CN101643380A - Process for producing industrial fluorene by coal tar wash oil - Google Patents
Process for producing industrial fluorene by coal tar wash oil Download PDFInfo
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- CN101643380A CN101643380A CN200810012775A CN200810012775A CN101643380A CN 101643380 A CN101643380 A CN 101643380A CN 200810012775 A CN200810012775 A CN 200810012775A CN 200810012775 A CN200810012775 A CN 200810012775A CN 101643380 A CN101643380 A CN 101643380A
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Abstract
The invention relates to a process for producing industrial fluorene by coal tar wash oil, which produces the industrial fluorene by taking heavy washing oil obtained by removing naphthalene, methylnaphthalene, dimethylnaphthalene, acenaphthene, and the like from coal tar washing oil as raw materials, and is characterized in that the heaving washing oil is taken as raw materials, and a continuousrectification method is adopted to extract fluorene fraction which is used for producing the qualified industrial fluorene and fluorene rich residual oil through processes of solvent crystallization or cooling crystallization, solvent reclamation, recrystallization and squeezing separation (or processes of washing, crystallization and solvent reclamation); and the residual oil is returned to the raw materials of the continuous rectification process. The process is suitable for a large-scale coal tar washing oil processing device, has high automation level of the continuous rectification process, and realizes the extraction of the fluorene fraction through once rectification of the heavy washing oil. The process has the advantages of simple operation, easy control and regulation, stable acquired fraction quality, low power consumption, high production efficiency and the like; and the fluorene rich residual oil is returned to the raw materials of the continuous rectification, so the yield of an industrial fluorene product can be remarkably improved.
Description
Technical field
The invention belongs to the coal tar manufacture field, specifically is a kind of processing method by producing industrial fluorene by coal tar wash oil.
Background technology
The typical process of existing producing industrial fluorene by coal tar wash oil is as shown in Figure 1: the heavy wash oil that removes with coal tar wash oil after the components such as naphthalene, methylnaphthalene, dimethylnaphthalene, acenaphthene is a raw material, heating in batch still 101, gas phase enters intermittent column 102, cat head oil gas enters backflash 104 after condenser 103 condensations, a cut part flows automatically to distillation tower 102 trim the top of column by backflash, all the other cuts enter separator tank 105, and Residual oil is sent outside at the bottom of the still.The starting fraction that enters separator tank 105 is sent outside, and cut groove before and after the front and back cut enters returns in the future and joins raw material and steam again.The fluorenes cut self-separation groove 105 that contains fluorenes about 60% enters fluorenes cut groove 106, being sent in the crystallizer 108 by fluorenes cut pump 107 then, adopt solvent crystallization, is that solvent carries out recrystallization with dimethylbenzene etc., after crystal solution is separated through whizzer 109, obtain the industrial fluorenes crystal of purity 〉=95%.The whizzer separated filtrate, or claim to take off brilliant mother liquor and deliver to dimethylbenzene and reclaim the unit.Can adopt method such as simple distillation to separate and take off brilliant mother liquor, the dimethylbenzene after the separation is reused, and removes oil product behind the dimethylbenzene for sending Residual oil outside.
Prior art adopts batch fractionating and solvent crystallization process combined flow process.Generally to have industrial scale little for batch fractionating technology, and operation easier is big, and automatization level is low, shortcomings such as power consumption height.The recrystallization method separation efficiency that dimethylbenzene is made solvent is low, obtain qualified industrial fluorenes crystal and only account for small part in the fluorenes cut that still kettle fractionates out in above-mentioned technological process, most fluorenes is stayed in the Residual oil and can't be extracted, and industrial fluorenes product yield is low, Residual oil contains fluorenes height, deficiency in economic performance.
Summary of the invention
The objective of the invention is to disclose a kind of processing method of from coal tar wash oil, separating the purifying industrial fluorenes, it is the explained hereafter fluorenes cut that heavy wash oil is adopted continuous rectification, the fluorenes cut enters crystalline element, can adopt the method for crystallisation by cooling or solvent crystallization to extract qualified industrial fluorenes earlier, remove solvent and remove wherein approaching processing such as non-fluorenes organism taking off brilliant mother liquor subsequently, obtain rich fluorenes Residual oil with the fluorenes boiling point; Also can adopt washings such as alcoholic solvent to remove non-fluorenes organism approaching in the fluorenes cut with the fluorenes boiling point, rich fluorenes cut after the washing adopts processing methodes such as benzene kind solvent crystallization or crystallisation by cooling, extract qualified industrial fluorenes, remove the fluorenes crystalline and take off brilliant mother liquor and after reclaiming solvent, can get rich fluorenes Residual oil.More than the rich fluorenes Residual oil that obtains of two kinds of methods all should return in the raw material that is fitted on continuous rectification.The present invention has not only improved the efficient of separating the purifying industrial fluorenes from coal tar wash oil, but also has improved the yield of industrial fluorenes product.
The objective of the invention is to realize by following processing method:
The heavy wash oil that removes with coal tar wash oil after the components such as naphthalene, methylnaphthalene, dimethylnaphthalene, acenaphthene is a raw material production industry fluorenes, be characterized in the heavy wash oil being that raw material adopts continuous rectificating technique to extract the fluorenes cut that contains fluorenes about 60%, the fluorenes cut adopts crystallisation by cooling or solvent crystallization method, the solvent crystallization method is to add solvent (as dimethylbenzene) at the fluorenes cut fluorenes is crystallized out, and produces 95% industrial fluorenes through centrifugation.Take off liquid phase material behind the crystalline substance for taking off brilliant mother liquor, this mother liquor enters solvent recovery unit and removes solvent, sends into crystallizer then, crystallization once more in Tc 0-5 ℃ scope.Send into the squeezing machine squeezing after filtering as the brilliant liquid of filter pulp and separate, approaching in the fluorenes cut to remove, fail to obtain the effectively isolating non-fluorenes organism that is soluble in this kind solvent at rectification working process with the fluorenes boiling point.Be rich fluorenes Residual oil after the filter cake fusion that squeezing obtains; In order to reach the manufacture fluorenes and to obtain the purpose of rich fluorenes Residual oil, also can adopt alcohols (as ethanol) solvent wash method, with the fluorenes cut by alcohols (as ethanol) extraction remove approaching in the fluorenes cut with the fluorenes boiling point, fail to obtain the effectively isolating non-fluorenes organism that is soluble in this kind solvent at rectification working process, rich fluorenes cut after the washing is with processing methodes such as solvent crystallization or crystallisation by cooling, contain the industrial fluorenes of fluorenes 〉=95% by product requirement production, taking off brilliant mother liquor and after reclaiming solvent, also can obtain rich fluorenes Residual oil after the Crystallization Separation.The rich fluorenes Residual oil that generates by above-mentioned processing method can return in the raw material that is fitted on the continuous rectification operation.
Processing method of the present invention has the following advantages and positively effect: this processing method coal tar wash oil processing unit (plant) that is suitable for maximizing, continuous rectificating technique automatization level height has realized that a rectifying of heavy wash oil cuts the fluorenes cut.This technology has simple to operate, is easy to control and adjusting, and the cut steady quality, the power consumption that cut are low, the production efficiency advantages of higher.Rich fluorenes Residual oil after the Crystallization Separation returns in the raw material that is fitted on continuous rectification, has obviously improved the yield of industrial fluorenes product.
Description of drawings
Accompanying drawing 1 is produced the process flow sheet of fluorenes for prior art;
Accompanying drawing 2 is the process flow sheet of one embodiment of the present invention;
Accompanying drawing 3 is the process flow sheet of another embodiment of the invention.
Embodiment
Below in conjunction with embodiment the specific embodiment of the present invention is elaborated
Embodiment 1, as shown in Figure 2: the heavy wash oil that the present invention removes with coal tar wash oil after the components such as naphthalene, methylnaphthalene, dimethylnaphthalene, acenaphthene is a tower 201 before raw material is sent into, in tower after normal pressure or rectification under vacuum, cut the fluorenes front-end volatiles at overhead condensation water cooler 103, this part fluorenes front-end volatiles is sent outside as a kind of byproduct.The bottoms material is sent into fluorenes tower 205 by fluorenes tower fresh feed pump 204, at the bottom of preceding tower 201 and fluorenes tower 205 towers by reboiler 202,208 heat supplies, material in fluorenes tower 205 through normal pressure or rectification under vacuum, at the bottom of the tower behind the extraction fluorenes cut Residual oil send outside.Cut the fluorenes cut that contains fluorenes about 60% at cat head.The fluorenes cut enters backflash 104 at fluorenes tower 205 cats head after condensate cooler 206 coolings, sending into cat head by reflux pump 207 parts refluxes, other sends into fluorenes cut groove 106, send into crystallizer 108 by fluorenes cut pump 107 again, carry out solvent crystallization or direct crystallisation by cooling with the dimethylbenzene equal solvent, Tc is between 20-40 ℃.Mother liquor after the crystallization carries out centrifugation through crystallization whizzer 109, and the crystal after the separation is the industrial fluorenes that contains fluorenes 〉=95%.Take off material behind the crystalline substance for taking off brilliant mother liquor, this mother liquor enters solvent recovery unit and removes solvent, sends into crystallizer 209 then, crystallization once more in Tc 0-5 ℃ scope.Send into squeezing machine 210 squeezings after filtering as the brilliant liquid of filter pulp and separate, the non-fluorenes component major part in the fluorenes cut is stored in squeezing raffinate inside and outside and send, and filter cake is sent into melting channel 211 heating fusions and is rich fluorenes Residual oil.Rich fluorenes Residual oil returns counterweight by 212 pumped back distillation unit and steams, before this richness fluorenes Residual oil can return and be fitted in tower charging or the charging of fluorenes tower, also can be separately as one charging of preceding tower or fluorenes tower.
In order to reach the manufacture fluorenes and to obtain the purpose of rich fluorenes Residual oil, also can adopt alcohols (as ethanol) solvent wash method, the fluorenes cut that cuts of distillation workshop section (fluorenes cut pump 107 backs) available alcoholic solvent (ethanol etc.) with the fluorenes cut by alcohols (as ethanol) extraction remove approaching in the fluorenes cut with the fluorenes boiling point, fail to obtain effective isolating non-fluorenes organism that is soluble in this kind solvent at rectification working process, alcoholic solvent after the washing can adopt method such as simple distillation to reclaim alcoholic solvent mutually, be rich in the fluorenes boiling point near but the vinasse that is soluble in alcoholic solvent send outside.Rich fluorenes cut after the washing is with processing methodes such as solvent crystallization or crystallisation by cooling, the industrial fluorenes that contains fluorenes 〉=95% by crystallization, centrifugation production, taking off brilliant mother liquor and can adopt methods such as simple distillation to remove solvent after the Crystallization Separation, the rich fluorenes Residual oil that obtains thereafter returns as raw material and is fitted on the distillation unit.
Adopt above different process that the rate of recovery of fluorenes is effectively improved, the rate of recovery can be greater than 65%.
Embodiment 2, and as shown in Figure 3, processing method of the present invention also can adopt a tower continuous rectification production equipment, and its flow process is:
The heavy wash oil raw material enters rectifying tower 301, and through normal pressure or rectification under vacuum, the extraction heavy still bottoms is sent outside at the bottom of the tower in tower.Cat head cuts the fluorenes front-end volatiles, and behind condensate cooler 103, the fluorenes front-end volatiles enter backflash 104, and a part of then fluorenes front-end volatiles are delivered in the tower by reflux pump 207 and refluxed, and all the other fluorenes front-end volatiles are sent outside.Cut the fluorenes cut at the discharging side line, through 304 coolings of fluorenes cut water cooler, the treatment process of cooled fluorenes cut such as the embodiment of front 1.Equally, rich fluorenes Residual oil can return and be fitted on the rectifying tower charging or advance tower as one raw material separately.
The tower that this processing method adopted can adopt packing tower, tray column, or filler and board-like bonded rectifying tower.
Claims (6)
1, a kind of processing method of producing industrial fluorene by coal tar wash oil, be that the heavy wash oil that removes with coal tar wash oil after the components such as naphthalene, methylnaphthalene, dimethylnaphthalene, acenaphthene is a raw material production industry fluorenes, it is characterized in that, adopt continuous rectification method to extract the fluorenes cut when the heavy wash oil raw material extracts the fluorenes cut, this fluorenes cut is as the intermediates of further manufacture fluorenes.
2, the processing method of a kind of producing industrial fluorene by coal tar wash oil according to claim 1 is characterized in that, the rich fluorenes Residual oil that extracts behind the industrial fluorenes returns in the raw material that is fitted on the continuous still battery operation.
3, the processing method of a kind of producing industrial fluorene by coal tar wash oil according to claim 2, it is characterized in that, take off brilliant mother liquor behind the separation industries fluorenes, remove non-fluorenes organism by cooling, crystallization, milling process as filtrate, the filter residue heating and melting obtains rich fluorenes Residual oil, this richness fluorenes Residual oil returns in the raw material that is fitted on the continuous still battery operation, or directly sends into distillation tower as one charging.
4, the processing method of a kind of producing industrial fluorene by coal tar wash oil according to claim 2, it is characterized in that, the fluorenes cut that distillation workshop section cuts extracts the non-fluorenes organism that removes in the fluorenes cut with alcoholic solvent with the fluorenes cut by alcohols, rich fluorenes cut after the washing is with the method manufacture fluorenes of solvent crystallization or crystallisation by cooling, centrifugation, the brilliant mother liquor of taking off after the centrifugation adopts method such as distillation to remove solvent, thereafter the rich fluorenes Residual oil that obtains returns in the raw material that is fitted on the continuous still battery operation, or directly sends into distillation tower as one charging.
5, the device that is used for the processing method of the described a kind of producing industrial fluorene by coal tar wash oil of claim 1 is characterized in that the continuous still battery tower adopts and to have the two-tower type of preceding tower and fluorenes tower, or adopts one tower.
6, according to the device of the processing method of a kind of producing industrial fluorene by coal tar wash oil of the described usefulness of claim 5, it is characterized in that described distillation tower adopts packing tower or plate tower, or filler and the board-like rectifying tower that combines.
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| CN 200810012775 CN101643380B (en) | 2008-08-08 | 2008-08-08 | Process for producing industrial fluorene by coal tar wash oil |
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| CN 200810012775 CN101643380B (en) | 2008-08-08 | 2008-08-08 | Process for producing industrial fluorene by coal tar wash oil |
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| CN101643380B CN101643380B (en) | 2013-04-10 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002380A (en) * | 2010-12-05 | 2011-04-06 | 天津市华瑞奕博化工科技有限公司 | Energy saving method of industrial fluorene distillation tower used in absorber oil processing |
| CN102776012A (en) * | 2012-07-20 | 2012-11-14 | 山西永东化工股份有限公司 | Method for reducing density of low-naphthalene washing oil |
| CN102807466A (en) * | 2012-07-20 | 2012-12-05 | 辽宁科技学院 | Process for purifying industrial fluorene |
| CN102898269A (en) * | 2012-10-17 | 2013-01-30 | 张家滔 | Supercritical extraction method for acenaphthene, fluorene and dibenzofuran in coal tar wash oil fraction |
| CN103304365A (en) * | 2013-06-28 | 2013-09-18 | 江西理工大学 | New process for purifying and refining coarse fluorene |
| CN103382148A (en) * | 2013-07-25 | 2013-11-06 | 攀钢集团攀枝花钢钒有限公司 | Industrial fluorene production process |
| CN110317124A (en) * | 2019-06-20 | 2019-10-11 | 袁玮 | The technique that environmental protection treatment produces the industrial residu that alkynes alcoholic product generates and waste coke oil |
| CN112933633A (en) * | 2021-04-12 | 2021-06-11 | 孝义市金精化工有限公司 | Negative-pressure continuous distillation and separation device for coal tar washing oil and coal tar washing oil separation and refining method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1027544C (en) * | 1992-10-31 | 1995-02-01 | 鞍山钢铁公司 | Technology for extracting naphthalene fraction, methyl naphthalene fraction and industrial acenaphthene from coal-tar washing oil |
| CN1208727A (en) * | 1997-08-14 | 1999-02-24 | 攀钢集团煤化工公司 | Continuous distillation technology for coking naphthalene oil fraction |
-
2008
- 2008-08-08 CN CN 200810012775 patent/CN101643380B/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002380A (en) * | 2010-12-05 | 2011-04-06 | 天津市华瑞奕博化工科技有限公司 | Energy saving method of industrial fluorene distillation tower used in absorber oil processing |
| CN102776012A (en) * | 2012-07-20 | 2012-11-14 | 山西永东化工股份有限公司 | Method for reducing density of low-naphthalene washing oil |
| CN102807466A (en) * | 2012-07-20 | 2012-12-05 | 辽宁科技学院 | Process for purifying industrial fluorene |
| CN102807466B (en) * | 2012-07-20 | 2014-07-16 | 辽宁科技学院 | Process for purifying industrial fluorene |
| CN102898269A (en) * | 2012-10-17 | 2013-01-30 | 张家滔 | Supercritical extraction method for acenaphthene, fluorene and dibenzofuran in coal tar wash oil fraction |
| CN103304365A (en) * | 2013-06-28 | 2013-09-18 | 江西理工大学 | New process for purifying and refining coarse fluorene |
| CN103304365B (en) * | 2013-06-28 | 2016-02-03 | 江西理工大学 | A kind of thick fluorenes purification novel process |
| CN103382148A (en) * | 2013-07-25 | 2013-11-06 | 攀钢集团攀枝花钢钒有限公司 | Industrial fluorene production process |
| CN103382148B (en) * | 2013-07-25 | 2015-06-17 | 攀钢集团攀枝花钢钒有限公司 | Industrial fluorene production process |
| CN110317124A (en) * | 2019-06-20 | 2019-10-11 | 袁玮 | The technique that environmental protection treatment produces the industrial residu that alkynes alcoholic product generates and waste coke oil |
| CN112933633A (en) * | 2021-04-12 | 2021-06-11 | 孝义市金精化工有限公司 | Negative-pressure continuous distillation and separation device for coal tar washing oil and coal tar washing oil separation and refining method |
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| CN101643380B (en) | 2013-04-10 |
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