene, the m-pentadiene concentrated solution that massfraction is 70% ~ 85% can be obtained simultaneously, further rectifying massfraction is the m-pentadiene of 90% ~ 99%.Different according to purposes, also by the further rectifying of cut after hot dimerization method separating cyclopentadiene, the m-pentadiene enriched material that massfraction is 50% ~ 75% can be obtained.Be mainly used to produce pentadiene resin, epoxy curing agent, methyl tetrahydro phthalic anhydride, rubber viscosity increaser and tackiness agent etc.
Summary of the invention
The object of this invention is to provide a kind of method that acetonitrile method prepares high purity m-pentadiene.Present method with the m-pentadiene enriched material obtained in cracking of ethylene carbon five sepn process for raw material, adopt hot dimerization, de-heavy, de-light, acetonitrile twice extracting rectifying and washing process, obtain high purity (more than 98%) m-pentadiene, and the dicyclopentadiene of attached product part purity more than 60%, adopt twice extraction and washing process, the advantage better can remove the impurity in the middle of m-pentadiene, there is rational technology, product purity is high, being easy to suitability for industrialized production.
A kind of acetonitrile method of the present invention prepares the method for high purity m-pentadiene, comprises the following steps:
(1) m-pentadiene enriched material enters hot polymerization still and carries out hot dimerization, and feeding temperature is 20 ~ 80 DEG C, polymerization temperature 60 ~ 140 DEG C, and polymerization time is 1 ~ 15 hour, and the hot dimerization of the cyclopentadiene in raw material is dicyclopentadiene;
(2) hot polymerization still material out enters weight-removing column, remove dicyclopentadiene heavy constituent in material, tower top obtains the m-pentadiene enriched material of purifying further, tower reactor obtains the dicyclopentadiene that purity is more than or equal to 60%, weight-removing column operational condition: tower top temperature is 30 ~ 90 DEG C, bottom temperature is 85 ~ 150 DEG C, and working pressure is 0.1 ~ 1MPa, and reflux ratio is 1 ~ 20;
(3) weight-removing column material out enters lightness-removing column, remove alkane and carbon four diolefin light constituent in material, the light constituent that it is main component that tower top obtains with Skellysolve A and 2-methyl-2-butene, tower reactor obtains m-pentadiene enriched material concentrated further, lightness-removing column operational condition: tower top temperature is 40 ~ 100 DEG C, bottom temperature is 70 ~ 120 DEG C, and working pressure is 0.1 ~ 1MPa, and reflux ratio is 10 ~ 60;
(4) m-pentadiene enriched material material out at the bottom of lightness-removing column enters single extraction tower and carries out extracting and separating, remove component close with m-pentadiene boiling point in material, the hydrocarbon mixture that it is main component that tower top obtains with cyclopentenes and pentamethylene, the material that it is main component that tower reactor obtains with m-pentadiene and extraction agent, wherein extraction agent is the acetonitrile solution of acetonitrile or moisture 2 ~ 20wt%, extraction agent and material feeding mass ratio are 0.5 ~ 15, extractant feed temperature is 15 ~ 75 DEG C, extraction tower operational condition: tower top temperature is 40 ~ 100 DEG C, bottom temperature is 70 ~ 120 DEG C, working pressure is 0.1 ~ 1MPa, reflux ratio is 1 ~ 30,
(5) m-pentadiene out at the bottom of single extraction tower and extraction agent are that the material of main component enters one parsing tower and carries out parsing rectifying, tower top obtains taking m-pentadiene as the enriched material of main component, tower reactor obtains the extraction agent based on acetonitrile and water, return extraction tower to recycle, Analytic Tower operational condition: tower top temperature is 30 ~ 90 DEG C, bottom temperature is 70 ~ 120 DEG C, and working pressure is 0.1 ~ 1MPa, and reflux ratio is 1 ~ 30;
(6) one parsing tower top out be that the enriched material material of main component enters reextraction tower with m-pentadiene, tower top obtains coarse piperyene, tower reactor obtains taking extraction agent as the material of main component, wherein extraction agent is the acetonitrile solution of acetonitrile or moisture 2 ~ 20wt%, extraction agent and material feeding mass ratio are 1 ~ 15, extractant feed temperature is 20 ~ 70 DEG C, extraction tower operational condition: tower top temperature is 40 ~ 90 DEG C, bottom temperature is 70 ~ 110 DEG C, working pressure is 0.1 ~ 1MPa, and reflux ratio is 5 ~ 20;
(7) reextraction column overhead coarse piperyene material out enters water wash column, tower top obtains high purity m-pentadiene, tower reactor obtains the water of purity more than 99%, the charge-mass ratio of water and material is 1 ~ 20, water wash column operational condition: tower top temperature is 10 ~ 50 DEG C, bottom temperature is 30 ~ 80 DEG C, and working pressure is 0.1 ~ 1MPa.
The present invention takes hot dimerization, the technique of de-heavy, de-light, acetonitrile reextraction rectifying and washing, the high purity m-pentadiene of more than 98% can be obtained, and the dicyclopentadiene of attached product part purity more than 60%, owing to adopting twice extraction and washing process, therefore, it is possible to better remove the impurity in the middle of m-pentadiene, there is the advantage that technique is simple, yield purity is high, be easy to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Wherein, R-101 hot polymerization still, T-101 weight-removing column, T-102 lightness-removing column, T-103 single extraction tower, T-104 one parsing tower, T-105 reextraction tower, T-106 water wash column.
Embodiment
Be further detailed below in conjunction with the embodiment of accompanying drawing to method provided by the present invention, all the other are various, and can to realize method of the present invention all similar, and the present invention repeats no more.
Embodiment 1 ~ 4
(1) mainly form in table 1 with the m-pentadiene enriched material 1(obtained in cracking of ethylene carbon five sepn process) enter hot polymerization still R-101 and carry out hot dimerization, each embodiment polymeric kettle operational condition is in table 2.
(2) hot polymerization still R-101 material 2 out enters weight-removing column T-101, tower top obtains the m-pentadiene enriched material 3 of purifying further, tower reactor obtains the dicyclopentadiene 4 that purity is greater than 60%, weight-removing column theoretical plate number 80, material 2 enters from the 44th block of column plate, and each embodiment weight-removing column operational condition is in table 3.
(3) weight-removing column T-101 material 3 out enters lightness-removing column T-102, tower top obtains the light constituent 5 based on Skellysolve A and 2-methyl-2-butene, tower reactor obtains m-pentadiene enriched material 6 concentrated further, lightness-removing column theoretical plate number 120, material 3 enters from the 60th block of column plate, and each embodiment lightness-removing column operational condition is in table 4.
(4) lightness-removing column T-102 material 6 out enters single extraction tower T-103 and carries out extracting and separating, tower top obtains the hydrocarbon mixture 7 based on cyclopentenes and pentamethylene, tower reactor obtains the material 8 based on m-pentadiene and extraction agent, wherein extraction agent is the acetonitrile solution of moisture 5%, extraction tower theoretical plate number 50, material 6 enters from the 44th block of column plate, and extraction agent enters from the 5th block of column plate, and each embodiment extraction tower operational condition is in table 5.
(5) single extraction tower T-103 material 8 out enters one parsing tower T-104 and carries out parsing rectifying, tower top obtains the enriched material 9 based on m-pentadiene, tower reactor obtains the extraction agent 10 based on acetonitrile and water, Analytic Tower tower theoretical plate number 50, material 8 enters from the 35th block of column plate, and each embodiment Analytic Tower operational condition is in table 6.
(6) one parsing tower T-104 material out enters reextraction tower T-105, tower top obtains coarse piperyene 11, tower reactor obtains the material 12 based on extraction agent, wherein extraction agent is the acetonitrile solution of moisture 5%, extraction tower theoretical plate number 80, material 9 enters from the 56th block of column plate, and extraction agent 16 enters from the 8th block of column plate, and each embodiment extraction tower operational condition is in table 7.
(7) reextraction tower T-105 material 11 out enters water wash column T-106, and tower top obtains high purity m-pentadiene 13, and tower reactor obtains the water 14 of purity more than 99%, and each embodiment water wash column operational condition is in table 8.
Finally can obtain the high purity m-pentadiene of more than 98%, each embodiment the results are shown in Table 9, and step (2) takes off
The dicyclopentadiene content that heavy tower T-101 tower reactor obtains is in table 10.
Table 1.
| Component | Content/wt% | Component | Content/wt% |
| Skellysolve A | 0.0850 | Cyclopentadiene | 0.1358 |
| Isoprene | 0.0158 | Cis-1,3-pentadiene | 0.1792 |
| Trans-2-amylene | 0.0174 | Cyclopentenes | 0.1200 |
| Cis-2-amylene | 0.0176 | Pentamethylene | 0.0500 |
| 2-methyl-2-butene | 0.0678 | Benzene | 0.0103 |
| Trans-1,3-pentadiene | 0.3011 | Dicyclopentadiene | 0.0000 |
Table 2.
| Feeding temperature/DEG C | Polymerization temperature/DEG C | Polymerization time/h | |
| Embodiment 1 | 60 | 110 | 3 |
| Embodiment 2 | 70 | 110 | 3 |
| Embodiment 3 | 60 | 120 | 4 |
| Embodiment 4 | 70 | 120 | 4 |
Table 3.
| Tower top temperature/DEG C | Bottom temperature/DEG C | Working pressure/MPa | Reflux ratio | |
| Embodiment 1 | 55 | 100 | 0.1 | 2 |
| Embodiment 2 | 65 | 110 | 0.1 | 3 |
| Embodiment 3 | 55 | 100 | 0.1 | 4 |
| Embodiment 4 | 65 | 110 | 0.1 | 5 |
Table 4.
| Tower top temperature/DEG C | Bottom temperature/DEG C | Working pressure/MPa | Reflux ratio | |
| Embodiment 1 | 75 | 80 | 0.2 | 25 |
| Embodiment 2 | 75 | 90 | 0.3 | 25 |
| Embodiment 3 | 85 | 80 | 0.2 | 35 |
| Embodiment 4 | 85 | 90 | 0.3 | 35 |
Table 5.
Table 6.
| Tower top temperature/DEG C | Bottom temperature/DEG C | Working pressure/MPa | Reflux ratio | |
| Embodiment 1 | 55 | 90 | 0.2 | 5 |
| Embodiment 2 | 55 | 100 | 0.2 | 7 |
| Embodiment 3 | 65 | 90 | 0.3 | 5 |
| Embodiment 4 | 65 | 100 | 0.3 | 7 |
Table 7.
Table 8.
| Water/material (mass ratio) | Tower top temperature/DEG C | Bottom temperature/DEG C | Working pressure/MPa | |
| Embodiment 1 | 1.5 | 25 | 55 | 0.2 |
| Embodiment 2 | 1.5 | 35 | 65 | 0.3 |
| Embodiment 3 | 2.5 | 25 | 55 | 0.2 |
| Embodiment 4 | 2.5 | 35 | 65 | 0.3 |
Table 9.
| Component content/wt% | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Skellysolve A | 8.79E-06 | 5.97E-06 | 4.95E-06 | 3.07E-06 |
| Isoprene | 5.39E-06 | 4.02E-06 | 4.21E-06 | 4.33E-06 |
| Trans-2-amylene | 1.02E-05 | 6.57E-06 | 5.61E-06 | 4.08E-06 |
| Cis-2-amylene | 2.56E-05 | 1.54E-05 | 1.40E-05 | 1.07E-05 |
| 2-methyl-2-butene | 4.07E-04 | 2.35E-04 | 4.46E-04 | 2.12E-04 |
| Trans-1,3-pentadiene | 0.7011 | 0.7017 | 0.7015 | 0.7012 |
| Cyclopentadiene | 0 | 0 | 0 | 0 |
| Cis-1,3-pentadiene | 0.2849 | 0.2854 | 0.2839 | 0.2851 |
| Cyclopentenes | 1.79E-03 | 1.68E-03 | 1.72E-03 | 1.87E-03 |
| Pentamethylene | 3.20E-06 | 2.42E-06 | 2.29E-06 | 1.88E-06 |
Table 10
| Component content/wt% | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Dicyclopentadiene | 0.6669 | 0.6458 | 0.6443 | 0.6213 |
Claims (7)
1. acetonitrile method prepares a method for high purity m-pentadiene, it is characterized in that: with the m-pentadiene enriched material obtained in cracking of ethylene carbon five sepn process for raw material, the method comprises following process:
(1) m-pentadiene enriched material enters hot polymerization still and carries out hot dimerization, and feeding temperature is 20 ~ 80 DEG C, polymerization temperature 60 ~ 140 DEG C, and polymerization time is 1 ~ 15 hour;
(2) hot polymerization still material out enters weight-removing column, tower top obtains the m-pentadiene enriched material of purifying further, tower reactor obtains the dicyclopentadiene that purity is more than or equal to 60%, weight-removing column operational condition: tower top temperature is 30 ~ 90 DEG C, bottom temperature is 85 ~ 150 DEG C, working pressure is 0.1 ~ 1MPa, and reflux ratio is 1 ~ 20;
(3) weight-removing column tower top m-pentadiene enriched material material out enters lightness-removing column, tower top obtains the light constituent mixture based on Skellysolve A and 2-methyl-2-butene, tower reactor obtains m-pentadiene enriched material concentrated further, lightness-removing column operational condition: tower top temperature is 40 ~ 100 DEG C, bottom temperature is 70 ~ 120 DEG C, working pressure is 0.1 ~ 1MPa, and reflux ratio is 10 ~ 60;
(4) m-pentadiene enriched material material out at the bottom of lightness-removing column enters single extraction tower and carries out extracting and separating, the hydrocarbon mixture that it is main component that tower top obtains with cyclopentenes and pentamethylene, the material that it is main component that tower reactor obtains with m-pentadiene and extraction agent, wherein extraction agent is the acetonitrile solution of acetonitrile or moisture 2 ~ 20wt%, extraction agent and material feeding mass ratio are 0.5 ~ 15, extractant feed temperature is 15 ~ 75 DEG C, extraction tower operational condition: tower top temperature is 40 ~ 100 DEG C, bottom temperature is 70 ~ 120 DEG C, working pressure is 0.1 ~ 1MPa, reflux ratio is 1 ~ 30,
(5) material being out main component with m-pentadiene and extraction agent at the bottom of single extraction tower enters one parsing tower and carries out parsing rectifying, tower top obtains the enriched material based on m-pentadiene, tower reactor obtains the extraction agent based on acetonitrile and water, return extraction tower to recycle, Analytic Tower operational condition: tower top temperature is 30 ~ 90 DEG C, bottom temperature is 70 ~ 120 DEG C, and working pressure is 0.1 ~ 1MPa, and reflux ratio is 1 ~ 30;
(6) one parsing tower top out be that the enriched material material of main component enters reextraction tower with m-pentadiene, tower top obtains coarse piperyene, tower reactor obtains the material based on extraction agent, wherein extraction agent is the acetonitrile solution of acetonitrile or moisture 2 ~ 20wt%, extraction agent and material feeding mass ratio are 1 ~ 15, extractant feed temperature is 20 ~ 70 DEG C, extraction tower operational condition: tower top temperature is 40 ~ 90 DEG C, bottom temperature is 70 ~ 110 DEG C, working pressure is 0.1 ~ 1MPa, and reflux ratio is 5 ~ 20;
(7) reextraction column overhead coarse piperyene material enters water wash column, tower top obtains high purity m-pentadiene, tower reactor obtain purity >=99% water, the charge-mass ratio of water and material is 1 ~ 20, water wash column operational condition: tower top temperature is 10 ~ 50 DEG C, bottom temperature is 30 ~ 80 DEG C, and working pressure is 0.1 ~ 1MPa.
2. the method preparing high purity m-pentadiene according to claim 1, is characterized in that: in process (4), (6), and described extraction agent is the acetonitrile solution of moisture 5wt%.
3. the method preparing high purity m-pentadiene according to claim 1, is characterized in that: in process (4), (6), and described extraction agent and material feeding mass ratio are respectively 1 ~ 7,3 ~ 10.
4. the method preparing high purity m-pentadiene according to claim 1, is characterized in that: in process (4), (6), and described extractant feed temperature is respectively 30 ~ 50 DEG C, 50 ~ 70 DEG C.
5. the method preparing high purity m-pentadiene according to claim 1, is characterized in that: in process (4), and described tower top temperature is 50 ~ 80 DEG C, and bottom temperature is 90 ~ 110 DEG C, and working pressure is 0.1 ~ 0.5MPa, and reflux ratio is 5 ~ 20.
6. the method preparing high purity m-pentadiene according to claim 1, is characterized in that: in process (6), and described tower top temperature is 60 ~ 90 DEG C, and bottom temperature is 80 ~ 100 DEG C, and working pressure is 0.1 ~ 0.5MPa, and reflux ratio is 5 ~ 15.
7. the method preparing high purity m-pentadiene according to claim 1, it is characterized in that: in process (7), described water and the charge-mass ratio of material are 1 ~ 5, and tower top temperature is 20 ~ 40 DEG C, bottom temperature is 50 ~ 70 DEG C, and working pressure is 0.1 ~ 0.5MPa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3510405A (en) * | 1967-11-11 | 1970-05-05 | Nippon Zeon Co | Isoprene purification process |
| CN1865201A (en) * | 2005-05-18 | 2006-11-22 | 中国石化上海石油化工股份有限公司 | Method for refining crude piperyene |
| CN101450885A (en) * | 2007-12-07 | 2009-06-10 | 中国石油化工股份有限公司 | Method for separating carbon 5 fraction by one-stage extraction and rectification |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3510405A (en) * | 1967-11-11 | 1970-05-05 | Nippon Zeon Co | Isoprene purification process |
| CN1865201A (en) * | 2005-05-18 | 2006-11-22 | 中国石化上海石油化工股份有限公司 | Method for refining crude piperyene |
| CN101450885A (en) * | 2007-12-07 | 2009-06-10 | 中国石油化工股份有限公司 | Method for separating carbon 5 fraction by one-stage extraction and rectification |
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