CN1027544C - Technology for extracting naphthalene fraction, methyl naphthalene fraction and industrial acenaphthene from coal-tar washing oil - Google Patents

Technology for extracting naphthalene fraction, methyl naphthalene fraction and industrial acenaphthene from coal-tar washing oil Download PDF

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Publication number
CN1027544C
CN1027544C CN 92111855 CN92111855A CN1027544C CN 1027544 C CN1027544 C CN 1027544C CN 92111855 CN92111855 CN 92111855 CN 92111855 A CN92111855 A CN 92111855A CN 1027544 C CN1027544 C CN 1027544C
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China
Prior art keywords
tower
acenaphthene
technology
naphthalene
washing oil
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Expired - Fee Related
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CN 92111855
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CN1078991A (en
Inventor
马中全
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Anshan Iron & Steel Co Design And Research Institute
Angang Steel Co Ltd
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Anshan Iron & Steel Co Design And Research Institute
Angang Steel Co Ltd
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Priority to CN 92111855 priority Critical patent/CN1027544C/en
Publication of CN1078991A publication Critical patent/CN1078991A/en
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Abstract

The present invention relates to a technological method for extracting naphthalene fractions, methyl naphthalene fractions and industrial acenaphthene from wash oil of coal tar. The raw material wash oil is fed into a front tower for distillation, and the naphthalene fractions whose naphthalene content is higher than 60% are produced from the top of the front tower, and the methyl naphthalene fractions whose naphthalene content is lower than 10% and methyl naphthalene content is lower than 70% are produced from the side of the front tower. The waste oil at the bottom of the front tower is fed into a rear tower; after distillation, medium wash oil which can be used as a benzene absorbent is produced from the top of the rear tower, and acenaphthene fractions of at the side are crystallized and filtered to obtain industrial acenaphthene whose acenaphthene content is higher than 95%. The filter liquor returns to the rear tower for being steamed again. The technology has the advantages of energy saving, simple equipment and technology and capability of enhancing product yield and quality.

Description

Technology for extracting naphthalene fraction, methyl naphthalene fraction and industrial acenaphthene from coal-tar washing oil
The invention belongs to a kind of processing method of from coal tar wash oil, extracting naphthalene cut, methylnaphthalene and industrial acenaphthylene.
At present, the domestic production equipment that extracts industrial acenaphthylene from washing oil is climbed factories such as steel coke-oven plant." fuel and chemical industry " the 2nd phase in 1989 recklessly winter hair tonic table " utilizing the NAPTHALENE FLAKES. (INDUSTRIAL GRADE device from washing oil, to extract an industrial acenaphthylene " literary composition.This factory is raw material with the washing oil, preceding column overhead extraction lightweight washing oil.Residual oil is as back tower raw material at the bottom of the preceding Tata, and back Tata bottom product is a heavy wash oil.Back column overhead extraction acenaphthene cut.The acenaphthene cut obtains the solid product industrial acenaphthylene after crystallization, filtration.Filtrate turns back in the preceding tower stock oil.Heat energy institute in Anshan turned round and look at and extensively meaningfully waited the people to deliver " separating the research of methylnaphthalene, biphenyl, indoles from washing oil " report " fuel and chemical industry " 1988 the 4th phases.This article has been introduced the lightweight washing oil that utilizes after the heavy constituent such as taking off acenaphthene from washing oil and has been made raw material, has carried out therefrom separating the test of products such as methylnaphthalene.With the lightweight washing oil is the raw material production methylnaphthalene, needs on the basis of the industrial acenaphthylene production equipment of climbing steel, builds the water distilling apparatus that a cover is produced methylnaphthalene again.
Utilize the less like this chemical industry equipment of industrial acenaphthylene production equipment that only is equivalent to climb steel, from washing oil, extract the naphthalene cut, the washing oil processing unit (plant) that the Anshan iron and steel plant chemical general factory is arranged that three kinds of main productss such as methylnaphthalene and industrial acenaphthylene are produced.Its process flow diagram is seen accompanying drawing 1.This technology is: the preceding tower raw material 2 based on raw material washing oil 1 is sent into anterior distillation tower 3.After adding thermal distillation, product is a heavy wash oil 4 at the bottom of the preceding Tata, tower side line extraction acenaphthene cut 5.Acenaphthene cut 5 obtains solid-state major product industrial acenaphthylene 7 through crystallization, filtration unit 6.Filtrate 8 turns back in the preceding tower raw material 2.The lightweight washing oil 9 of preceding column overhead extraction is as the stock oil of rear portion distillation tower 10.The tower bottoms 11 of back tower 10 turns back in the preceding tower raw material 2.Matter washing oil 12 in the following side line extraction.Last side line extraction major product methylnaphthalene 13.Overhead product is a major product naphthalene cut 14.
Three kinds of technologies of washing oil processing have more than been introduced.In brief, climb steel and only from washing oil, extract a kind of product industrial acenaphthylene.The test of heat energy institute is that the lightweight washing oil that takes off with washing oil after the heavy constituent such as acenaphthene is a raw material, therefrom extracts components such as methylnaphthalene, biphenyl and indoles.The Anshan iron and steel plant chemical general factory extracts three kinds of main productss such as naphthalene cut, methylnaphthalene and industrial acenaphthylene from washing oil.
Day disclosure special permission communique on April 11st, 1985 and on June 7th, 1986 priority the patent application of three minutes " tar processing method " is disclosed.Its publication number is respectively clear 60-63279, clear 60-63280, clear 61-120894.These three patents are mainly narrated the treatment process that reclaims naphthalene with high-recovery from tar.Its main technique is to distill out washing oil a and naphthalene cut from coal tar.The naphthalene cut distills out NAPTHALENE FLAKES. (INDUSTRIAL GRADE and washing oil b after dephenolize.Behind washing oil a that obtains and the washing oil b modified technique through dealkylation or day lighting, redistillation goes out naphthalene cut and washing oil c etc.This naphthalene cut continues fractionation by distillation and goes out NAPTHALENE FLAKES. (INDUSTRIAL GRADE and washing oil b.Washing oil b carries out recirculation processing.This invention has added some component that makes in the washing oil and has been converted into the production process of naphthalene through hydrogenation reaction, thereby increased the rate of recovery of naphthalene in the tar in original technology of tar extraction naphthalene.This shows that this invention and the present invention do not have greatly gets in touch.
The object of the present invention is to provide a kind of technology of from coal tar wash oil, producing products such as naphthalene cut, methylnaphthalene and industrial acenaphthylene simultaneously.It is low that this technology has energy consumption, and production operation is simple, characteristics such as reliable product quality, cost are low.
Production technique outline flowchart of the present invention as shown in Figure 2.
The present invention adopts double tower distil process.Raw material washing oil 15 is sent into anterior distillation tower 16 and is distilled.Preceding top of tower extraction contains the major product naphthalene cut 17 of naphthalene amount 〉=60%.The extraction of tower side line contains naphthalene≤10%, contains the major product methylnaphthalene 18 of first naphthalene 〉=70%.Before tower Residual oil 19 send into this tower as one of raw material of rear portion distillation tower 20.Back column overhead product is middle matter washing oil 21.This product can be used as the coke-oven plant reclaims benzene from coal gas absorption agent.Tower side line extraction acenaphthene cut 22.This cut is produced the major product industrial acenaphthylene 24 that contains acenaphthene 〉=95% through crystallization filtration unit 23.Filtrate 25 is returned back tower 20 and is handled.Output heavy wash oil 26 at the bottom of the tower.
The former technology key distinction that technology of the present invention and Anshan iron and steel plant chemical general factory are produced naphthalene cut, methylnaphthalene and industrial acenaphthylene with washing oil has following 2 points:
1. the sequencing that cuts naphthalene cut, methylnaphthalene and industrial acenaphthylene is different.Former technology is to cut heavy constituent in the wash oil process earlier, after cut light constituent, promptly before the high boiling acenaphthene cut of tower extraction, back tower is produced lower boiling naphthalene cut, methylnaphthalene.Technology of the present invention is to cut light constituent earlier, after cut heavy constituent, promptly before tower elder generation's lower boiling naphthalene cut of extraction and methylnaphthalene, back tower cuts high boiling acenaphthene cut again.
The acenaphthene cut of technology of the present invention through crystallization, filtrate filtered directly as after tower raw material and before no longer turning back in the tower stock oil.
Technology of the present invention has the following advantages and positively effect:
1. adopt the comparable former technology of its energy consumption of this technology to descend more than 20%.Its major cause has:
A. this technology has improved the acenaphthene content of back tower charging, concentrates in the washing oil acenaphthene component this subtracts the energy consumption of entropy process thereby reduced distillation method.The acenaphthene cut will return by former technology through crystallization, filtrate filtered and be fitted in the raw material washing oil.This filtrate then no longer turns back in the preceding tower stock oil by technology of the present invention, and directly as back tower raw material.In addition, the preceding tower Residual oil as back tower raw material has reduced naphthalene cut and methylnaphthalene again than the raw material washing oil.Therefore, technology of the present invention is low to the dilute strength of active principle acenaphthene in the filtrate.Dilution reduction means lacking of entropy increase, thereby makes this energy consumption that subtracts the entropy process of extraction industrial acenaphthylene also few.
B. reduce the ratio of cat head extraction cut, reduced latent heat of vaporization energy consumption.The naphthalene cut has been vaporized once as the part of preceding overhead product lightweight washing oil in the former technology, and tower has been vaporized once as overhead product again in the back, is secondary vaporizing.In technology of the present invention, the naphthalene cut has only been vaporized once as the overhead product of preceding tower, and promptly the more former technology of naphthalene cut has reduced once vaporization in this technology.Methylnaphthalene has passed through once vaporization as the part in the preceding column overhead product lightweight washing oil in this exogenesis technology.In technology of the present invention, only with the liquid form extraction, promptly the more former technology of methylnaphthalene has also reduced once vaporization to methylnaphthalene in this technology as preceding tower sideline product.
C. technology of the present invention has been cancelled back these intermediates of tower Residual oil of former technology, and also more former technology has reduced the energy consumption of producing these intermediates.
D. technology of the present invention can directly be sent into the back tower as back tower raw material with preceding tower Residual oil.So sensible heat of tower Residual oil before can making full use of.
2. but simplified apparatus and operation:
A. tower has two places discharging side line after the former technology, and each tower of this technology all has only place discharging side line.
B. cancelled back these intermediates of tower Residual oil that tower weight steams before will turning back in the former technology, and production unit such as this oil product storage tank of corresponding cancellation.
3. can reduce initial cost to newly-built production equipment, can utilize less water distilling apparatus to replace the production equipment of former technology.
4. adopt this technology only to need pipeline configuration work is suitably adjusted to the old factory that adopts former technology through transforming, existing equipment all can utilize and need not to increase new installation.Use the surplus capacity of existing equipment after this technology instead and can be used to enlarge the treatment capacity of raw material washing oil, also can be used for improving the quality of products or product recovery rate.
It below is implementation of processes example of the present invention.
Utilize my company of technology of the present invention to carry out half type approval test in 1991.This device through the bimester surplus operation, it is as follows to draw relevant testing data:
Two kinds of raw material washing oil composition such as tables 1 that technology adopted.
Table 1
Component concentration (%)
Naphthalene 12.39
Intermediate component 5.14
Methylnaphthalene 33.08
Intermediate component 18.34
Acenaphthene 12.34
Heavy constituent 18.71
Add up to 100.00
Novel process and former technological test are that yield, quality index and the energy consumption of 100 product sees Table 2 to handle washing oil.
Table 2
Former technology technology of the present invention
Productive rate content (%) productive rate content (%)
Naphthalene cut 14.9 contains naphthalene 63.4 14.8 and contains naphthalene 63.7
Methylnaphthalene contains naphthalene 9.9 and contains naphthalene 9.8
28.6 28.8
Cut contains methylnaphthalene 75.2 and contains methylnaphthalene 75.3
Industrial acenaphthylene 8.4 contains acenaphthene 95.4 8.4 and contains acenaphthene 95.6
Thermal losses (GJ) 2.27 1.75
Table 2 data declaration, technology of the present invention and former processes washing oil of the same race, under the quality index and the essentially identical condition of productive rate of product, washing oil by this processes equivalent, the per-cent that its energy consumption accounts for former technology is: (1.75/2.27) * 100% ≈ 77.1%, the more former process energy consumption 1-77.1%=22.9% that descended.To handling the processing unit (plant) of 6000t washing oil year, under the identical situation of energy consumption, if adopt technology of the present invention, a year Treatment of Washing oil mass is 6000 * 100/77.1 ≈ 7780(t), but i.e. multiprocessing in every year washing oil 1780t.

Claims (1)

1, a kind of processing method of from coal tar wash oil, extracting naphthalene cut, methylnaphthalene and industrial acenaphthylene, it is characterized in that raw material washing oil 15 enters preceding tower 16, by preceding tower 16 cat head extraction major product naphthalene cuts 17, preceding tower 16 side line extraction major product methylnaphthalenes 18, the tower bottoms 19 of preceding tower 16 is as the raw material of back towers 20, matter washing oil 21 in the cat head extraction of back tower 20, back tower 20 side line extraction acenaphthene cuts 22, after crystallization, filtration unit 23 filter, filter residue is a major product industrial acenaphthylene 24, filtrate 25 is returned the back tower as raw material, output heavy wash oil 26 at the bottom of back tower 20 towers.
CN 92111855 1992-10-31 1992-10-31 Technology for extracting naphthalene fraction, methyl naphthalene fraction and industrial acenaphthene from coal-tar washing oil Expired - Fee Related CN1027544C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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CN101643380B (en) * 2008-08-08 2013-04-10 鞍钢集团工程技术有限公司 Process for producing industrial fluorene by coal tar wash oil

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CN1314780C (en) * 2005-07-27 2007-05-09 中钢集团鞍山热能研究院 Technique for processing hypothermal tar oil
CN1986735B (en) * 2006-12-13 2010-09-22 上海奥韦通工程技术有限公司 Processing method for medium and low temperature tar
CN101812311B (en) * 2009-12-17 2012-12-12 曲靖众一精细化工股份有限公司 Method for effectively refining tar anthracene oil and concentrating naphthalene
CN102267858A (en) * 2010-06-03 2011-12-07 鞍钢集团工程技术有限公司 Method and apparatus for producing industrial acenaphthene from wash oil of coal tar
CN101899313A (en) * 2010-07-29 2010-12-01 河南宝硕焦油化工有限公司 Oil-washing deep processing technology of coal tar
CN101982523B (en) * 2010-11-24 2013-03-20 孝义市金精化工有限公司 Washing oil continuous processing method
CN102180763B (en) * 2011-03-17 2014-01-29 宝舜科技股份有限公司 Method for fractionating industrial acenaphthene during wash oil processing
CN102776012B (en) * 2012-07-20 2014-04-09 山西永东化工股份有限公司 Method for reducing density of low-naphthalene washing oil
CN102876360B (en) * 2012-10-17 2015-08-05 新疆大学 Increase device of naphthalene and its derivative content and preparation method thereof in washing oil
CN104569257A (en) * 2014-12-23 2015-04-29 武汉钢铁(集团)公司 Gas chromatograph determination method of coking scrubbing oil distillation range
CN111334324A (en) * 2020-03-26 2020-06-26 河南开炭新材料有限公司 Production method of high-quality wash oil and coal tar processing method

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Publication number Priority date Publication date Assignee Title
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