CN102268273B - Deep processing technology for coking wash oil - Google Patents
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Abstract
The invention relates to a deep processing technology for coking wash oil. The coking wash oil serving as a raw material passes through three continuous rectification towers respectively provided with a side extraction port in sequence, so that a naphthalene fraction with naphthalene content of more than 80 percent, a beta-methyl naphthalene fraction with beta-methyl naphthalene content of more than 70 percent, an alpha-methyl naphthalene fraction with alpha-methyl naphthalene content of more than 60 percent, medium wash oil, an acenaphthene fraction with acenaphthene content of more than 60 percent, a dibenzofuran fraction with dibenzofuran content of more than 55 percent and a fluorene fraction with fluorene content of more than 50 percent can be extracted at one step. The technology iseasy to operate and low in equipment investment, has various types of product fractions, provides great convenience for further obtaining industrial products of naphthalene, beta-methyl naphthalene, alpha-methyl naphthalene, acenaphthene, fluorene and the like, and is particularly suitable for being matched with wash oil fraction deep processing of coal tar processing enterprises with scale of 15-30 megatons/year.
Description
Technical field
The invention belongs to chemical technology field, particularly a kind of deep processing technology of coking washing oil.
Background technology
Washing oil is a kind of mixture of complexity, is rich in valuable Organic Chemicals such as quinoline, isoquinoline 99.9, indoles, alpha-methyl-naphthalene, beta-methylnaphthalene, biphenyl, dimethylnaphthalene, acenaphthene, dibenzofuran and fluorenes.These Organic Chemicals are important intermediate of synthetic dyestuff, pigment, medicine, macromolecular material, need reasonably fully utilize this precious resources.
At present, domestic coal tar processing enterprise working ability is having about 30 families more than 100,000 tons/year, wherein Jue Dabufen working ability is between 150,000～300,000 tons/year, the washing oil throughput of enterprise of every family is generally at 10,000～20,000 tons/year, each tame enterprise areal distribution is very wide, this makes washing oil concentrate processing to become very difficult, becomes particularly important so seek a kind of working ability that is suitable at 10,000～20,000 tons/year oil-washing deep processing technology.
Patent CN 1078991A adopts the oil-washing deep processing technology of twin furnace double tower, two towers all respectively have a side line, extraction naphthalene cut, mixed methylnaphthalene cut, middle matter washing oil, acenaphthene cut and five kinds of cuts of heavy wash oil, that adopts this kind explained hereafter has Anshan iron and steel plant, Baogang, Wuhan Iron and Steel Plant, climbs coke-oven plant such as steel, and wherein major part is the intermittent phase of utilizing the twin furnace double tower to handle NAPTHALENE FLAKES. (INDUSTRIAL GRADE to handle washing oil.The cut that this twin furnace double tower process subject matter is extraction is meticulous inadequately, makes following process become difficult.Such as, before the extraction of tower side line be the mixed methylnaphthalene cut, contain methylnaphthalene 70%, the washing oil process scale can be produced this kind cut 0.3 ten thousand～0.5 ten thousand ton/year at 10,000～20,000 tons/year, this kind scale is uneconomical with continuous rectification, uses batch fractionating, must just can obtain qualified beta-methylnaphthalene through twice rectifying or a rectifying, a freezing and crystallizing, and yield is lower, has only 50%; The heavy wash oil of extraction is the mixed fraction of dibenzofuran and fluorenes at the bottom of the back Tata, needs further separation just can obtain dibenzofuran cut and fluorenes cut.
Patent CN 1208727A has proposed the technology of three stoves, three tower manufacture naphthalenes and methylnaphthalene, namely on the basis of NAPTHALENE FLAKES. (INDUSTRIAL GRADE twin furnace double tower, set up similar or identical rectifying tower and tube furnace, be raw material to mix naphtalene oil, the 3rd tower extraction methylnaphthalene and demethylation naphthalene washing oil, three rectifying tower all do not have side line, they also propose another kind of processing scheme simultaneously, the demethylation naphthalene washing oil that produces of looking unfamiliar namely is raw material, the course of processing is similar, produces lightweight washing oil, acenaphthene cut, dibenzofuran cut and four kinds of cut products of fluorenes cut.This technology subject matter is that facility investment is big, and the cut kind of output is few.Though be also referred to as three stoves, three tower process, its raw material is a kind of to be to mix naphtalene oil, produces carbolic oil, NAPTHALENE FLAKES. (INDUSTRIAL GRADE, technical methylnaphthalene and four kinds of products of demethylation naphthalene washing oil.Another kind of raw material is the demethylation naphthalene washing oil of producing previously, and the product of producing has lightweight washing oil, acenaphthene cut, dibenzofuran cut and fluorenes cut.So concerning the raw material washing oil, its essence is the complete processing of four stoves, four towers, the product of producing has technical methylnaphthalene, lightweight washing oil, acenaphthene cut, dibenzofuran cut and five kinds of narrow fractions of fluorenes cut.Not only equipment is many, and investment is big, and the cut kind of output is also less, such as can only the extraction mixed methylnaphthalene, produces beta-methylnaphthalene difficulty equally.
Patent CN 101899313 A have proposed a kind of oil-washing deep processing technology of eight tower continuous rectifications, and eight kinds of materials such as alpha-methyl-naphthalene, beta-methylnaphthalene are separated.This technological equipment investment is too big, and eight tower continuous rectification operation easier are very big, and the washing oil treatment capacity must go up certain scale just can have economy.Have, hundreds of component is arranged in the washing oil, the component of wherein congruent melting, azeotropic is a lot, only by rectifying just obtain content greater than 99% 2, it is very big that 6-dimethylnaphthalene, acenaphthene, dibenzofuran, fluorenes etc. implement difficulty.
(Zhang Xiongwen such as Zhang Xiongwen, Yan Hongfu. new daily use chemicals company washing oil processing technology brief introduction ［ J ］. fuel and chemical industry, 2002,33(4): 212-213) washing oil processing technology and the characteristics thereof of chemical company of Japanese Nippon Steel are introduced, its main technique is to cut middle oil at primary tower earlier, low naphthalene washing oil and Residual oil, low naphthalene washing oil is used for washing benzene, Residual oil gets industrial acenaphthylene through rectifying, middle oil cuts NAPTHALENE FLAKES. (INDUSTRIAL GRADE through the NAPTHALENE FLAKES. (INDUSTRIAL GRADE distillation tower, mixed methylnaphthalene cut and Residual oil, the rectifying in the methylnaphthalene distillation tower of mixed methylnaphthalene cut gets beta-methylnaphthalene cut and Residual oil, the beta-methylnaphthalene cut through rectifying tower again rectifying get purity greater than 98% beta-methylnaphthalene.Adopt above-mentioned washing oil complete processing, can obtain products such as high-quality washing oil, industrial acenaphthylene, NAPTHALENE FLAKES. (INDUSTRIAL GRADE, technical methylnaphthalene, beta-methylnaphthalene.From the washing oil complete processing of new daily use chemicals as can be seen, its technology is advanced, and quality product is also better, but that shortcoming is facility investment is big, only the production of beta-methylnaphthalene also needs two rectifying tower of methylnaphthalene tower and beta-methylnaphthalene tower except a tower of producing the mixed methylnaphthalene cut.So the washing oil complete processing of chemical company of Nippon Steel must reach certain scale and be only economical.
Summary of the invention
According to present domestic enterprise coal tar process scale mostly 150,000～300,000 tons/year present situation, the present invention aims to provide a kind of simple coking oil-washing deep processing technology, the washing oil process scale is adapted at 10,000～20,000 tons/year, can obtain plurality of narrow cuts such as naphthalene cut, beta-methylnaphthalene cut, alpha-methyl-naphthalene cut, middle matter washing oil, acenaphthene cut, dibenzofuran cut and fluorenes cut simultaneously, for follow-up various product separation provide great facility with making with extra care.Characteristics such as this technology has that facility investment is few, the product cut kind is many, following process is convenient, production operation is simple, reliable product quality, cost are low.
What the present invention adopted is the oil-washing deep processing technology of three stoves, three towers, and its technological process of production figure sees Fig. 1.
It is characterized in that comprising following process:
1. enter first rectifying tower from the middle part behind raw material washing oil and the cat head naphtalene oil steam heat-exchanging, cat head extraction naphthalene cut contains naphthalene greater than 80%, can return to be fitted on naphtalene oil or three and to mix and to produce content in the cuts greater than 95% NAPTHALENE FLAKES. (INDUSTRIAL GRADE; The beta-methylnaphthalene cut of top side line output contains beta-methylnaphthalene greater than 70%, and after quinoline, indoles were removed in pickling, a rectifying can obtain content greater than 96% beta-methylnaphthalene; The tower bottoms major part is got back in the tower after tube furnace heating, supplies with the tower heat in oil circulation mode, and all the other are as the raw material of second rectifying tower,
2. the first rectifying tower tower bottoms mixes with the acenaphthene raffinate of acenaphthene cut after crystallisation by cooling is centrifugal and enters second rectifying tower from the middle part, the alpha-methyl-naphthalene cut of cat head output contains alpha-methyl-naphthalene greater than 60%, after quinoline, indoles are removed in pickling, twice rectifying can obtain content greater than 95% alpha-methyl-naphthalene, or directly sells as mixed methylnaphthalene; The middle matter washing oil of top side line extraction can be used as the coke-oven plant and washes benzene usefulness; The tower bottoms major part is got back in the tower after tube furnace heating, supplies with the tower heat in oil circulation mode, and all the other are as the raw material of the 3rd rectifying tower,
3. the second rectifying tower tower bottoms enters the 3rd rectifying tower from the middle part, the content of cat head output greater than 60% acenaphthene cut after crystallisation by cooling is centrifugal, obtain content greater than 96% industrial acenaphthylene, filtrate is mixed the raw material as second rectifying tower with the first rectifying tower tower bottoms; The dibenzofuran cut of side line output contains dibenzofuran greater than 55%, can further produce dibenzofuran; The fluorenes cut of output contains fluorenes greater than 50% at the bottom of the tower, is the fabulous raw material of manufacture fluorenes.
The naphthalene cut of the described first rectifying tower cat head output contains naphthalene greater than 80%, can return to be fitted on naphtalene oil or three and to mix and to produce content in the cuts greater than 95% NAPTHALENE FLAKES. (INDUSTRIAL GRADE; The beta-methylnaphthalene cut of side line output contains beta-methylnaphthalene greater than 70%, after quinoline, indoles are removed in pickling, does not need freezing and crystallizing, and batch fractionating can obtain content greater than 97% beta-methylnaphthalene.
The alpha-methyl-naphthalene cut of the described second rectifying tower cat head output contains alpha-methyl-naphthalene greater than 60%, and after quinoline, indoles were removed in pickling, twice rectifying can obtain content greater than 95% alpha-methyl-naphthalene, or directly sells as mixed methylnaphthalene; The middle matter washing oil of side line extraction can be used as the coke-oven plant and washes benzene usefulness.
The content of described the 3rd rectifying tower cat head output after crystallisation by cooling is centrifugal, obtains content greater than 96% industrial acenaphthylene greater than 60% acenaphthene cut; The dibenzofuran cut of side line output contains dibenzofuran greater than 55%, can further produce dibenzofuran; The fluorenes cut of output contains fluorenes greater than 50% at the bottom of the tower, is the fabulous raw material of manufacture fluorenes.
The acenaphthene raffinate of described acenaphthene cut after crystallisation by cooling is centrifugal returns second rectifying tower as raw material.
The theoretical plate number of described three rectifying tower is 40～60, and tray column and packing tower all can.
The tower top temperature of described first rectifying tower is 218 ℃-224 ℃, and side stream temperature is 235 ℃-240 ℃, and column bottom temperature is 295 ℃-300 ℃.Tower spirit phase pressure is 35-40Kpa, the middle part charging, and side line extraction mouth is at 1/7 place of theoretical stage number.
The tower top temperature of described second rectifying tower is 240 ℃-245 ℃, and side stream temperature is 255 ℃-260 ℃, and column bottom temperature is 305 ℃-310 ℃.Tower spirit phase pressure is 35-40Kpa, the middle part charging, and side line extraction mouth is at 1/4 place of theoretical stage number.
The tower top temperature of described the 3rd rectifying tower is 265 ℃-270 ℃, and side stream temperature is 275 ℃-280 ℃, and column bottom temperature is 325 ℃-330 ℃.Tower spirit phase pressure is 35-40Kpa, the middle part charging, and side line extraction mouth is at 1/4 place of theoretical stage number.
The invention has the advantages that and only utilize three cover rectifying tower and the so simple equipment of tube furnace that the coking washing oil is carried out deep processing, can obtain naphthalene cut, beta-methylnaphthalene cut, alpha-methyl-naphthalene cut, middle matter washing oil, acenaphthene cut, dibenzofuran cut and seven kinds of narrow fractions of fluorenes cut simultaneously, for the separation of subsequent product with refiningly provide very big facility.The economic scale of this technology is for handling washing oil 10,000～20,000 ton/year.
Description of drawings
Fig. 1 is schematic flow sheet of the present invention
1-first rectifying tower; 2-second rectifying tower; 3-the 3rd rectifying tower; The 4-tube furnace; 5-acenaphthene crystallizer
Embodiment
The invention will be further described below in conjunction with Fig. 1 and by embodiment:
10000 tons/year of embodiment 1 washing oil treatment capacities
Three valve tray columns of Φ 900, stage number all is 81, the drum type brake tube furnace that three thermal loads are 1,000,000 kilocalories/hour.Raw material washing oil inlet amount is 1500kg/h.
As shown in Figure 1, enter first rectifying tower from the middle part after raw material washing oil and cat head naphtalene oil steam heat-exchanging reach 180 ℃-200 ℃, tower top temperature remains on 220 ℃-222 ℃, and it is the 84%(chromatography that the naphthalene cut of extraction contains the naphthalene amount); From top side line (several the 12nd block of column plates from top to bottom) extraction beta-methylnaphthalene cut, the extraction temperature is 237 ℃-238 ℃, contains beta-methylnaphthalene 72%, alpha-methyl-naphthalene 6.5%; Column bottom temperature remains on 297 ℃-298 ℃.Tower spirit phase pressure is 42KPa.
Enter second rectifying tower after Residual oil and the mixed of acenaphthene raffinate by 4:1 at the bottom of one Tata, tower top temperature remains on 242 ℃-243 ℃, and the alpha-methyl-naphthalene cut of extraction contains beta-methylnaphthalene 22%, alpha-methyl-naphthalene 62%; Matter washing oil from top side line (several the 20th block of column plates from top to bottom) extraction, the extraction temperature is 255 ℃-256 ℃; Column bottom temperature remains on 307 ℃-308 ℃.Tower spirit phase pressure is 30KPa.
Residual oil enters the 3rd rectifying tower from the tower middle part at the bottom of two Tatas, and tower top temperature remains on 267 ℃-268 ℃, and the acenaphthene cut of extraction contains acenaphthene 62%, dibenzofuran 8%; Top side line (several the 20th column plate places from top to bottom) extraction dibenzofuran cut, the extraction temperature is 278 ℃-279 ℃, contains acenaphthene 8%, dibenzofuran 58%, fluorenes 10%; Column bottom temperature remains on 328 ℃-329 ℃, and the fluorenes cut of extraction contains fluorenes 52%, dibenzofuran 8%, and tower spirit phase pressure is 38KPa.
15000 tons/year of embodiment 2 washing oil treatment capacities
Three valve tray columns of Φ 1000, stage number all is 81, the drum type brake tube furnace that three thermal loads are 1,200,000 kilocalories/hour.Raw material washing oil inlet amount is 2100kg/h.
Enter first rectifying tower from the middle part after raw material washing oil and cat head naphtalene oil steam heat-exchanging reach 180 ℃-200 ℃, tower top temperature remains on 220 ℃-222 ℃, and it is the 82%(chromatography that the naphthalene cut of extraction contains the naphthalene amount); From top side line (several the 12nd block of column plates from top to bottom) extraction beta-methylnaphthalene cut, the extraction temperature is 237 ℃-238 ℃, contains beta-methylnaphthalene 71%, alpha-methyl-naphthalene 7%; Column bottom temperature remains on 297 ℃-298 ℃.Tower spirit phase pressure is 40KPa.
Enter second rectifying tower after Residual oil and the mixed of acenaphthene raffinate by 4:1 at the bottom of one Tata, tower top temperature remains on 242 ℃-243 ℃, and the alpha-methyl-naphthalene cut of extraction contains beta-methylnaphthalene 24%, alpha-methyl-naphthalene 61%; Matter washing oil from top side line (several the 20th block of column plates from top to bottom) extraction, the extraction temperature is 255 ℃-256 ℃; Column bottom temperature remains on 307 ℃-308 ℃.Tower spirit phase pressure is 38KPa.
Residual oil enters the 3rd rectifying tower from the tower middle part at the bottom of two Tatas, and tower top temperature remains on 267 ℃-268 ℃, and the acenaphthene cut of extraction contains acenaphthene 62%, dibenzofuran 8%; Top side line (several the 20th column plate places from top to bottom) extraction dibenzofuran cut, the extraction temperature is 278 ℃-279 ℃, contains acenaphthene 8%, dibenzofuran 59%, fluorenes 9%; Column bottom temperature remains on 328 ℃-329 ℃, and the fluorenes cut of extraction contains fluorenes 53%, dibenzofuran 7%, and tower spirit phase pressure is 38KPa.
20000 tons/year of embodiment 3 washing oil treatment capacities
Three valve tray columns of Φ 1200, stage number all is 81, the drum type brake tube furnace that three thermal loads are 1,400,000 kilocalories/hour.Raw material washing oil inlet amount is 2800kg/h.
Enter first rectifying tower from the middle part after raw material washing oil and cat head naphtalene oil steam heat-exchanging reach 180 ℃-200 ℃, tower top temperature remains on 220 ℃-222 ℃, and it is the 82%(chromatography that the naphthalene cut of extraction contains the naphthalene amount); From top side line (several the 12nd block of column plates from top to bottom) extraction beta-methylnaphthalene cut, the extraction temperature is 237 ℃-238 ℃, contains beta-methylnaphthalene 71%, alpha-methyl-naphthalene 7%; Column bottom temperature remains on 297 ℃-298 ℃.Tower spirit phase pressure is 40KPa.
Enter second rectifying tower after Residual oil and the mixed of acenaphthene raffinate by 4:1 at the bottom of one Tata, tower top temperature remains on 242 ℃-243 ℃, and the alpha-methyl-naphthalene cut of extraction contains beta-methylnaphthalene 24%, alpha-methyl-naphthalene 61%; Matter washing oil from top side line (several the 20th block of column plates from top to bottom) extraction, the extraction temperature is 255 ℃-256 ℃; Column bottom temperature remains on 307 ℃-308 ℃.Tower spirit phase pressure is 38KPa.
Residual oil enters the 3rd rectifying tower from the tower middle part at the bottom of two Tatas, and tower top temperature remains on 267 ℃-268 ℃, and the acenaphthene cut of extraction contains acenaphthene 62%, dibenzofuran 8%; Top side line (several the 20th column plate places from top to bottom) extraction dibenzofuran cut, the extraction temperature is 278 ℃-279 ℃, contains acenaphthene 8%, dibenzofuran 58%, fluorenes 10%; Column bottom temperature remains on 328 ℃-329 ℃, and the fluorenes cut of extraction contains fluorenes 52%, dibenzofuran 8%, and tower spirit phase pressure is 38KPa.
Claims (1)
1. coking oil-washing deep processing technology, it comprises following process:
⑴ enter first rectifying tower behind raw material washing oil and the cat head naphtalene oil steam heat-exchanging, cat head extraction naphthalene cut, side line extraction beta-methylnaphthalene cut, tower bottoms is as the raw material of second rectifying tower;
⑵ the first rectifying tower tower bottoms and the acenaphthene raffinate of acenaphthene cut after crystallisation by cooling is centrifugal are mixed into second rectifying tower, cat head extraction alpha-methyl-naphthalene cut, the side line extraction mainly contains the middle matter washing oil of dimethylnaphthalene and biphenyl, and tower bottoms is as the raw material of the 3rd rectifying tower;
⑶ the second rectifying tower tower bottoms enters the 3rd rectifying tower, cat head extraction acenaphthene cut, and side line extraction dibenzofuran cut, tower bottoms is the fluorenes cut; It is characterized in that:
The naphthalene cut of the described first rectifying tower cat head output contains naphthalene greater than 80%, can return to be fitted on naphtalene oil or three and to mix and to produce content in the cuts greater than 95% NAPTHALENE FLAKES. (INDUSTRIAL GRADE; The beta-methylnaphthalene cut of side line output contains beta-methylnaphthalene greater than 70%, after quinoline, indoles are removed in pickling, does not need freezing and crystallizing, and batch fractionating namely obtains content greater than 97% beta-methylnaphthalene;
The alpha-methyl-naphthalene cut of the described second rectifying tower cat head output contains alpha-methyl-naphthalene greater than 60%, and after quinoline, indoles were removed in pickling, twice batch fractionating namely obtained content greater than 95% alpha-methyl-naphthalene, or directly sells as mixed methylnaphthalene; The middle matter washing oil of side line extraction is washed benzene as the coke-oven plant and is used;
The content of described the 3rd rectifying tower cat head output after crystallisation by cooling is centrifugal, obtains content greater than 96% industrial acenaphthylene greater than 60% acenaphthene cut; The dibenzofuran cut of side line output contains dibenzofuran greater than 55%, can further produce dibenzofuran; The fluorenes cut of output contains fluorenes greater than 50% at the bottom of the tower, is the fabulous raw material of manufacture fluorenes;
The tower top temperature of described first rectifying tower is 218 ℃-224 ℃, and side stream temperature is 235 ℃-240 ℃, and column bottom temperature is 295 ℃-300 ℃, and tower spirit phase pressure is 35-40KPa, the middle part charging, side line extraction mouth theoretical stage number from top to bottom the number 1/7 place;
The tower top temperature of described second rectifying tower is 240 ℃-245 ℃, and side stream temperature is 255 ℃-260 ℃, and column bottom temperature is 305 ℃-310 ℃, and tower spirit phase pressure is 35-40KPa, the middle part charging, side line extraction mouth theoretical stage number from top to bottom the number 1/4 place;
The tower top temperature of described the 3rd rectifying tower is 265 ℃-270 ℃, and side stream temperature is 275 ℃-280 ℃, and column bottom temperature is 325 ℃-330 ℃, and tower spirit phase pressure is 35-40KPa, the middle part charging, side line extraction mouth theoretical stage number from top to bottom the number 1/4 place.
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| CN103611328B (en) * | 2013-12-03 | 2015-03-25 | 天津市创举科技有限公司 | Process for extracting naphthalene by continuously rectifying heavy benzol |
| CN106336338A (en) * | 2015-07-09 | 2017-01-18 | 上海宝钢化工有限公司 | Method for removing quinoline in DMNO-3 |
| CN107129422A (en) * | 2016-02-28 | 2017-09-05 | 华东理工大学 | The continuous distillation method of high-purity biphenyl is extracted in a kind of tower first raffinate from crude benzol |
| CN107382653A (en) * | 2017-08-28 | 2017-11-24 | 贾海亮 | A kind of efficiently industrial acenaphthylene fractionating device |
| CN109053355B (en) * | 2018-09-29 | 2020-12-25 | 上海化工研究院有限公司 | Method for purifying biphenyl by continuous rectification |
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| CN101982523A (en) * | 2010-11-24 | 2011-03-02 | 孝义市金精化工有限公司 | Washing oil continuous processing method |
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| JPH02202592A (en) * | 1989-01-31 | 1990-08-10 | Nkk Corp | Separation and recovery of 2-methylnaphthalene |
| JP3657635B2 (en) * | 1994-10-24 | 2005-06-08 | 新日鐵化学株式会社 | Method for producing methylnaphthalene |
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