CN1037171C - Separation method of C+10 heavy aromatic hydrocarbon - Google Patents
Separation method of C+10 heavy aromatic hydrocarbon Download PDFInfo
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- CN1037171C CN1037171C CN94105030A CN94105030A CN1037171C CN 1037171 C CN1037171 C CN 1037171C CN 94105030 A CN94105030 A CN 94105030A CN 94105030 A CN94105030 A CN 94105030A CN 1037171 C CN1037171 C CN 1037171C
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- rich
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- rectifying
- durene
- durol
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Abstract
The present invention relates to a method for separating C10<+> heavy aromatic hydrocarbons, which comprises: reformed C10<+> heavy aromatic hydrocarbons are used as raw materials; durene and naphthalene are obtained by separation with a rectification and crystallisation method, wherein in the rectification of the C10<+> heavy aromatic hydrocarbons, an operating method for changing a reflux ratio is adopted, namely that the operation of a high reflux ratio is adopted when tetramethylbenzene-enriched fractions are cut, and the operation of a low reflux ratio is adopted when other fractions are cut. Thus, the concentration of durene in the tetramethylbenzene-enriched liquid is increased, and the input concentration of a tetramethylbenzene-enriched crystallizer liquid is increased. Thereby, the yield of durene crystals and the yield of the total technology are increased.
Description
The invention relates to C
10 +The separation method of heavy aromatics, more specifically say so about by rectifying and crystallization from C
10 +High yield is isolated the method for durol in the heavy aromatics.
In the prior art for C
10 +Comprehensive Utilization of Heavy Aromatics, comparatively general method are durol and the naphthalenes that separates wherein, and remaining ingredient is made solvent oil.The technical process of these class methods is shown in Figure 1.Raw material C wherein
10 +Through rectifying, be generally batch fractionating earlier, cut into solvent oil, rich durene liquid, several fraction sections such as rich naphthalene liquid, then, and the rich durene liquid of gained, rich naphthalene liquid is isolated durol and naphthalene respectively through the crystalline method again.
But the method for prior art is all lower because of the durol crystallization yield, and makes the yield of whole technology on the low side, can not be effectively, and with high yield from C
10 +Isolate durol in the heavy aromatics.
Influence the factor of durol crystallization yield, except with the processing parameter of crystallisation process, as Tc, outside crystallization times etc. are relevant, also with the input concentration of crystallizer, durol concentration is relevant in the promptly rich durene liquid, and this input concentration is controlled by the processing parameter of rectifying.In the control of the processing parameter of rectifying, for batch fractionating, after the rectifying tower stage number is increased to a certain degree, increase again stage number then separating effect can not be significantly improved, and must improve reflux ratio.Usually adopt the constant reflux ratio operation in the prior art, and reflux ratio is lower, like this, under the prerequisite that guarantees rectifying durol yield, caused the concentration of durol in rich durene liquid on the low side inevitably, as domestic some producer, the reflux ratio of rectifying tower≤5, the concentration of durol is about about 20M% in the rich durene liquid.Because of the crystallizer input concentration is lower, make the durol crystallization yield be difficult to reach higher level, the result makes total process recovery ratio lower.This shows, still adopt big reflux ratio operation if influenced the process recovery ratio of durol in the prior art because of the rectifying reflux ratio is lower in the whole process of rectifying, though can improve the concentration of durol in the rich durene liquid, but process cost is raise greatly, and do not have practical value.Therefore need in the prior art a kind of can obtain high density durol input concentration and the isolating whole process recovery ratio of durol is improved and don't increase substantially process cost from C
10 +The method of separating durol in the heavy aromatics.
The purpose of this invention is to provide a kind of C
10 +The separation method of heavy aromatics.
Applicant of the present invention for the problem that the method that solves prior art exists has been carried out a large amount of research, and has invented a kind of from C at the method for above-mentioned prior art
10 +The novel method of separating durol in the heavy aromatics is by at C
10 +Adopt the working method of varying reflux ratio to realize improving the concentration of durol in the rich durene liquid and then improved the isolating whole process recovery ratio of durol and don't the goal of the invention of increase process cost in the heavy aromatics rectifying.
Method of the present invention is according to C
10 +The characteristic of heavy aromatics material is according to C
10 +Solvent oil and rich naphthalene liquid can satisfy separation than cutting under the low reflux ratio in the heavy aromatics separation method, the enrichment requirement, and the adjacent component of durol is more, must operation can satisfy these characteristics of enrichment under big reflux ratio, at C
10 +Adopt the varying reflux ratio working method in the heavy aromatics rectifying, promptly when cutting solvent oil and rich naphthalene cut, adopt than low reflux ratio, as 3-5, and when the rich durene liquid of cutting, adopt big reflux ratio, as 12-18, thereby the concentration that has improved durol in the rich durene liquid is the input concentration of crystallizer, and its result has improved the crystallization yield of durol and total process recovery ratio.Method of the present invention is not only applicable to the single tower distillation operation, and can be applicable to the multitower distillation operation, promptly adopts the low reflux ratio operation in the rectifying tower of cutting solvent oil and rich naphthalene liquid, and adopt big reflux ratio operation in the rectifying tower of the rich durene of cutting.
Working method of the present invention is, is the 45-60 piece at number of theoretical plate, and vaporator rate is under the operational condition of 6-8g/min, with raw material C
10 +Heavy aromatics cuts into I through rectifying earlier
#Solvent oil (HK～192 ℃), rich durene liquid (192 ℃～200 ℃), the several fraction sections of rich naphthalene liquid (206 ℃～230 ℃) Residual oils (＞238 ℃), then, make it be separated into durol and solvent oil through the crystalline method rich durene liquid, rich naphthalene liquid, naphthalene and solvent oil.At C
10 +In the heavy aromatics rectifying, adopting number of theoretical plate when cutting rich durene liquid is the 45-60 piece, vaporator rate is 6-8g/min, reflux ratio is a 12-18 process conditions condition, can cut the rich durene liquid that obtains durol content 〉=36% (m/m), and durol recovery per pass 〉=90% (m/m) has improved the input concentration of rich durene liquid crystallizer like this, has also promptly improved the recovery per pass of durol in the crystallization operation sequence.Adopting number of theoretical plate when cutting solvent oil and rich naphthalene liquid fraction is the 45-60 piece, and vaporator rate is 6-8g/min, and reflux ratio is the processing condition operation of 3-5.C
10 +The rectifying of heavy aromatics is to carry out in single tower or a plurality of rectifying tower.
A kind of from C
10 +Isolate the method for durol and naphthalene in the heavy aromatics, this method comprises raw material C
10 +Heavy aromatics cuts into solvent oil through rectifying earlier, rich durene liquid, and rich naphthalene liquid, the several fraction sections of Residual oil, then, with rich durene liquid, rich naphthalene liquid makes it be separated into durol and solvent oil, naphthalene and solvent oil through the crystalline method, it is characterized in that C
10 +The working method that adopts varying reflux ratio in the heavy aromatics rectifying promptly improves the input concentration of rich durene liquid crystallizer to improve the concentration of durol in the rich durene liquid.Wherein at C
10 +In the heavy aromatics rectifying, when cutting solvent oil and rich naphthalene liquid fraction, adopt, and when cutting is the richest in benzene liquid, adopt big reflux ratio operation than the low reflux ratio operation.Wherein at C
10 +In the heavy aromatics rectifying, used reflux ratio is 3～5 in the operation of cutting solvent oil and rich naphthalene fraction, and used reflux ratio is 12-18 in the operation of the rich durene liquid of cutting.C wherein
10 +The rectifying of heavy aromatics is to carry out in single rectifying tower.C wherein
10 +The rectifying of heavy aromatics is to carry out in a plurality of rectifying tower.
Method of the present invention is applied to C
10 +In the heavy aromatics rectifying, durol enrichment concentration can reach more than the 30m%.(theoretical number of plates of rectifying tower is 60), and enrichment concentration improves 10m% approximately.As the crystallization raw material, under same crystallization condition, the crystallization yield of durol can improve 7m% approximately with this pregnant solution.
Embodiment 1
1000gC
10 +Heavy aromatics carries out single tower atmospheric pressure batch fractionating, and theoretical number of plates of rectifying tower is 60, and each temperature range reflux ratio is as follows:
HK～186℃ R＝2
186-187.5 R＝3
187.5～189 R＝8
189～202 R＝15
202～206 R＝6
206～238 R＝3
The rectifying result obtains rich durene liquid (192～200 ℃) 136.5g, and wherein the concentration of durol is 35m%, and the rectifying rate of recovery of durol is 94.5m%; Rich naphthalene liquid (206～230 ℃) 102.6g, wherein naphthalene concentration is 48.6m%, the rectifying rate of recovery of naphthalene is 97.7%; Solvent oil 578.2g, Residual oil 167.2g.
Embodiment 21230gC
10 +Heavy aromatics carries out the cutting of three towers, and condition is as follows:
| Tower number | Stage number | Cutting temperature | Reflux ratio |
| I # | 45 | 174～189 | 3 |
| II # | 60 | 189～202 | 12 |
| III # | 45 | 202～230 | 4 |
It is 30.3m% that the rectifying result obtains the middle durol concentration of rich durene liquid (192～200 ℃), and the durol rectifying rate of recovery is 95.3m%; The concentration of naphthalene is 44.3m% in the rich naphthalene liquid (206～230 ℃), and the rectifying rate of recovery of naphthalene is 97.2m%.
Claims (3)
1, a kind of method of from C+10 heavy aromatic hydrocarbon, isolating durol and naphthalene, this method comprises the material carbon+10 heavy aromatic hydrocarbon is earlier cut into solvent oil through rectifying, rich durene liquid, rich naphthalene liquid, the several fraction sections of Residual oil, then, with rich durene liquid, rich naphthalene liquid makes it be separated into durol and solvent oil through the crystalline method, naphthalene and solvent oil, it is characterized in that, adopt the working method of varying reflux ratio to improve the concentration of durol in the rich durene liquid in the C+10 heavy aromatic hydrocarbon rectifying, promptly improve the input concentration of rich durene liquid crystallizer, in C+10 heavy aromatic hydrocarbon rectifying, used reflux ratio is 3-5 in the operation of cutting solvent oil and rich naphthalene fraction, and used reflux ratio is 12-18 in the operation of the rich durene liquid of cutting.
2, according to the method for claim 1, the rectifying that it is characterized in that C+10 heavy aromatic hydrocarbon is to carry out in single rectifying tower.
3, according to the method for claim 1, the rectifying that it is characterized in that C+10 heavy aromatic hydrocarbon is to carry out in a plurality of rectifying tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94105030A CN1037171C (en) | 1994-05-12 | 1994-05-12 | Separation method of C+10 heavy aromatic hydrocarbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94105030A CN1037171C (en) | 1994-05-12 | 1994-05-12 | Separation method of C+10 heavy aromatic hydrocarbon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1120035A CN1120035A (en) | 1996-04-10 |
| CN1037171C true CN1037171C (en) | 1998-01-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94105030A Expired - Fee Related CN1037171C (en) | 1994-05-12 | 1994-05-12 | Separation method of C+10 heavy aromatic hydrocarbon |
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| Country | Link |
|---|---|
| CN (1) | CN1037171C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318874B (en) * | 2008-06-18 | 2010-11-10 | 常熟市联邦化工有限公司 | Process for joint production of aromatic solvent, stone oil naphthalin and durene line products with C10 heavy aromatic raw material |
| CN103102239A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Method for continuous extraction of durene from C10 heavy aromatics |
| CN104610005A (en) * | 2015-01-31 | 2015-05-13 | 江苏华伦化工有限公司 | Production process of industrial high-quality naphthalene |
| CN107815164A (en) * | 2017-09-30 | 2018-03-20 | 江苏华伦化工有限公司 | Boiling range is the preparation method of 175~205 DEG C of the low naphthalene aromatic solvent of C+10 heavy aromatic hydrocarbon |
| WO2020051886A1 (en) * | 2018-09-14 | 2020-03-19 | 江苏华伦化工有限公司 | Preparation method for carbon 10 heavy aromatic low naphthalene aromatic solvent having distillation range of 175-205°c |
| CN111377793A (en) * | 2020-04-09 | 2020-07-07 | 北方华锦化学工业股份有限公司 | Method for decoloring solvent oil and extracting durene |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3031513A (en) * | 1958-12-03 | 1962-04-24 | Exxon Research Engineering Co | Process for obtaining durene |
| CN1062522A (en) * | 1990-12-22 | 1992-07-08 | 天津石油化工公司研究所 | From carbon 10 heavy aromaticss, extract durol |
-
1994
- 1994-05-12 CN CN94105030A patent/CN1037171C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3031513A (en) * | 1958-12-03 | 1962-04-24 | Exxon Research Engineering Co | Process for obtaining durene |
| CN1062522A (en) * | 1990-12-22 | 1992-07-08 | 天津石油化工公司研究所 | From carbon 10 heavy aromaticss, extract durol |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1120035A (en) | 1996-04-10 |
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