CN102180763B - Method for fractionating industrial acenaphthene during wash oil processing - Google Patents
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Abstract
The invention discloses a method for fractionating industrial acenaphthene during wash oil processing. The method comprises the following steps of: (1) allowing hot oil from the bottom of a methylnaphthalene tower and acenaphthene-removed oil from an acenaphthene-removing oil groove to enter an industrial acenaphthene fractionating tower, condensing steam on the top of the industrial acenaphthene fractionating tower by using a steam generator, allowing part of the condensed steam serving as backflow to return to the tower top, withdrawing the rest condensed steam serving as a medium-weight wash oil fraction, withdrawing a liquid phase acenaphthene fraction from the side line of the acenaphthene fractionating tower, circularly heating the residual oil at the bottom of the acenaphthene fractionating tower, discharging part of heavy wash oil, and allowing the heavy wash oil to enter a subsequent dibenzofuran tower for further distillation; and (2) condensing the withdrawn acenaphthene fraction by using a heat exchanger, allowing the acenaphthene fraction to enter an industrial acenaphthene crystallizer through a pipeline, performing melt crystallization, cooling slowly to the crystallization temperature, discharging materials at one time, separating the crystallized materials by using a centrifugal machine to obtain an industrial acenaphthene product, preheating the mother liquid by using the heat exchanger, and introducing the preheated mother liquid into the acenaphthene-removing oil groove. The method has the advantages that: the process flow is simple, continuous production operation can be realized, and the quality of the product is stable; the acenaphthene fraction entering the industrial acenaphthene crystallizer is subjected to melt crystallization and slow cooling operation, so that problems of solvent recovery and environmental pollution and the like are solved; and an air preheater and the steam generator are introduced into the flow.
Description
Technical field
The invention belongs to coal tar processing field, be specifically related to a kind of fractionating method for washing oil processing industrial acenaphthylene.
Background technology
Coal tar is the coal liquid of vicidity that high temperature pyrolysis process produces in coking chamber of coke oven under the condition of isolated air.Coal tar is the important sources of a kind of Organic Chemicals of preciousness, especially polycyclic aromatic hydrocarbons and heteroaromatic compounds, and wherein some product cannot or can not be obtained economically from petrochemical materials.Anthracene, acenaphthene, the pyrene as coking industry, produced can meet the above demand in the world 90%, the carbazole of industrial use and quinoline almost 100% ground from coke chemicals.
Coal tar generally obtains light oil, carbolic oil, naphtalene oil, washing oil, carbolineum and pitch through roughing, and the boiling range cutting when wherein washing oil is coal tar distillation is the cut of 230～300 ℃, and its productive rate is anhydrous tar 4.5%～6.5%.In washing oil, contain the valuable Organic Chemicals such as naphthalene, methylnaphthalene, quinoline, indoles, biphenyl, acenaphthene, dibenzofuran, fluorenes, dimethylnaphthalene.Washing oil is owing to having good solubility energy and stability, much for washing absorption coke-oven gas benzene hydrocarbon and various organic gas or directly as oil fuel, this has caused the huge wasting of resources undoubtedly.
Acenaphthene is content approximately 15% in washing oil, and under normal pressure, boiling point is 277.2 ℃, 95.3 ℃ of fusing points.Acenaphthene is water-soluble hardly, is slightly soluble in methyl alcohol, ethanol, propyl alcohol and Glacial acetic acid, is dissolved in benzene, toluene, trichloromethane and ether etc.Acenaphthene is a kind of important industrial chemicals, is mainly used in synthetic dyestuff particularly high-grade organic dye, coating, synthetic resins, engineering plastics etc.Acenaphthene also can be used as the intermediate of medicine, sterilant, sterilant, weedicide, plant growth hormones etc.Acenaphthene can directly be used as candle and the additive of hard wax and the protective agent of rubber and heatproof electrically insulating material etc.Owing to having comprised larger π-electron conjugated structure in acenaphthene molecular structure, in the last few years, Many researchers synthesized a series of material with photo-sensitive characteristic and electroconductibility with acenaphthene or derivatives thereof, and these materials can be as producing sealed cell.
Industrial acenaphthylene is mainly derived from the processing of coal tar wash oil cut, the method of extracting at present industrial acenaphthylene both at home and abroad from coal tar wash oil is mainly the coupling separation method that adopts rectifying and crystallization, this is lower than simple rectifying separation energy consumption, the investment cost of also having saved equipment simultaneously.The supply and demand situation of the current energy is more and more nervous, and country proposes an important goal of Eleventh Five-Year Plan: per Unit GDP Energy Consumption reduces by 21%.Under this situation, require us when continually developing new forms of energy and substitute energy, take energetically a series of measures to effectively increase energy savings and reduce material consumption.
Those skilled in the art are known, energy-saving and cost-reducing technical process and waste heat recovery must being combined, can realize like this energy consumption and significantly reduce.Existing industrial acenaphthylene separation column operational condition is much based on empirical design, and the operating parameters of process is not good, and this causes energy consumption very large.In addition, because the boiling point of each material in wash oil fraction is higher, and boiling point is more approaching, therefore energy consumption is also very high in the course of processing, the heat energy that a large amount of process streams carry is directly discharged in atmosphere, and the waste heat of these processes is not used adequately reasonably.For example tower top high-temperature steam enters crystallization apparatus crystallization after circulating heat conduction oil cooling again conventionally, a large amount of gasification latent heats are recycled thermal oil and take away and fall apart in atmosphere, and other workshop sections that can utilize the gasification latent heat of high-temperature steam product to produce steam Ke Gong factory utilize.Because tubular oven stack gas has been carried a large amount of heat energy and has been directly released in atmosphere, therefore funnel temperature is very large on the thermo-efficiency impact of tube furnace, the temperature of stack gas is higher in addition, and thermosteresis is larger, and thermo-efficiency is also lower.If can fully recycle these waste heats, the ，Gei enterprise that will reduce production costs brings considerable economic benefit.
Summary of the invention
The present invention, in order to solve high this problem of industrial acenaphthylene separation column energy consumption in current coal tar deep processing link, provides a kind of fractionating method for washing oil processing industrial acenaphthylene.This technical process energy-saving effect is obvious, has higher capacity usage ratio.The industrial acenaphthylene product purity >95% of this flow process gained, yield can reach more than 80%.
For achieving the above object, the technical solution used in the present invention is as follows:
Fractionating method for washing oil processing industrial acenaphthylene of the present invention, comprises the steps:
(1) from deep fat at the bottom of the tower at the bottom of methylnaphthalene tower tower and come the de-acenaphthene oil of autospasy acenaphthene oil groove to enter industrial acenaphthylene separation column, the overhead vapours of industrial acenaphthylene separation column returns to tower top as backflow through vapour generator condensation rear section, and all the other are as the extraction of middle matter wash oil fraction; In the acenaphthene cut of the side line extraction liquid phase of acenaphthene separation column, in tower bottoms circulating-heating the discharge section heavy wash oil of acenaphthene tower, heavy wash oil enters follow-up dibenzofuran tower and further distills.
(2) the acenaphthene cut of extraction enters industrial acenaphthylene crystallizer by pipeline after heat exchanger condensation, adopt fusion-crystallization to be cooled to lentamente disposable blowing after Tc, material after crystallization obtains industrial acenaphthylene product through whizzer separation, and mother liquor is squeezed into de-acenaphthene oil groove after heat exchanger preheating.
Described industrial acenaphthylene separation column in the present invention, number of theoretical plate is 60～80, and tower top working pressure is normal pressure, and tower top temperature is 248 ℃～258 ℃, and reflux ratio is 9:1～18:1.
The middle matter washing oil of industrial acenaphthylene fractionator overhead extraction is 0.3:1～0.4:1 with the mass ratio of deep fat at the bottom of the methylnaphthalene tower tower entering, the acenaphthene cut of side line extraction is 0.35:1～0.5:1 with deep fat mass ratio at the bottom of the methylnaphthalene tower tower entering, and at the bottom of methylnaphthalene tower tower, deep fat and de-acenaphthene oil content are not done bifilar charging in the two sections corresponding position of tower; At the bottom of tower, deep fat feed entrance point is 25th～40 blocks of plates, and de-acenaphthene oil feed entrance point is 40th～60 blocks of plates, and side line extraction position is 6～15 blocks of plates.
Air preheater in the present invention is the air preheater of single-revolution formula, its formation comprises that the cylindrical rotor of rotation and fixed housing form, its rotor is heating surface, it is divided into many storehouses lattice, heat accumulation plate (heat exchange element) is equipped with in the inside, fan-shaped T&B plate is divided into exhaust gases passes and air passageways by rotor: heat exchange element is laminated by the thick zores bar of 0.5～1.2mm, is contained in dismountable frame, is convenient to change.The rotating speed of described rotor is 1～3 turn/min.
The gasification latent heat that adopts steam invention device to reclaim overhead vapours in the present invention produces low pressure steam, adopts rotary regenerative air preheater to improve the thermo-efficiency of tubular oven simultaneously.
In the present invention, adopt vapour generator to reclaim the latent heat of acenaphthene fractionator overhead steam, can make full use of the steam that this latent heat of vaporization produces 0.3～0.8MPa, for other workshop sections in factory, use.
The present invention proposes a kind of energy-saving technique of novel industrial acenaphthylene separation column, in addition waste heat recovery is introduced to flow process.Compared with prior art, the present invention has the following advantages:
(1) technical process is simple, realizes serialization production operation, has alleviated labor strength;
(2) adopt fusion-crystallization operation, avoided the problems such as solvent recuperation and environmental pollution;
(3) air preheater and vapour generator are introduced to flow process, make full use of the waste heat of process, further improved the thermo-efficiency of process, energy-saving effect is obvious.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of technique of the present invention.
Fig. 2 is the rotary regenerative air preheater schematic diagram adopting in the present invention.
Mark in figure: 1-gas line, 2-hot-air duct, 3-cool flue gas pipeline, 4-cold-air duct, 5-rotary regenerative air preheater, 6-hot flue gases pipeline, 7-tubular oven, 8-hot oil pipeline, 9-industrial acenaphthylene separation column, 10-vapour generator, matter wash oil fraction pipeline in 11-, 12-acenaphthene cut pipeline, 13-heat exchanger, 14-industrial acenaphthylene crystallizer, 15-industrial acenaphthylene product conduit, 16-takes off acenaphthene oil-piping, and 17-takes off acenaphthene oil groove, 18-heavy wash oil pipeline, 19-heat exchange element, 20-rotor.
Embodiment
Below in conjunction with drawings and Examples, the inventive method is described in detail.
Embodiment 1
Fractionating method for washing oil processing industrial acenaphthylene of the present invention, is implemented according to the technical process shown in Fig. 1, and it is specific as follows:
(1) from deep fat at the bottom of the tower at the bottom of methylnaphthalene tower tower, by hot oil pipeline 8, enter industrial acenaphthylene separation column 9, come the de-acenaphthene oil of autospasy acenaphthene oil groove 17 to enter industrial acenaphthylene separation column 9, the overhead vapours of industrial acenaphthylene separation column 9 returns to tower top as backflow through vapour generator 10 condensation rear sections, all the other as middle matter wash oil fraction by middle matter wash oil fraction 11 extraction.Side line in industrial acenaphthylene separation column 9 passes through the acenaphthene cut of acenaphthene cut pipeline extraction liquid phase, in the tower bottoms circulating-heating of industrial acenaphthylene separation column 9, by heavy wash oil pipeline 18 discharge section heavy wash oils, heavy wash oil enters follow-up dibenzofuran tower and further distills.
(2) the acenaphthene cut of extraction enters industrial acenaphthylene crystallizer 14 by pipeline after heat exchanger 13 condensations, adopt fusion-crystallization to be cooled to lentamente disposable blowing after Tc, material after crystallization obtains industrial acenaphthylene product through whizzer separation, mother liquor is squeezed into de-acenaphthene oil groove 17 by de-acenaphthene oil-piping after heat exchanger 13 preheatings, and de-acenaphthene oil enters industrial acenaphthylene separation column 9.
The number of theoretical plate of industrial acenaphthylene separation column is 60, and tower top working pressure is normal pressure, and tower top temperature is 248 ℃, and reflux ratio is 12:1.At the bottom of methylnaphthalene tower tower, deep fat and de-acenaphthene oil content are not done bifilar charging in the two sections corresponding position of tower, and at the bottom of tower, the flow of deep fat is 3020kg/h.At the bottom of methylnaphthalene tower tower, deep fat feed entrance point is the 35th block of plate, and de-acenaphthene oil feed entrance point is the 50th block of plate, and side line extraction position is 10 blocks of plates.The middle matter washing oil of overhead extraction: deep fat=0.35:1(mass ratio at the bottom of methylnaphthalene tower tower), the acenaphthene cut of side line extraction: deep fat=0.45:1 at the bottom of methylnaphthalene tower tower.The industrial acenaphthylene product that centrifugation obtains after drying, adopts gas chromatographic analysis device to consist of 95.26%(massfraction), the acenaphthene rate of recovery reaches 84.6%.The water vapour of the 0.4MPa of tubular oven load 1289KW vapour generator generation per hour 7.56t/h.
Air preheater in the present embodiment is the helicoid air preheater 5 shown in Fig. 2, its formation comprises that the cylindrical rotor 20 of rotation and fixed housing form, its rotor is heating surface, it is divided into many storehouses lattice, heat accumulation plate (heat exchange element) 19 is equipped with in the inside, fan-shaped T&B plate is divided into exhaust gases passes and air passageways by rotor: heat exchange element is laminated by the thick zores bar of 0.5～1.2mm, is contained in dismountable frame, is convenient to change.The rotating speed of described rotor 20 is 1～3 turn/min.
In the enforcement of the inventive method, when rotor 20 rotation, stack gas and air are by respectively through described air preheater adverse current through described heat accumulation plate 19 Shang Xia 5, and constantly generation heat exchange in passing the process of heat accumulation plate 19, with reference to Fig. 2 and in conjunction with Fig. 1: when hot flue gases 6 passes through, can constantly transfer heat to described heat accumulation plate 19, temperature forms 3 of cool flue gass after reducing and after blower fan, enters chimney; When freezing air 4 flows through, can constantly from heat accumulation plate 19, absorb heat, 2 of the warm airs that temperature forms after raising enter described tubular oven 7 and participate in burning.
The fractionation process that adopts above-described embodiment, different: the number of theoretical plate of industrial acenaphthylene tower is 70, tower top working pressure is normal pressure, and tower top temperature is 255 ℃, and reflux ratio is 10:1.At the bottom of tower at the bottom of methylnaphthalene tower tower, deep fat and de-acenaphthene oil content are not done bifilar charging in the two sections corresponding position of tower, and at the bottom of tower, the flow of deep fat is 3020kg/h.At the bottom of methylnaphthalene tower tower, deep fat feed entrance point is the 38th block of plate, and de-acenaphthene oil feed entrance point is the 52nd block of plate, and side line extraction position is 12 blocks of plates.The middle matter washing oil of overhead extraction: deep fat=0.34:1(mass ratio at the bottom of methylnaphthalene tower tower), the acenaphthene cut of side line extraction: deep fat=0.43:1 at the bottom of methylnaphthalene tower tower.The industrial acenaphthylene product that centrifugation obtains after drying, adopts gas chromatographic analysis device to consist of 96.18%(massfraction), the acenaphthene rate of recovery reaches 86.5%.Tubular oven load 1079KW, the water vapour of the 0.4MPa of vapour generator generation per hour 6.33t/h.
The fractionation process that adopts above-described embodiment, different: the number of theoretical plate of industrial acenaphthylene tower is 75, tower top working pressure is normal pressure, and tower top temperature is 258 ℃, and reflux ratio is 18:1.At the bottom of tower at the bottom of methylnaphthalene tower tower, deep fat and de-acenaphthene oil content are not done bifilar charging in the two sections corresponding position of tower, and at the bottom of tower, the flow of deep fat is 3020kg/h.At the bottom of methylnaphthalene tower tower, deep fat feed entrance point is the 20th block of plate, and de-acenaphthene oil feed entrance point is the 40th block of plate, and side line extraction position is 6 blocks of plates.The middle matter washing oil of overhead extraction: deep fat=0.3:1(mass ratio at the bottom of methylnaphthalene tower tower), the acenaphthene cut of side line extraction: deep fat=0.35:1 at the bottom of methylnaphthalene tower tower.The industrial acenaphthylene product that centrifugation obtains after drying, adopts gas chromatographic analysis device to consist of 95.65%(massfraction), the acenaphthene rate of recovery reaches 85.9%.Tubular oven load 1079KW, the water vapour of the 0.6MPa of vapour generator generation per hour 6.35t/h.
The fractionation process that adopts above-described embodiment, different: the number of theoretical plate of industrial acenaphthylene tower is 80, tower top working pressure is normal pressure, and tower top temperature is 250 ℃, and reflux ratio is 16:1.At the bottom of tower at the bottom of methylnaphthalene tower tower, deep fat and de-acenaphthene oil content are not done bifilar charging in the two sections corresponding position of tower, and at the bottom of tower, the flow of deep fat is 3020kg/h.At the bottom of methylnaphthalene tower tower, deep fat feed entrance point is the 40th block of plate, and de-acenaphthene oil feed entrance point is the 60th block of plate, and side line extraction position is 15 blocks of plates.The middle matter washing oil of overhead extraction: deep fat=0.4:1(mass ratio at the bottom of methylnaphthalene tower tower), the acenaphthene cut of side line extraction: deep fat=0.45:1 at the bottom of methylnaphthalene tower tower.The industrial acenaphthylene product that centrifugation obtains after drying, adopts gas chromatographic analysis device to consist of 96.18%(massfraction), the acenaphthene rate of recovery reaches 86.2%.Tubular oven load 1079KW, the water vapour of the 0.8MPa of vapour generator generation per hour 6.62t/h.
Energy-saving effect of the present invention is obvious, and its conservation measures of introducing flow process comprises 2 points:
The one, utilize the smoke pre-heating air of tubular oven, improve into the temperature of stove air, be not only conducive to burning and the heat transfer of coal gas in tube furnace, can also reduce the funnel temperature of stack gas, thereby improve the thermo-efficiency of tubular oven;
The 2nd, utilize the latent heat of vaporization of overhead vapours to produce steam, and utilized by other workshop sections that vapour generator reclaims the waste heat ，Gong factory of product cut.
Such design, make the present invention there is higher capacity usage ratio, the object that can reach save energy and significantly reduce production costs, and, by the industrial fluorenes product purity >95% of the method gained, yield can reach more than 80%, can bring considerable economic benefit to enterprise.
Below in conjunction with the accompanying drawings and embodiments invention is schematically described.The present invention proposes a kind of energy-saving technique of novel industrial acenaphthylene separation column, by preferred embodiment, be described, person skilled obviously can be within not departing from content of the present invention, spirit and scope to structure as herein described with equipment is changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the artly, they are deemed to be included in spirit of the present invention, scope and content.
Claims (1)
1. for a fractionating method for washing oil processing industrial acenaphthylene, it is characterized in that comprising the steps:
(1) from deep fat at the bottom of the tower at the bottom of methylnaphthalene tower tower, by hot oil pipeline (8), enter industrial acenaphthylene separation column (9), come the de-acenaphthene oil of autospasy acenaphthene oil groove (17) to enter industrial acenaphthylene separation column (9), the overhead vapours of industrial acenaphthylene separation column (9) returns to tower top as backflow through vapour generator (10) condensation rear section, all the other as middle matter wash oil fraction by middle matter wash oil fraction pipeline (11) extraction; Side line in industrial acenaphthylene separation column (9) passes through the acenaphthene cut of acenaphthene cut pipeline (12) extraction liquid phase, in the tower bottoms of industrial acenaphthylene separation column (9) through tubular oven (7) circulating-heating, by heavy wash oil pipeline (18) discharge section heavy wash oil, heavy wash oil enters follow-up dibenzofuran tower and further distills;
(2) the acenaphthene cut of extraction enters industrial acenaphthylene crystallizer (14) by pipeline after heat exchanger (13) condensation, adopt fusion-crystallization to be cooled to lentamente disposable blowing after Tc, material after crystallization obtains industrial acenaphthylene product through whizzer separation, mother liquor is squeezed into de-acenaphthene oil groove (17) by de-acenaphthene oil-piping after heat exchanger (13) preheating, and de-acenaphthene oil enters industrial acenaphthylene separation column (9);
Wherein: the number of theoretical plate of described industrial acenaphthylene separation column is 60, tower top working pressure is normal pressure, tower top temperature is 248 ℃, reflux ratio is 12:1, at the bottom of methylnaphthalene tower tower, deep fat and de-acenaphthene oil content are not done bifilar charging in the two sections corresponding position of tower, and at the bottom of methylnaphthalene tower tower, the flow of deep fat is 3020kg/h, and at the bottom of methylnaphthalene tower tower, deep fat feed entrance point is the 35th block of plate, de-acenaphthene oil feed entrance point is the 50th block of plate, and side line extraction position is the 10th block of plate; The middle matter washing oil of overhead extraction: deep fat=0.35:1 at the bottom of methylnaphthalene tower tower, the acenaphthene cut of side line extraction: deep fat=0.45:1 at the bottom of methylnaphthalene tower tower; After drying, adopt its massfraction of gas chromatographic analysis is 95.26% to the industrial acenaphthylene product that centrifugation obtains, and the acenaphthene rate of recovery reaches 84.6%; Tubular oven load is 1289kW, the water vapour of the 0.4MPa of vapour generator generation per hour 7.56t;
Tubular oven (7) is connected with rotary regenerative air preheater (5), rotary regenerative air preheater (5) comprises cylindrical rotor (20) and the fixed housing of rotation, its rotor is heating surface, it is divided into many storehouses lattice, heat accumulation plate is equipped with in the inside, be heat exchange element (19), fan-shaped T&B plate is divided into exhaust gases passes and air passageways by rotor, heat exchange element is laminated by the thick zores bar of 0.5～1.2mm, be contained in dismountable frame, be convenient to change, the rotating speed of described rotor (20) is 1～3 turn/min;
When rotor (20) rotates, stack gas and air will also pass described heat accumulation plate through the upper and lower adverse current of described air preheater (5) respectively, and constantly generation heat exchange in passing the process of heat accumulation plate, when hot flue gases passes through, can constantly transfer heat to described heat accumulation plate, temperature forms cool flue gas after reducing and after blower fan, enters chimney; When cold air flow is out-of-date, can constantly from heat accumulation plate, absorb heat, the warm air that temperature forms after raising enters described tubular oven (7) and participates in burning.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078991A (en) * | 1992-10-31 | 1993-12-01 | 鞍山钢铁公司 | From coal tar wash oil, extract the technology of naphthalene cut, methylnaphthalene and industrial acenaphthylene |
| 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 |
| CN101982523A (en) * | 2010-11-24 | 2011-03-02 | 孝义市金精化工有限公司 | Washing oil continuous processing method |
-
2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078991A (en) * | 1992-10-31 | 1993-12-01 | 鞍山钢铁公司 | From coal tar wash oil, extract the technology of naphthalene cut, methylnaphthalene and industrial acenaphthylene |
| 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 |
| 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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