CN104276915A - Separation method for C9-C10 fractions - Google Patents
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- CN104276915A CN104276915A CN201310294366.XA CN201310294366A CN104276915A CN 104276915 A CN104276915 A CN 104276915A CN 201310294366 A CN201310294366 A CN 201310294366A CN 104276915 A CN104276915 A CN 104276915A
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Abstract
The invention relates to a separation method for C9-C10 fractions. The separation method for the C9-C10 fractions comprises the following steps: carrying out vacuum distillation separation on raw materials in a vacuum distillation tower for obtaining rich phenylethylene and alpha methyl styrene fractions at the tower top and obtaining residual fractions at the tower bottom; enabling tower bottom materials to enter a depolymerization and distillation tower and carrying out depolymerization and distillation for obtaining rich cyclopentadiene fraction at the tower top, methyl cyclopentadiene material at a lateral line and mixed fraction of indene and residual dicyclopentadiene at the tower bottom; enabling tower bottom fraction to enter the vacuum distillation tower and carrying out vacuum distillation for obtaining mixed fraction rich in indene and dicyclopentadiene at the tower top and heavy component impurities at the tower bottom; and enabling fraction rich in indene and dicyclopentadiene to enter the depolymerization and distillation tower and carrying out depolymerization and distillation for obtaining cyclopentadiene fraction at the tower top and fraction rich in indene at the tower bottom. The separation method for the C9-C10 fractions has the advantages that high-purity cyclopentadiene and methyl cyclopentadiene are obtained while a high-quality petroleum resin raw material is obtained; dimerization reaction is greatly reduced in a distillation separation process, so that generation of polymers is avoided, the yield of one-way products is high, and the problem that dicyclopentadiene and indene are difficult to separate is also solved.
Description
Technical field
The invention belongs to petrochemical industry, particularly a kind of extraction and application method by petroleum cracking Crude products.deep process C9 ~ C10 cut, obtains the raw material of high-quality petroleum resin by the method such as depolymerization, separation by C9 ~ C10 cut.
Background technology
C9 ~ C10 cut is that petroleum naphtha or Pyrolysis Reaction of Gas Oil by product go out the residue cut after C 5 fraction, C6 ~ C8 cut through extraction and isolation, accounts for 10% ~ 20% of ethylene yield.C9 ~ C10 fractions consisting is complicated, about there is this cut of 150 various ingredients, mainly contain the components such as more than C9 aromatic hydrocarbons, vinylbenzene, vinyl toluene, dicyclopentadiene (DCPD), indenes, naphthalene class and cyclopentadiene (CPD), methyl cyclopentadiene (MCPD) various forms autohemagglutination, gather dimer mutually, wherein the highest with the content of vinyl toluene and dicyclopentadiene again.The content preparing dicyclopentadiene in petroleum resin raw material is high, then resin productive rate is high, darkens, and molecular weight reduces.In C9 ~ C10 cut, dicyclopentadiene amount is more, is the principal element affecting resin form and aspect.Increase cinnamic content and can improve color and luster, improve productive rate, but the softening temperature of resin and the intermiscibility with other resins can be reduced.The content of vinyl toluene can not affect yield, but too high levels can damage form and aspect.Softening temperature is general more high better, and the content increasing indenes can improve the softening temperature of resin, but content easy coking more than 20%.The diversity of this component and complicacy make the polymerization of C9 be different from general single component polymerization, and the molecular weight of polymerisate is not in normal distribution, and C9 heavy component is more simultaneously, and intrinsic colour is comparatively dark, so gained resin must be low-grade resin.Therefore, industrial C9 ~ C10 cut that started carries out thick rectifying in certain temperature range, raw material is cut into styrenic, dicyclopentadiene class and indenes class 3 fraction section, then is polymerized, obtain the resin of stable performance.
Patent 200610130712.0 discloses a kind of method of C9 prepared using, the rectifying of C9 raw material is cut into styrenic petroleum resin, dicyclopentadiene resinoid oil and indenes class petroleum resin three fraction section by the method, by these three fraction section according to product requirement, add heat polymerization still.Heat polymerization still is four still series connection, and material continues through four reactors successively.By the material after four still series connection hot polymerizations, distill the solvent removed wherein, namely obtain petroleum resin products.Patent 200610144206.7 discloses a kind of C
9 +the method that fraction seperation utilizes, the method is by C
9 +cut rectification under vacuum is divided into rich in styrene cut and tower bottom distillate; Atmospheric distillation is carried out, by isolating cyclopentadiene cut, methyl cyclopentadiene cut at the bottom of atmospheric distillation tower top to tower successively, being rich in the higher cut of dicyclopentadiene cut, indenes content and heavy ends after more described tower bottom distillate being heated to 180 ~ 380 DEG C.In the method, when still temperature is heated to more than 180 DEG C easily there is depolymerization in dicyclopentadiene, if C when temperature reaches 260 DEG C
9 +can there is thermopolymerization in the polymer monomer in cut, thus add the generation of other dipolymers and polymer in material, not only have impact on the separation of material but also add the loss of material.。
US 6,258,989 B1 disclose a kind of method of pyrolysis gasoline comprehensive treating process, pyrolysis gasoline heating makes cyclopentadiene wherein be dicyclopentadiene by the method, then adopt the method for rectifying that this material is cut into C5 ~ C9 and C10+ fraction section, C5 ~ C9 cut obtains the products such as benzene, toluene and dimethylbenzene through Hydrogenation, and C10+ cut goes out dicyclopentadiene and oil fuel by rectifying separation.US 4,522,688 discloses a kind of method producing CPD and MCPD only by depolymerization C9 ~ C10 fraction seperation.
It can thus be appreciated that, be only be separated by depolymerization to produce CPD and MCPD to the utilization of C9 ~ C10 cut in prior art, or only using C9 raw material rectifying cutting as the raw material of petroleum resin, C9 raw material is not utilized fully; And in the process of rectification under vacuum C9 raw material, because DCPD concentration is higher, ratio shared by vinylbenzene, vinyl toluene and indenes is relatively low, the boiling point of DCPD and vinyl toluene and indenes is more or less the same, more close under a reduced pressure, the cut wanting to obtain high level then needs larger reflux ratio, also loses more vinyl toluene simultaneously.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of separation method by petroleum cracking Crude products.deep process C9 ~ C10 cut, and the present invention, in minimizing rectifying cutting difficulty, while obtaining high-quality petroleum resin raw material, improves the comprehensive utilization ratio of C9 ~ C10 cut.
The separation method of a kind of C9 ~ C10 cut of the present invention, comprising:
(1) C10 raw material is through vacuum rectification tower, and tower top obtains rich in styrene, vinyl toluene cut, and kettle material enters next processing unit.Bottom temperature is 80 ~ 120 DEG C, and tower top temperature is 50 ~ 67 DEG C, and reflux ratio is 3 ~ 10, and tower top pressure is-80 ~-90KPaG.
(2) kettle material that step (1) obtains enters depolymerization rectifying tower and is separated, and tower top obtains CPD cut, and side line obtains MCPD cut, and kettle material enters next processing unit.De-polymerization temperature is 160 ~ 220 DEG C, and tower top temperature is 37 ~ 50 DEG C, and side stream temperature is 65 ~ 80 DEG C, and reflux ratio is 1 ~ 5, and tower top pressure is 0 ~ 10KPaG.
(3) kettle material that step (2) obtains enters vacuum rectification tower and is separated, and tower top obtains the cut being rich in dicyclopentadiene and indenes, and tower reactor obtains heavy constituent.Bottom temperature is 105 ~ 160 DEG C, and tower top temperature is 56 ~ 78 DEG C, and reflux ratio is 1 ~ 7, and tower top pressure is-80 ~-90KPaG.
(4) the tower top material that step (3) obtains carries out depolymerization rectifying, and tower top obtains being rich in cyclopentadiene cut, and tower reactor is indenes.De-polymerization temperature is 160 ~ 210 DEG C, and tower top temperature is 35 ~ 49 DEG C, and reflux ratio is 1 ~ 5, and tower top pressure is 0 ~ 10KPaG.
Above-mentioned steps (1) described bottom temperature is preferably 90 ~ 105 DEG C, and tower top temperature is preferably 54 ~ 59 DEG C, and reflux ratio is preferably 5 ~ 8, and tower top pressure is preferably-82 ~-88KPaG..
Above-mentioned steps (2) described de-polymerization temperature is preferably 180 ~ 210 DEG C, and tower top temperature is preferably 41 ~ 44 DEG C, and side stream temperature is preferably 68 ~ 72 DEG C, and reflux ratio is preferably 2 ~ 4, and tower top pressure is preferably 2 ~ 8KPaG.
Above-mentioned steps (3) described bottom temperature is preferably 105 ~ 135 DEG C, and tower top temperature is preferably 60 ~ 70 DEG C, and reflux ratio is preferably 2 ~ 5, and tower top pressure is preferably-82 ~-88KPaG.
Above-mentioned steps (4) described de-polymerization temperature is 170 ~ 190 DEG C, and tower top temperature is 41 ~ 44 DEG C, and reflux ratio is 1 ~ 3, and tower top pressure is 2 ~ 8KPaG.
Beneficial effect
Compared with prior art, the invention has the advantages that and obtain highly purified cyclopentadiene and methyl cyclopentadiene while obtaining high-quality petroleum resin raw material; Rectifying separation process dimerization reaction greatly reduces, and whole flow process can think substantially there is not recycle stock, avoids the generation of polymer, makes one way product yield higher; Meanwhile, the improvement of flow process also solves the contradiction of dicyclopentadiene and indenes separation difficulty.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention, first its Raw C9 ~ C10 cut W1 enters the first vacuum rectification tower 1(theoretical plate number 25) rectification under vacuum, tower top obtains vinylbenzene, vinyl toluene cut W2, tower reactor cut W3 enters the first depolymerization rectifying tower 2(theoretical plate number 20) carry out depolymerization rectifying, tower top obtains dicyclopentadiene cut W4, side line obtains methyl cyclopentadiene cut W5, tower reactor cut W6 enters the second vacuum rectification tower 3(theoretical plate number 25) carry out rectification under vacuum, tower top obtains indenes and dicyclopentadiene mixed fraction W7, tower reactor periodic exhaustion heavy constituent material W8.W7 enters the second depolymerization rectifying tower 4(theoretical plate number 15) carry out depolymerization rectifying, tower top obtains cyclopentadiene cut W9, and tower reactor obtains indenes cut W10.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
In the present embodiment, the yield of cyclopentadiene yield, methyl cyclopentadiene yield, vinylbenzene, vinyl toluene yield and indenes is defined as respectively:
Wherein:
Flow × dicyclopentadiene the molecular fraction of unit time dicyclopentadiene mole of feed amount=W1;
Unit time cyclopentadiene mole load=(flow × W9 cyclopentadiene molecular fraction of the flow × W4 cyclopentadiene molecular fraction+W9 of W4);
Flow × bis-methyl cyclopentadiene molecular fraction of unit time two methyl cyclopentadiene mole of feed amount=W1;
Flow × methyl cyclopentadiene the molecular fraction of unit time methyl cyclopentadiene mole load=W5;
Unit time vinylbenzene, the flow × W1 vinylbenzene of vinyl toluene mole of feed amount=W1, vinyl toluene molecular fraction;
Flow × W25 vinylbenzene, the vinyl toluene molecular fraction of unit time vinylbenzene, vinyl toluene mole load=W2;
Flow × W1 indenes the molecular fraction of unit time indenes molar product inlet amount=W1;
Flow × W10 indenes the molecular fraction of unit time indenes molar product load=W10.
[embodiment 1 ~ 10]
(1) C9 ~ C10 cut is carried out underpressure distillation by the first vacuum rectification tower 1, tower top obtains vinylbenzene, vinyl toluene cut, and tower reactor must remain cut; Wherein bottom temperature is 80 ~ 120 DEG C, and tower top temperature is 50 ~ 67 DEG C, and reflux ratio is 3 ~ 10, and tower top pressure is-80 ~-90KPaG.;
(2) the tower reactor cut of step (1) gained is entered the first depolymerization rectifying tower 2 depolymerization rectifying, tower top obtains cyclopentadiene cut, and side line obtains methyl cyclopentadiene, and tower reactor must remain cut; Wherein, bottom temperature is 160 ~ 220 DEG C, and tower top temperature is 37 ~ 50 DEG C, and side stream temperature is 65 ~ 80 DEG C, and reflux ratio is 1 ~ 5, and tower top pressure is 0 ~ 10KPaG;
(3) the tower reactor cut of step (2) gained is entered the second vacuum rectification tower 3 and carry out underpressure distillation, tower top obtains dicyclopentadiene and indenes mixed fraction, and tower reactor obtains heavy constituent; Wherein, bottom temperature is 105 ~ 160 DEG C, and tower top temperature is 56 ~ 78 DEG C, and reflux ratio is 1 ~ 7, and tower top pressure is-80 ~-90KPaG;
(4) overhead fraction of step (3) is passed through the second depolymerization rectifying tower 4 depolymerization rectifying, tower top obtains cyclopentadiene cut, obtains indenes cut at the bottom of tower; Wherein, depolymerization reaction temperature is 160 ~ 210 DEG C, and tower top temperature is 35 ~ 49 DEG C, and reflux ratio is 1 ~ 5, and tower top pressure is 0 ~ 10KPaG.
Accompanying drawing 1 is shown in the technical process of embodiment 1 ~ 10, and raw material is C9 ~ C10 cut of petroleum cracking ethylene by-product, mainly forms in table 1.
The process conditions of each embodiment first vacuum rectification tower 1, first depolymerization rectifying tower 2, second vacuum rectification tower 3 and the second depolymerization rectifying tower 4 is respectively in table 2,3,4 and 5.Adopt vapor-phase chromatography to analyze the composition of material W2, W4, W5, W9 and W10 respectively, in each material, the content of enriched composition is in table 6.Again in conjunction with the yield of the flow rate calculation product of each material, the results are shown in Table 7.
Table 1
Table 2
Table 3
Table 4
Table 5
Table 6
Table 7
Although preferred embodiment discloses as above by the present invention; so itself and be not used to limit content of the present invention; anyly be familiar with this those skilled in the art; not departing from main spirits of the present invention and context; when doing various change and retouching, the protection domain therefore invented should be as the criterion with the basic right claimed range applied for a patent.
Claims (9)
1. a separation method for C9 ~ C10 cut, is characterized in that, the method comprises the steps:
(1) C9 ~ C10 cut is carried out underpressure distillation by the first vacuum rectification tower (1), tower top obtains vinylbenzene, vinyl toluene cut, and tower reactor must remain cut; Wherein, bottom temperature is 80 ~ 120 DEG C, and tower top temperature is 50 ~ 67 DEG C, and reflux ratio is 3 ~ 10, and tower top pressure is-80 ~-90KPaG;
(2) the tower reactor cut of step (1) gained is entered the first depolymerization rectifying tower (2) depolymerization rectifying, tower top obtains cyclopentadiene cut, and side line obtains methyl cyclopentadiene, and tower reactor must remain cut; Wherein, bottom temperature is 160 ~ 220 DEG C, and tower top temperature is 37 ~ 50 DEG C, and tower top pressure is 0 ~ 10KPaG, and side stream temperature is 65 ~ 80 DEG C, and reflux ratio is 1 ~ 5;
(3) the tower reactor cut of step (2) gained is entered the second vacuum rectification tower (3) and carry out underpressure distillation, tower top obtains dicyclopentadiene and indenes mixed fraction, and tower reactor obtains heavy constituent; Wherein, bottom temperature is 105 ~ 160 DEG C, and tower top temperature is 56 ~ 78 DEG C, and tower top pressure is-80 ~-90KPaG, and reflux ratio is 1 ~ 7;
(4) overhead fraction of step (3) is passed through the second depolymerization rectifying tower (4) depolymerization rectifying, tower top obtains cyclopentadiene cut, obtains indenes cut at the bottom of tower; Wherein, depolymerization reaction temperature is 160 ~ 210 DEG C, and tower top temperature is 35 ~ 49 DEG C, and tower top pressure is 0 ~ 10KPaG, and reflux ratio is 1 ~ 5.
2. the separation method of C9 ~ C10 cut according to claim 1, is characterized in that: the bottom temperature in described step (1) is 90 ~ 105 DEG C, and tower top temperature is 54 ~ 59 DEG C, and tower top pressure is-82 ~-88KPaG.
3. the separation method of C9 ~ C10 cut according to claim 1, is characterized in that: the reflux ratio in described step (1) is 5 ~ 8.
4. the separation method of C9 ~ C10 cut according to claim 1, is characterized in that: the bottom temperature in described step (2) is 180 ~ 210 DEG C, and tower top temperature is 41 ~ 44 DEG C, and tower top pressure is 2 ~ 8KPaG, and side stream temperature is 68 ~ 72 DEG C.
5. the separation method of C9 ~ C10 cut according to claim 1, is characterized in that: the reflux ratio in described step (2) is 2 ~ 4.
6. the separation method of C9 ~ C10 cut according to claim 1, is characterized in that: the bottom temperature in described step (3) is 105 ~ 135 DEG C, and tower top temperature is 60 ~ 70 DEG C, and tower top pressure is-82 ~-88KPaG.
7. the separation method of C9 ~ C10 cut according to claim 1, is characterized in that: the reflux ratio in described step (3) is 2 ~ 5.
8. the separation method of C9 ~ C10 cut according to claim 1, is characterized in that: the depolymerization reaction temperature in described step (4) is 170 ~ 190 DEG C, and tower top temperature is 41 ~ 44 DEG C, and tower top pressure is 2 ~ 8KPaG.
9. the separation method of C9 ~ C10 cut according to claim 1, is characterized in that: the reflux ratio in described step (4) is 1 ~ 3.
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CN108865259A (en) * | 2018-06-09 | 2018-11-23 | 濮阳市联众兴业化工有限公司 | A method of the cracking decoloration of carbon nine is deodorized |
CN111548246A (en) * | 2020-04-23 | 2020-08-18 | 广东新华粤石化集团股份公司 | Method for preparing high-purity dicyclopentadiene from cracking carbon nine fraction |
CN114426445A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Comprehensive utilization method of carbon nine-carbon ten-fraction as byproduct in ethylene preparation through petroleum cracking |
CN115124403A (en) * | 2022-09-01 | 2022-09-30 | 淄博鲁华泓锦新材料集团股份有限公司 | Method for separating cracked carbon nine by single-tower rectification in petroleum resin system |
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CN115124403A (en) * | 2022-09-01 | 2022-09-30 | 淄博鲁华泓锦新材料集团股份有限公司 | Method for separating cracked carbon nine by single-tower rectification in petroleum resin system |
CN115124403B (en) * | 2022-09-01 | 2022-12-06 | 淄博鲁华泓锦新材料集团股份有限公司 | Method for separating cracked carbon nine by single-tower rectification in petroleum resin system |
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