CN101643380A - Process for producing industrial fluorene by coal tar wash oil - Google Patents

Process for producing industrial fluorene by coal tar wash oil Download PDF

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CN101643380A
CN101643380A CN 200810012775 CN200810012775A CN101643380A CN 101643380 A CN101643380 A CN 101643380A CN 200810012775 CN200810012775 CN 200810012775 CN 200810012775 A CN200810012775 A CN 200810012775A CN 101643380 A CN101643380 A CN 101643380A
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fluorene
oil
process
fraction
coal tar
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CN 200810012775
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CN101643380B (en )
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徐蓬勃
梁洪淼
波 王
陆友文
马中全
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鞍钢集团设计研究院
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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

一种煤焦油洗油生产工业芴的工艺方法 Coal tar oil washing process for the production of fluorene

技术领域 FIELD

本发明属于煤焦油加工领域,具体是一种由煤焦油洗油生产工业芴的工艺方法。 The present invention belongs to the field of coal tar processing, in particular to a process for the production of oil from coal tar washing fluorene. 背景技术 Background technique

现有煤焦油洗油生产工业芴的典型工艺如附图1所示:以煤焦油洗油脱除萘、甲基萘、二甲基萘、苊等组分后的重质洗油为原料,在间歇蒸馏 A typical coal tar wash oil production process prior fluorene as shown in Figure 1: coal tar wash oil to remove naphthalene, methylnaphthalene, dimethylnaphthalene, acenaphthene heavy components after wash oil as raw material, in the batch distillation

釜101中加热,气相进入间歇蒸馏塔102,塔顶油气经冷凝器103冷凝后进入回流槽104,馏分一部分由回流槽自流到蒸馏塔102塔顶回流,其余馏分进入分离槽105,釜底残油外送。 Heating tank 101, gaseous phase into batch distillation column 102, 103 into the return slot 104 after the condensed hydrocarbon overhead through the condenser, part of fraction gravity from the tank to the reflux for the distillation column 102 overhead reflux, the remaining fraction into the separation tank 105, still bottoms residue outside the oil delivery. 进入分离槽105的初馏分外送,前后馏分进入前后馏分槽,日后回配原料复蒸。 First fraction into the separation groove 105 for delivery, fraction fraction longitudinal groove into the front, back later with steaming material. 含芴60%左右的芴馏分自分离槽105 进入芴馏分槽106,然后由芴馏分泵107送入结晶器108内,采用溶剂结晶法,以二甲苯等为溶剂进行重结晶,结晶液经过离心机109分离后,得到纯度》95%的工业荷晶体。 Fluorene fluorene fraction of about 60% from the separation tank 105 into the groove 106 fluorenyl fraction, and then fed from the pump 107 fluorenyl fraction crystallizer 108, by solvent crystallization, and the like xylene as solvent recrystallization, crystallization solution after centrifugation after separation unit 109, purity> 95% charge of industrial crystals. 离心机分离的滤液,或称脱晶母液送到二甲苯回收单元。 Centrifuge filtrate, or the mother liquor, said crystals to de-xylene recovery unit. 可采用简单蒸馏等方法分离脱晶母液,分离后的二甲苯重复使用, 脱除二甲苯后的油品为外送残油。 Simple distillation or the like can be separated off crystal mother liquor after the separation repeated use of xylene, oil xylene is removed after the outgoing resid.

现有技术采用间歇精馏和溶剂结晶相结合的工艺流程。 Prior art batch distillation and solvent crystallization process in combination. 通常情况下间歇精馏工艺具有生产规模小,操作难度大,自动化水平低,动力消耗高等缺点。 Typically a batch distillation small scale production and difficult operation, the low level of automation, power consumption disadvantages. 二甲苯作溶剂的重结晶法分离效率低,在上述工艺过程中获得合格的工业芴晶体只占蒸馏釜分馏出的芴馏分中的少部分,大部分的笏留在残油中无法提取,工业芴产品收率低,残油含芴高,经济效益差。 Separation efficiency is low recrystallization xylene as a solvent, the above-described process to obtain a qualified fluorene crystals only a small portion of the fractionated distillation still fluorene fraction, most of the residual oil left in Wat can not be extracted, industrial low production yield fluorene, fluorene-containing residual oil high economic efficiency is poor. 发明内容 SUMMARY

本发明的目的在于公开一种从煤焦油洗油中分离提纯工业芴的工艺方法,是对重质洗油采用连续精馏的工艺生产芴馏分,芴馏分进入结晶单元, 可先采用冷却结晶或溶剂结晶的方法提取合格工业芴,随后对脱晶母液进行脱除溶剂及脱除其中与芴沸点接近的非芴有机物等处理,得到富芴残油;也可采用醇类溶剂等洗涤脱除芴馏分中与芴沸点接近的非笏有机物,洗涤后的富芴馏分采用苯类溶剂结晶或冷却结晶等工艺方法,提取合格工业荷, 脱除芴晶体的脱晶母液在回收溶剂后可得富芴残油。 Object of the present invention is to disclose a process for purifying wash from coal tar oil fluorene separation, washing oil is a heavy process to produce a continuous distillation fraction fluorene, fluorene fraction into the crystallization unit may be employed before the cooling crystallization or passing the solvent extraction fluorene crystallization, followed by removal of the solvent was removed and the mother liquid crystal removing treatment wherein the fluorene close boiling organics and other non-fluorene, fluorene-rich raffinate obtained; the like may also be washed with an alcohol solvent removal fluoren close boiling fraction and a non-fluorene Wat organics-rich fraction fluorene washed using benzene solvent crystallization or cooling crystallization process for extraction industry qualified charge, removal of fluorene crystals off crystal mother liquor obtained after recovering the rich solvent fluorene residual oil. 以上两种方法得到的富芴残油均应回配到连续精馏的原料中。 The above two methods of residual oil-rich fluorene should be back with the continuous distillation of raw materials. 本发明不但提高了从煤焦油洗油中分离提纯工业芴的效率,而且还提高了工业芴产品的收率。 The present invention not only improves the efficiency of the separation and purification of the fluorene from coal tar wash oil, but also increasing the yield of fluorene products. 本发明的目的是通过下述工艺方法实现的: Object of the present invention are achieved by the following process methods:

以煤焦油洗油脱除萘、甲基萘、二甲基萘、苊等组分后的重质洗油为原料生产工业芴,其特点是以重质洗油为原料采用连续精馏工艺提取含芴60%左右的芴馏分,芴馏分采用冷却结晶或溶剂结晶方法,溶剂结晶方法是在芴馏分加入溶剂(如二甲苯)使芴结晶出来,经离心分离生产出95%工 After the heavy coal tar oil wash to remove naphthalene, methylnaphthalene, dimethylnaphthalene, acenaphthene wash oil component as raw material fluorene, which is characteristic of heavy oil as raw material wash continuous distillation extraction process fluorene fluorene fraction of about 60%, fluorenyl or solvent fraction crystallization using cooling crystallization method, the crystallization solvent is added in a fraction fluorene solvent (such as xylene) fluorene crystallized, centrifuged to produce a 95% ENGINEERING

业芴。 Fluorene industry. 脱晶后的液相物料为脱晶母液,该母液进入溶剂回收单元脱除溶剂, The liquid crystal material after removal of off crystal mother, liquor into the solvent recovery unit the solvent was removed,

然后送入结晶器,在结晶温度0-5'C范围内再次结晶。 It is then fed to a crystallizer, crystallized again within a crystallization temperature range 0-5'C. 作为滤浆的晶液过滤后送入压榨机压榨分离,以脱除芴馏分中与芴沸点接近、未能在精馏工序得到有效分离的易溶于该类溶剂的非芴有机物。 After filtering the slurry as crystals was filtered into the press pressing separated to remove fluorene fluorene close boiling fraction, it has not been effectively separated in the distillation step to a non-soluble organics such solvents fluorenyl. 压榨得到的滤饼熔融后即为富芴残油;为了达到生产工业芴及得到富芴残油的目的,也可采用醇类(如乙醇)溶剂洗涤方法,将芴馏分通过醇类(如乙醇)萃取脱除芴馏分中与芴沸点接近、未能在精馏工序得到有效分离的易溶于该类溶剂的非苑有机物,洗涤后的富芴馏分用溶剂结晶或冷却结晶等工艺方法,按产品要求生产含芴^95。 The press cake obtained after melting fluorene-rich raffinate; To achieve the object of the production of fluorene and fluorene obtained residual oil-rich, an alcohol (e.g. ethanol) may also be washed with a solvent method, fluorene fraction by alcohols (e.g., ethanol ) removal of fluorene was extracted with fluorene close boiling fraction, it has not been effectively separated in the distillation step to a non-soluble organics such solvents Yuan, fluorene-rich fraction with a solvent crystallization or cooling crystallization method after the washing process, by fluorene-containing products require production ^ 95. /。 /. 的工业芴,结晶分离后的脱晶母液在回收溶剂后亦可得到富芴残油。 The fluorene, separating off the crystals after crystallization mother liquor obtained after recovering the solvent may fluorenyl rich raffinate. 通过上述工艺方法生成的富芴残油可以回配到连续精馏工序的原料中。 Generated by the above process can be enriched raffinate fluorenyl ligand to feed back the continuous distillation step.

本发明工艺方法具有以下优点和积极效果:该工艺方法适于大型化煤 Process of the present invention has the following advantages and positive effects: the method is adapted to process coal size

焦油洗油加工装置,连续精馏工艺自动化水平高,实现了重质洗油一次精馏切取芴馏分。 Tar wash oil processing apparatus, a continuous distillation process a high level of automation, to achieve a heavy wash oil fraction is a distillation cut fluorene. 该工艺具有操作简单,易于控制和调节,切取的馏分质量稳定、动力消耗低,生产效率高等优点。 The process is simple, easy to control and adjust, cut fraction stable quality, low power consumption, high production efficiency. 结晶分离后的富莉残油回配到连续精馏的原料中,明显提高了工业芴产品的收率。 Li-rich raffinate back isolated after crystallization with continuous distillation of the feedstock, significantly increasing the yield of fluorene products. 附图说明 BRIEF DESCRIPTION

附图1为现有技术生产芴的工艺流程图; Figure 1 is a prior art production flow chart fluorene;

4附图2为本发明的一种实施方式的工艺流程图; 附图3为本发明的另一种实施方式的工艺流程图。 Process flow diagram of an embodiment 4 of the present invention FIG. 2; FIG. 3 of the present invention is a process flow diagram of another embodiment of the embodiment. 具体实施方式 detailed description

下面结合实施例对本发明的具体实施方式做详细说明 The following embodiments in conjunction with the specific embodiments of the present invention are described in detail

实施例l,如图2所示:本发明以煤焦油洗油脱除萘、甲基萘、二甲基 Example L, 2: In the present invention, the removal of coal tar wash oil naphthalene, methylnaphthalene, dimethyl

萘、苊等组分后的重质洗油为原料送入前塔201,在塔内经常压或减压精馏后,在塔顶冷凝冷却器103切取芴前馏分,这部分芴前馏分作为一种副产品外送。 After naphthalene, acenaphthene after heavy oil as raw material components into the wash before column 201, at normal pressure or reduced pressure distillation column, condensed in the cooler 103 before overhead distillate cut fluorenyl, fluorenyl front part of this fraction as send outside a byproduct. 塔底物料由芴塔进料泵204送入芴塔205,前塔201和芴塔205塔底通过再沸器202、 208供热,物料在芴塔205内经常压或减压精馏,塔底采出荷馏分后残油外送。 Column bottoms fluorene fluorene feed pump 204 into column 205, column 201 and fluorenyl front column 205 through bottom reboiler 202, 208 heat, the material in the distillation normal pressure or reduced pressure within the fluorene column 205, column Produced outer bottom resid feed bEARING fraction. 在塔顶切取含药60%左右的芴馏分。 Cut at the top 60% of the drug-containing fluorene fraction. 銜馏分在銜塔205塔顶经冷凝冷却器206冷却后进入回流槽104,通过回流泵207 —部分送入塔顶进行回流,其它送入芴馏分槽106,再由芴馏分泵107送入结晶器108,用二甲苯等溶剂进行溶剂结晶或直接冷却结晶,结晶温度在20-40 。 Title fraction was condensed into the cooler 206 is cooled in the title column 205 overhead reflux tank 104 through return pump 207-- reflux into the overhead portion, a fluorenyl other fraction into the groove 106, and then into the crystal fraction from the pump 107 fluoren 108, direct crystallization or solvent cooling crystallization solvent such as xylene, 20-40 crystallization temperature. C之间。 Between C. 结晶后的母液经结晶离心机109进行离心分离,分离后的晶体为含荷》95%的工业芴。 Crystallization mother liquor after crystallization was centrifuged centrifuge 109, containing crystals separated charge "95% fluorene. 脱晶后的物料为脱晶母液,该母液进入溶剂回收单元脱除溶剂,然后送入结晶器209,在结晶温度0-5"C范围内再次结晶。作为滤浆的晶液过滤后送入压搾机210压榨分离,芴馏分中的非芴组分大部分存于压榨残液里外送,滤饼送入熔化槽211加热熔解即为富药残油。富荷残油由212泵送回蒸馏单元回配重蒸,该富芴残油即可回配到前塔进料或芴塔进料中,亦可单独作为前塔或芴塔的一股进料。 After removal of crystalline material off crystal mother liquor, the mother liquor into the solvent recovery unit the solvent was removed, and then fed to the crystallizer 209, 0-5 "C crystallized again within a crystallization temperature range as liquid crystal slurry was filtered after filtration fed press 210 press separation, most of the non-fluorene fluorene fraction components present in the raffinate in the press outgoing cake was heated and melted into a melting bath 211 is the oil-rich drug residue-rich raffinate from the charge pump 212 back to back with redistilled distillation unit, fluorene-rich residuum to the front to back with the column feed or feed fluorenyl column, also as an individual feed or fluorenyl column before the column.

为了达到生产工业芴及得到富芴残油的目的,也可采用醇类(如乙醇) 溶剂洗涤方法,蒸馏工段切取的芴馏分(芴馏分泵107后)可用醇类溶剂(乙醇等)将芴馏分通过醇类(如乙醇)萃取脱除笏馏分中与荷沸点接近、 未能在精馏工序得到有效分离的易溶于该类溶剂的非芴有机物,洗涤后的醇类溶剂相可采用简单蒸馏等方法回收醇类溶剂,富含与药沸点接近但易溶于醇类溶剂的蒸馏残液外送。 To achieve the object of the production of fluorene and fluorene obtained rich residual oil, may be employed alcohols (e.g. ethanol) solvent washing method, a distillation section cut fraction fluorene (fluorene fraction pump 107) may be an alcohol solvent (ethanol etc.) fluorene fraction by alcohols (e.g., ethanol) and extracted with charge removal Wat close boiling fraction, has not been effectively separated in the distillation step to a non-soluble organics such solvents fluorenyl, an alcohol solvent phase after washing can be simple alcohol solvents such as distillation recovered, rich in close drugs but soluble in an alcoholic solvent having a boiling point distillation residue outgoing. 洗涤后的富芴馏分相用溶剂结晶或冷却结晶等工艺方法,通过结晶、离心分离生产含芴》95%的工业芴,结晶分离后的脱晶母液可采用简单蒸馏等方法脱除溶剂,其后得到的富芴残油作为原料回配到蒸馏单元。 Fluorene-rich phase with a solvent fraction crystallization or cooling crystallization method after the washing process and the like, by crystallization, centrifugation production of fluorene-containing> 95% of fluorene, after crystallization mother liquid crystals can be separated off simple method such as removal of the solvent by distillation, which after obtaining rich raffinate as a raw material fluorene ligand back to the distillation unit.

采用以上不同工艺均可使芴的回收率得到有效提高,回收率可大于 With the above processes can make different fluorene recovery is effectively improved, the recovery may be greater than

65%。 65%.

实施例2,如附图3所示,本发明工艺方法也可采用一塔式连续精馏生产装置,其流程为- Example 2, as shown in Figure 3, the process of this invention may also be a continuous distillation tower production facility, which is a process -

重质洗油原料进入精馏塔301,在塔内经常压或减压精馏,塔底采出重质残油外送。 Wash the heavy oil feedstock into the fractionator 301, normal pressure or reduced pressure in the distillation column, the produced heavy resid bottoms Delivery. 塔顶切取芴前馏分,经冷凝冷却器103后,芴前馏分进入回流槽104,然后一部分芴前馏分通过回流泵207送到塔中进行回流,其余芴前馏分外送。 The overhead fraction before cutting takes fluorenyl, condensed cooler 103, the groove 104 cut into the return before fluorene, fluorene and the front portion of the fraction is refluxed by the reflux pump 207 to the column, before the remaining fraction Delivery fluorene. 在出料侧线切取銜馏分,经芴馏分冷却器304冷却,冷却后的芴馏分的处理工艺如前面的实施例l。 Outfeed side-cut fraction title, cooled by cooler 304 fraction fluorene, fluorene fraction treatment process after cooling as in the previous Example l. 同样,富芴残油可回配到精馏塔进料或单独作为一股原料进塔。 Similarly, fluorene-rich raffinate can return to the distillation column equipped with a separate feed or as an starting material into the tower.

本工艺方法所采用的塔器可采用填料塔、板式塔,或填料与板式结合的精馏塔。 The method of the present process can be used in a packed column tower, plate tower or packed distillation column with a plate binding.

Claims (6)

  1. 1、一种煤焦油洗油生产工业芴的工艺方法,是以煤焦油洗油脱除萘、甲基萘、二甲基萘、苊等组分后的重质洗油为原料生产工业芴,其特征在于,从重质洗油原料提取芴馏分时采用连续精馏法提取芴馏分,该芴馏分作为进一步生产工业芴的中间产品。 1. A process for coal tar oil produced fluorene washing, the coal tar is a heavy oil wash to remove naphthalene, methylnaphthalene, dimethylnaphthalene, acenaphthene wash oil component as raw material fluorene, characterized in that the wash from the heavy oil feedstock was extracted by continuous distillation extraction method fluorene fluorene fraction fraction when the further production of fluorene fluorene fraction as an intermediate product.
  2. 2、 根据权利要求1所述的一种煤焦油洗油生产工业芴的工艺方法,其特征在于,提取工业药后的富芴残油回配到连续蒸馏工序的原料中。 2, the coal tar according to claim 1, process for the production of oil washing fluorene, wherein the fluorene-rich raffinate after extraction industry with the drug to the feed back step in a continuous distillation.
  3. 3、 根据权利要求2所述的一种煤焦油洗油生产工业芴的工艺方法,其特征在于,分离工业芴后的脱晶母液,通过冷却、结晶、压榨法去除作为滤液的非芴有机物,滤渣加热熔融得到富芴残油,该富芴残油回配到连续蒸馏工序的原料中,或直接作为一股进料送入蒸馏塔。 3. A coal tar according to claim 2 fluorene process for the production of oil washing, characterized in that the separating off the mother liquor after crystallization fluorene, fluorene remove non-organic material as filtrate by cooling, crystallization, compression, heating and melting resulting fluorene residue rich residual oil, the residual oil rich fluorenyl ligand to feed back the continuous distillation step, or directly as feed to a distillation column surge.
  4. 4、 根据权利要求2所述的一种煤焦油洗油生产工业芴的工艺方法,其特征在于,蒸馏工段切取的芴馏分用醇类溶剂将芴馏分通过醇类萃取脱除芴馏分中的非芴有机物,洗涤后的富芴馏分相用溶剂结晶或冷却结晶、离心分离的方法生产工业芴,离心分离后的脱晶母液采用蒸馏等方法脱除溶剂,其后得到的富芴残油回配到连续蒸馏工序的原料中,或直接作为一股进料送入蒸馏塔。 4, according to claim 2, wherein the coal tar oil process for the production of industrial washing fluorene, wherein the distillation section cut fraction with a fluorene fluorene fraction of non-alcoholic solvent is extracted by removing the alcohol fraction fluorene organic fluorene, fluorene-rich fraction after the washing solvent crystallization or cooling crystallization, centrifugal separation method of producing fluorene, after the mother liquid crystal centrifuged off using a method such as distillation removal of the solvent phase was subsequently obtained residual oil rich fluorenyl back with a continuous feed to the distillation step, or as a direct feed to an distillation column.
  5. 5、 用于权利要求1所述的一种煤焦油洗油生产工业芴的工艺方法的装置,其特征是连续蒸馏塔采用具有前塔和芴塔的两塔式,或采用一塔式。 5. A coal tar according to claim 1 for the oil producing apparatus process for washing fluorene, characterized in that the continuous distillation column having a two-tower front and tower fluorene column, or using a tower.
  6. 6、 根据权利要求5所述用的一种煤焦油洗油生产工业芴的工艺方法的装置,其特征在于,所述的蒸馏塔采用填料塔或板式蒸馏塔,或填料与板式相结合的精馏塔。 6, with coal tar as claimed in claim 5, wherein the device process for the production of oil washing fluorene, wherein said distillation column using a packed column or plate distillation columns, or a combination of filler and fine plate distillation tower.
CN 200810012775 2008-08-08 2008-08-08 Process for producing industrial fluorene by coal tar wash oil CN101643380B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
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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

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CN1027544C (en) 1992-10-31 1995-02-01 鞍山钢铁公司 Process for extracting naphthalene fraction, methyl naphthalene fraction and industrial acenaphthene from coal-tar oil washing oil and reducing energy consumption
CN1208727A (en) 1997-08-14 1999-02-24 攀钢集团煤化工公司 Continuous rectifying tech for crude naphthalene fraction from coke prond. plant

Cited By (9)

* Cited by examiner, † Cited by third party
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 heavy fluorene refined purification New 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

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