A kind of fractionating method that is used for washing oil processing industrial acenaphthylene
Technical field
The invention belongs to the coal tar manufacture field, be specifically related to a kind of fractionating method that is used for washing oil processing industrial acenaphthylene.
Background technology
Coal tar is coal at the liquid of vicidity that the high temperature pyrolysis process produces in the pit kiln coking chamber under the condition of secluding air.Coal tar is the important source of a kind of Organic Chemicals of preciousness, especially polycyclic aromatic hydrocarbons and heteroaromatic compounds, and wherein some product can't or can not be obtained from petrochemical materials economically.Anthracene, acenaphthene, pyrene as coking industry production can satisfy the world's 90% above demand, the carbazole of industrial usefulness 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 that cuts when wherein washing oil is coal tar distillation is 230~300 ℃ a cut, and its productive rate is 4.5%~6.5% of an anhydrous tar.Contain valuable Organic Chemicals such as naphthalene, methylnaphthalene, quinoline, indoles, biphenyl, acenaphthene, dibenzofuran, fluorenes, dimethylnaphthalene in the washing oil.Washing oil much is used for washing and absorbs coke-oven gas benzene hydrocarbon and various organic gas or the oil that directly acts as a fuel owing to have good solubility energy and stability, and this has caused the huge wasting of resources undoubtedly.
Acenaphthene content in washing oil is about 15%, and boiling point is 277.2 ℃ under the normal pressure, 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 chemical material, is mainly used in the particularly high-grade organic dye of synthetic dyestuff, 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.Because comprised bigger π-electron conjugated structure in the acenaphthene molecular structure, in the last few years, Many researchers synthesized a series of material with photo-sensitive characteristic and electroconductibility with the acenaphthene or derivatives thereof, 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 industrial acenaphthylene at present both at home and abroad from coal tar wash oil mainly is to adopt rectifying and crystalline coupling separation method, this is lower than simple rectifying separation energy consumption, has also saved investment cost of 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: the per GDP energy consumption reduces by 21%.Under this situation, require us when continually developing new forms of energy and substitute energy, take a series of measures to effectively increase energy savings and reduce material consumption energetically.
Those skilled in the art are known, energy-saving and cost-reducing technical process and waste heat recovery must being combined, can realize that like this energy consumption reduces significantly.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 big.In addition, because the boiling point of each material is higher in the wash oil fraction, and boiling point is more approaching, so energy consumption is also very high in the course of processing, the heat energy that a large amount of process streams carry directly is discharged in the atmosphere, and the waste heat of these processes is not used adequately reasonably.For example the cat head high-temperature steam advances the crystallization apparatus crystallization again behind the circulating heat conduction oil cooling usually, a large amount of gasification latent heats are recycled that thermal oil is taken away and loose in atmosphere, can utilize the gasification latent heat of high-temperature steam product to produce steam and can utilize for other workshop sections of factory.Because tubular oven stack gas has been carried a large amount of heat energy and has been directly released in the atmosphere, so funnel temperature is very big to the thermo-efficiency influence of tube furnace, the temperature of stack gas is high more, and thermosteresis is big more, thermo-efficiency is also low more in addition.If can fully recycle these waste heats, will reduce production costs, bring considerable economic to enterprise.
Summary of the invention
The present invention provides a kind of fractionating method that is used for washing oil processing industrial acenaphthylene in order to solve high this problem of industrial acenaphthylene separation column energy consumption in the present coal tar deep processing link.This technical process energy-saving effect is obvious, has high energy utilization rate.The industrial acenaphthylene product purity of this flow process gained〉95%, yield can reach more than 80%.
For achieving the above object, the technical solution used in the present invention is as follows:
The fractionating method that is used 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 the methylnaphthalene Tata and come the acenaphthene oil that takes off of autospasy acenaphthene oil groove to enter the industrial acenaphthylene separation column, the overhead vapours of industrial acenaphthylene separation column returns cat head as backflow through vapour generator condensation rear section, all the other as in the extraction of matter wash oil fraction; In the acenaphthene cut of the side line extraction liquid phase of acenaphthene separation column, in the tower bottoms circulation heating and 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 the industrial acenaphthylene crystallizer by pipeline after the heat exchanger condensation, adopt fusion-crystallization to be cooled to disposable blowing after the Tc lentamente, material after the crystallization obtains the industrial acenaphthylene product through the whizzer separation, and mother liquor is squeezed into after the heat exchanger preheating and taken off the acenaphthene oil groove.
Described industrial acenaphthylene separation column among the present invention, number of theoretical plate is 60~80, and the cat head working pressure is a 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 Tata that enters, the deep fat mass ratio is 0.35:1~0.5:1 at the bottom of the acenaphthene cut of side line extraction and the methylnaphthalene Tata that enters, deep fat and take off the acenaphthene oil content and do not do bifilar charging in the two sections corresponding position of tower at the bottom of the methylnaphthalene Tata; The deep fat feed entrance point is the 25th~40 a block of plate at the bottom of the tower, and taking off acenaphthene oil feed entrance point is the 40th~60 block of plate, and side line extraction position is 6~15 blocks of plates.
Air preheater among the present invention is the air preheater of single-revolution formula, its formation comprises the cylindrical rotor and the fixed housing composition of rotation, its rotor is a 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 with 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 commentaries on classics/min.
The gasification latent heat that adopts steam invention device to reclaim overhead vapours among the present invention produces low pressure steam, adopts rotary regenerative air preheater to improve the thermo-efficiency of tubular oven simultaneously.
Adopt vapour generator to reclaim the latent heat of acenaphthene fractionator overhead steam among the present invention, can make full use of the steam that this latent heat of vaporization produces 0.3~0.8MPa, use for other workshop sections in the factory.
The present invention proposes a kind of energy-saving technique of novel industrial acenaphthylene separation column, in addition flow process is introduced in waste heat recovery.Compared with prior art, the present invention has the following advantages:
(1) technical process is simple, realizes the serialization production operation, has alleviated labor strength;
(2) adopt the fusion-crystallization operation, avoided problems such as solvent recuperation and environmental pollution;
(3) air preheater and vapour generator are introduced flow process, make full use of the waste heat of process, further improved the thermo-efficiency of process, energy-saving effect is obvious.
Description of drawings
Fig. 1 is the schematic flow sheet of technology of the present invention.
The rotary regenerative air preheater synoptic diagram that Fig. 2 is among the present invention to be adopted.
Mark among the figure: 1-gas line, 2-hot-air duct, 3-cool flue gas pipeline, 4-cold-air duct, the 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 among the 11-, 12-acenaphthene cut pipeline, 13-heat exchanger, 14-industrial acenaphthylene crystallizer, 15-industrial acenaphthylene product conduit, 16-takes off the acenaphthene oil-piping, and 17-takes off the 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
The fractionating method that is used for washing oil processing industrial acenaphthylene of the present invention is implemented according to technical process shown in Figure 1, and it is specific as follows:
(1) enters industrial acenaphthylene separation column 9 from deep fat at the bottom of the tower at the bottom of the methylnaphthalene Tata by hot oil pipeline 8, come the acenaphthene oil that takes off of autospasy acenaphthene oil groove 17 to enter industrial acenaphthylene separation column 9, the overhead vapours of industrial acenaphthylene separation column 9 returns cat head as backflow through vapour generator 10 condensation rear sections, and the matter wash oil fraction is by middle matter wash oil fraction 11 extraction in all the other conducts.Pass through the acenaphthene cut of acenaphthene cut pipeline extraction liquid phase in the side line of industrial acenaphthylene separation column 9, tower bottoms circulation heating in 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 disposable blowing after the Tc lentamente, material after the crystallization obtains the industrial acenaphthylene product through the whizzer separation, mother liquor is squeezed into and is taken off acenaphthene oil groove 17 by taking off the acenaphthene oil-piping after heat exchanger 13 preheatings, takes off acenaphthene oil and enters industrial acenaphthylene separation column 9.
The number of theoretical plate of industrial acenaphthylene separation column is 60, and the cat head working pressure is a normal pressure, and tower top temperature is 248 ℃, and reflux ratio is 12:1.Deep fat and take off the acenaphthene oil content and do not do bifilar charging in the two sections corresponding position of tower at the bottom of the methylnaphthalene Tata, the flow of deep fat is 3020kg/h at the bottom of the tower.The deep fat feed entrance point is the 35th a block of plate at the bottom of the methylnaphthalene Tata, and taking off 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 cat head extraction: deep fat at the bottom of the methylnaphthalene Tata=0.35:1(mass ratio), the acenaphthene cut of side line extraction: deep fat=0.45:1 at the bottom of the methylnaphthalene Tata.The industrial acenaphthylene product that centrifugation obtains adopts the gas chromatographic analysis device to consist of the 95.26%(massfraction after drying), the acenaphthene rate of recovery reaches 84.6%.Tubular oven load 1289KW vapour generator per hour produces the water vapour of the 0.4MPa of 7.56t/h.
Air preheater in the present embodiment is a helicoid air preheater 5 shown in Figure 2, its formation comprises the cylindrical rotor 20 and the fixed housing composition of rotation, its rotor is a 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 with 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 commentaries on classics/min.
In the enforcement of the inventive method, when rotor 20 rotations, stack gas and air will be respectively through described air preheater adverse current and pass described heat accumulation plate 19 about in the of 5, and constantly generation heat exchange in the process of passing heat accumulation plate 19, with reference to Fig. 2 and in conjunction with Fig. 1: when hot flue gases 6 passes through, understand constantly with the described heat accumulation plate 19 of heat transferred, form after temperature reduces and enter chimney after 3 of cool flue gass pass through blower fan; 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.
Embodiment 2
Adopt the fractionation process of the foregoing description, different is: the number of theoretical plate of industrial acenaphthylene tower is 70, and the cat head working pressure is a normal pressure, and tower top temperature is 255 ℃, and reflux ratio is 10:1.Deep fat and take off the acenaphthene oil content and do not do bifilar charging in the two sections corresponding position of tower at the bottom of the tower at the bottom of the methylnaphthalene Tata, the flow of deep fat is 3020kg/h at the bottom of the tower.The deep fat feed entrance point is the 38th a block of plate at the bottom of the methylnaphthalene Tata, and taking off 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 cat head extraction: deep fat at the bottom of the methylnaphthalene Tata=0.34:1(mass ratio), the acenaphthene cut of side line extraction: deep fat=0.43:1 at the bottom of the methylnaphthalene Tata.The industrial acenaphthylene product that centrifugation obtains adopts the gas chromatographic analysis device to consist of the 96.18%(massfraction after drying), the acenaphthene rate of recovery reaches 86.5%.Tubular oven load 1079KW, vapour generator per hour produces the water vapour of the 0.4MPa of 6.33t/h.
Embodiment 3
Adopt the fractionation process of the foregoing description, different is: the number of theoretical plate of industrial acenaphthylene tower is 75, and the cat head working pressure is a normal pressure, and tower top temperature is 258 ℃, and reflux ratio is 18:1.Deep fat and take off the acenaphthene oil content and do not do bifilar charging in the two sections corresponding position of tower at the bottom of the tower at the bottom of the methylnaphthalene Tata, the flow of deep fat is 3020kg/h at the bottom of the tower.The deep fat feed entrance point is the 20th a block of plate at the bottom of the methylnaphthalene Tata, and taking off 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 cat head extraction: deep fat at the bottom of the methylnaphthalene Tata=0.3:1(mass ratio), the acenaphthene cut of side line extraction: deep fat=0.35:1 at the bottom of the methylnaphthalene Tata.The industrial acenaphthylene product that centrifugation obtains adopts the gas chromatographic analysis device to consist of the 95.65%(massfraction after drying), the acenaphthene rate of recovery reaches 85.9%.Tubular oven load 1079KW, vapour generator per hour produces the water vapour of the 0.6MPa of 6.35t/h.
Embodiment 4
Adopt the fractionation process of the foregoing description, different is: the number of theoretical plate of industrial acenaphthylene tower is 80, and the cat head working pressure is a normal pressure, and tower top temperature is 250 ℃, and reflux ratio is 16:1.Deep fat and take off the acenaphthene oil content and do not do bifilar charging in the two sections corresponding position of tower at the bottom of the tower at the bottom of the methylnaphthalene Tata, the flow of deep fat is 3020kg/h at the bottom of the tower.The deep fat feed entrance point is the 40th a block of plate at the bottom of the methylnaphthalene Tata, and taking off 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 cat head extraction: deep fat at the bottom of the methylnaphthalene Tata=0.4:1(mass ratio), the acenaphthene cut of side line extraction: deep fat=0.45:1 at the bottom of the methylnaphthalene Tata.The industrial acenaphthylene product that centrifugation obtains adopts the gas chromatographic analysis device to consist of the 96.18%(massfraction after drying), the acenaphthene rate of recovery reaches 86.2%.Tubular oven load 1079KW, vapour generator per hour produces the water vapour of the 0.8MPa of 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 the temperature of advancing the stove air, not only help the burning and the heat transfer of coal gas in the 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 reclaim the waste heat of product cut by vapour generator, utilize for other workshop sections of factory.
Such design makes the present invention have high energy utilization rate, the purpose that can reach save energy and reduce production costs significantly, and, industrial fluorenes product purity by this method gained〉95%, yield can reach more than 80%, can bring considerable economic 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, be described by preferred embodiment, person skilled obviously can be in not breaking away 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, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.