CN1121103A - Method of refining anthracene, phenanthrene and carbazole - Google Patents
Method of refining anthracene, phenanthrene and carbazole Download PDFInfo
- Publication number
- CN1121103A CN1121103A CN 94116941 CN94116941A CN1121103A CN 1121103 A CN1121103 A CN 1121103A CN 94116941 CN94116941 CN 94116941 CN 94116941 A CN94116941 A CN 94116941A CN 1121103 A CN1121103 A CN 1121103A
- Authority
- CN
- China
- Prior art keywords
- anthracene
- carbazole
- solvent
- milliliters
- phenanthrene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
In the present invention, anthracene phenanthrene and carbazole in crude coal tar anthracene or anthracene sludge is refined through mixed solvent extraction and precipitation process. Anthracene material is mixed with solvent mixture of strong polar solvent, non-polar solvent and alcohol, heated to dissolve, mixed with precipitant and filtered and washed to obtain refined anthracene. The filtrate is mixed with precipitant to obtain crude carbazole, which is washed with non-polar solvent, filtered to obtain filtrate and filter cake. The filterate is vacuum distilled and washed with alcohol to obtain pure phenanthrene, and refined carbazole is obtained through dissolution, preipitation, filteration, re-precipitation and re-filteration of the filter cake.
Description
The present invention relates to a kind of method of in coal tar crude anthracene or anthracene slag, extracting anthracene, phenanthrene and carbazole, extract the method for high-load anthracene, phenanthrene and carbazole especially continuously.
Crude anthracene processing is both at home and abroad at present produced anthracene, carbazole and luxuriant and rich with fragrance method and can roughly be divided into following several:
1) crude anthracene is to the material component method of recrystallization the solvent selectively;
2) method that recrystallization combines with still-process from solvent;
3) chemical process---use two kinds of immiscible solvents to carry out the liquid-phase extraction method;
4) integrated processes-recrystallization-distillation-recrystallization method;
5) liquid-phase extraction method in extraction tower.
The problem that above method exists is:
1) operation steps is many, and product content is not high.Product color is not pure, can not realize direct refined product;
2) separation efficiency is not high, equipment dynamic consumption is big;
3) investment is high, and waste residue can not be eliminated fully.
Reference:
1.[Soviet Union] Т. Я. Г о г о π e в а coal tar fraction processing (publishing in instalments)
" external coking chemistry " the 6th phase in 1989
2.[Soviet Union] Т. Я. Г о г о π e в а coal tar fraction processing (publishing in instalments)
" external coking chemistry " the 1st phase of nineteen ninety
The objective of the invention is to provide a kind of with the mixed extractant solvent precipitator method continuous method of extracting high-load anthracene, phenanthrene and carbazole from coal tar, this method separation efficiency height can be realized coproduction, and raw material is fully utilized.
The object of the present invention is achieved like this: anthracene slag and mixed solvent are mixed in proportion.Anthracene slag/solvent is/100～150 milliliters of 50～100 grams, intensive polar solvent has DMF in the mixed solvent, DMAC, N-MNP, N-MM, non-polar solvent has light oil or heavy aromatics, as benzene, toluene, dimethylbenzene etc., the volume ratio of intensive polar solvent/non-polar solvent is 10～40/0～50, also contain other solvent such as ethanol in the mixed solvent, acetone, butanols etc., consumption is 30～70% of whole solvent volume, after in temperature is 30 ℃～75 ℃ scopes, dissolving, add precipitation agent, precipitation agent can be water or straight-chain paraffin, preferably deionized water, consumption accounts for 5～20% of total liquor capacity, at this moment, solution is suspension, filters to obtain crude anthracene and filtrate, filtrate processes in addition, contain a large amount of anthracenes in the crude anthracene, a spot of carbazole and phenanthrene with aqueous intensive polar solvent washing secondary, obtain crude anthracene＞95% anthracene, / 80～180 milliliters of crude anthracene and water-containing solvent ratio 100 grams, the water yield is 2～35 milliliters in 100 milliliters of water-containing solvents.
The filtrate that the recovery crude anthracene obtains further adds precipitation agent, obtains thick carbazole precipitation, and it contains a large amount of carbazoles, phenanthrene and a spot of anthracene.
With the thick carbazole of 100 grams with 80～180 milliliters of non-polar solvents such as light oil, heavy aromatics, benzene,toluene,xylene etc. soak, washing, remove phenanthrene, filtration contains a large amount of phenanthrene in the filtrate, through underpressure distillation, washing with alcohol, can obtain＞98% pure phenanthrene.
The filter cake that washing by soaking is produced by 100 gram filter cakes with the mixed solvent of 80～180 milliliters of intensive polar solvents and ethanol volume ratio 1～4/9～6 30 ℃～75 ℃ dissolvings, press whole soln volume 5～20% and add precipitation agent, the anthracene that contains in the solution all is precipitated out, filter, filter cake is an anthracene, filtrate pouring into contained in the container of precipitation agent, and carbazole is precipitated to come out, and filters to obtain＞95% white carbazole.
The present invention is owing to adopted the mixed extractant solvent precipitator method, and its advantage is as follows:
1. this method is the physical operations process, no chemical reaction, and the operational cycle is short, output is big, good product quality.
2. anthracene, phenanthrene and carbazole coproduction, the separation efficiency height is fully utilized raw material, reduces waste residue.
3. isolated anthracene, phenanthrene and carbazole content height, anthracene are that yellow-green colour, carbazole and phenanthrene are white.
Principle used in the present invention is: utilize the physical properties of anthracene, phenanthrene and carbazole, promptly the solubleness in different solvents and the sequencing of separating out in mixed solvent reach the purified purpose.
The concrete steps of extracting high-content anthracene, phenanthrene and carbazole coproduction novel method from coal tar that propose according to the present invention are as follows:
Embodiment 1. in three mouthfuls of round-bottomed flasks of agitator, reflux condensing tube and thermometer are housed, pack into 75 gram anthracene slags, 35 milliliters of DMF, 50 milliliters of ethanol and 25 milliliters of heavy aromaticss, put into water-bath, stirring is warming up to 70 ℃, kept 20 minutes, and added 7 milliliters of 70 ℃ of hot water, stirred 10 minutes, slowly be cooled to 45 ℃, filter, filter cake is a crude anthracene, and filtrate is for 1..Crude anthracene is added 20 milliliters in DMF80 milliliter, water at normal temperatures, and washing and filtering obtains the anthracene product, and content is greater than 95%.1. filtrate poured in 70 ml waters, filter, filter cake is thick carbazole, with 100 milliliters of heavy aromatics normal temperature washings 30 minutes, filtration, obtains filter cake for 2..With the mother liquor distillation, solvent recuperation is reused, and residue is luxuriant and rich with fragrance slag, uses dissolve with ethanol, and the water precipitation after-filtration is led refining luxuriant and rich with fragrance.2. filter cake is added 30 milliliters of DMF, 40 milliliters of ethanol, in 70 ℃ of dissolvings, add 3 ml waters, cool to 45 ℃, filter, filter cake is a small amount of anthracene.Filtrate is directly poured in the suction lottle that 70 ml waters are housed, obtain white precipitate, sedimentation and filtration obtains white carbazole, and content is greater than 95%.
Embodiment 2. puts into flask with 75 gram anthracene slags, 15 milliliters of N-MNP, 60 milliliters of ethanol, 35 milliliters of heavy aromaticss, step such as embodiment 1, different is: with filter cake 2. add 10 milliliters of N-MNP, 60 milliliters of ethanol get final product in 70 ℃ of dissolvings.
Claims (2)
1. refined anthracene, the novel method of phenanthrene and carbazole, it is characterized in that: anthracene slag and mixed solvent are mixed in proportion, anthracene slag and solvent are/100～150 milliliters of 50～100 grams, intensive polar solvent is arranged (as DMF in the mixed solvent, DMAC, N-MNP, N-MM), non-polar solvent (light oil or heavy aromatics, as benzene, toluene, dimethylbenzene), the volume ratio of intensive polar solvent and non-polar solvent is 10～40/0～50, also contain ethanol in the mixed solvent, acetone, butanols, consumption is 30～70% of whole solvent volume, after in temperature is 30 ℃～75 ℃ scopes, dissolving, add precipitation agent, precipitation agent is water or straight-chain paraffin, consumption accounts for 5～20% of total liquor capacity, filtration obtains crude anthracene and filtrate, and crude anthracene with aqueous intensive polar solvent washing secondary, is obtained＞95% anthracene, / 80～180 milliliters of crude anthracene and water-containing solvent ratio 100 grams, the water yield is 2～35 milliliters in 100 milliliters of water-containing solvents;
The filtrate that the recovery crude anthracene is obtained further adds precipitation agent, obtains thick carbazole precipitation;
With the thick carbazole of 100 grams with 80～180 milliliters of non-polar solvents (as light oil, heavy aromatics, benzene,toluene,xylene) soak, washing, remove phenanthrene, filtration, filtrate is through underpressure distillation, washing with alcohol, obtains＞98% pure phenanthrene;
The filter cake that washing by soaking is produced by 100 gram filter cakes with the mixed solvent of 80～180 milliliters of intensive polar solvents and ethanol volume ratio 1-4/9-6 30 ℃～75 ℃ dissolvings, press whole soln volume 5～20% and add precipitation agent, filter, filter cake is an anthracene, filtrate pouring into contained in the container of precipitation agent, carbazole is precipitated to come out, and filters to obtain＞95% white carbazole.
2. the novel method of a kind of refined anthracene as claimed in claim 1, phenanthrene and carbazole, it is characterized in that: precipitation agent is deionized water preferably.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94116941 CN1121103A (en) | 1994-10-18 | 1994-10-18 | Method of refining anthracene, phenanthrene and carbazole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94116941 CN1121103A (en) | 1994-10-18 | 1994-10-18 | Method of refining anthracene, phenanthrene and carbazole |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1121103A true CN1121103A (en) | 1996-04-24 |
Family
ID=5038166
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94116941 Pending CN1121103A (en) | 1994-10-18 | 1994-10-18 | Method of refining anthracene, phenanthrene and carbazole |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1121103A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061640C (en) * | 1997-09-19 | 2001-02-07 | 鞍山钢铁集团公司 | Method for preparing industrial phenanthrene |
| WO2001079387A3 (en) * | 2000-04-18 | 2002-01-17 | Exxonmobil Res & Eng Co | Method for isolating enriched source of conducting polymers precursors using monohydroxyl alcohol treating agent |
| WO2001079388A3 (en) * | 2000-04-18 | 2002-04-18 | Exxonmobil Res & Eng Co | Method for isolating enriched source of conducting polymers precursors |
| CN100575343C (en) * | 2006-08-24 | 2009-12-30 | 宝山钢铁股份有限公司 | Process for refining carbazole |
| CN102363608A (en) * | 2011-11-24 | 2012-02-29 | 太原理工大学 | Method for preparing carbazole |
| CN102746103A (en) * | 2012-07-13 | 2012-10-24 | 韩钊武 | Method for preparing refined anthracene by using coal tar as raw material |
| CN103204761A (en) * | 2013-04-27 | 2013-07-17 | 武汉科技大学 | Method for preparing refined anthracene from crude anthracene as raw material by coupling extraction with solventing-out crystallization |
| CN103880732A (en) * | 2014-03-05 | 2014-06-25 | 上海鸿道节能环保科技发展有限公司 | Refined anthracene and carbazole purification method |
| CN104311381A (en) * | 2014-11-17 | 2015-01-28 | 宁夏中远天宇科技有限公司 | Novel dissolving procedure of production technology of refined anthracene |
| CN115141077A (en) * | 2022-06-01 | 2022-10-04 | 太原理工大学 | Method for selectively separating anthracene from condensed ring aromatic compound |
-
1994
- 1994-10-18 CN CN 94116941 patent/CN1121103A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061640C (en) * | 1997-09-19 | 2001-02-07 | 鞍山钢铁集团公司 | Method for preparing industrial phenanthrene |
| WO2001079387A3 (en) * | 2000-04-18 | 2002-01-17 | Exxonmobil Res & Eng Co | Method for isolating enriched source of conducting polymers precursors using monohydroxyl alcohol treating agent |
| WO2001079388A3 (en) * | 2000-04-18 | 2002-04-18 | Exxonmobil Res & Eng Co | Method for isolating enriched source of conducting polymers precursors |
| US6642421B1 (en) | 2000-04-18 | 2003-11-04 | Exxonmobil Research And Engineering Company | Method for isolating enriched source of conducting polymers precursors |
| AU2001249290B2 (en) * | 2000-04-18 | 2005-01-20 | Exxonmobil Research And Engineering Company | Method for isolating enriched source of conducting polymers precursors |
| AU2001247583B2 (en) * | 2000-04-18 | 2005-01-20 | Exxonmobil Research And Engineering Company | Method for isolating enriched source of conducting polymers precursors using monohydroxyl alcohol treating agent |
| AU2001247583C1 (en) * | 2000-04-18 | 2005-07-07 | Exxonmobil Research And Engineering Company | Method for isolating enriched source of conducting polymers precursors using monohydroxyl alcohol treating agent |
| AU2001249290C1 (en) * | 2000-04-18 | 2005-07-14 | Exxonmobil Research And Engineering Company | Method for isolating enriched source of conducting polymers precursors |
| CN100575343C (en) * | 2006-08-24 | 2009-12-30 | 宝山钢铁股份有限公司 | Process for refining carbazole |
| CN102363608A (en) * | 2011-11-24 | 2012-02-29 | 太原理工大学 | Method for preparing carbazole |
| CN102363608B (en) * | 2011-11-24 | 2013-01-30 | 太原理工大学 | Method for preparing carbazole |
| CN102746103A (en) * | 2012-07-13 | 2012-10-24 | 韩钊武 | Method for preparing refined anthracene by using coal tar as raw material |
| CN103204761A (en) * | 2013-04-27 | 2013-07-17 | 武汉科技大学 | Method for preparing refined anthracene from crude anthracene as raw material by coupling extraction with solventing-out crystallization |
| CN103204761B (en) * | 2013-04-27 | 2015-01-07 | 武汉科技大学 | Method for preparing refined anthracene from crude anthracene as raw material by coupling extraction with solventing-out crystallization |
| CN103880732A (en) * | 2014-03-05 | 2014-06-25 | 上海鸿道节能环保科技发展有限公司 | Refined anthracene and carbazole purification method |
| CN103880732B (en) * | 2014-03-05 | 2016-06-08 | 上海鸿道节能环保科技发展有限公司 | A kind of method of purification of anthracene and carbazole |
| CN104311381A (en) * | 2014-11-17 | 2015-01-28 | 宁夏中远天宇科技有限公司 | Novel dissolving procedure of production technology of refined anthracene |
| CN115141077A (en) * | 2022-06-01 | 2022-10-04 | 太原理工大学 | Method for selectively separating anthracene from condensed ring aromatic compound |
| CN115141077B (en) * | 2022-06-01 | 2023-09-19 | 太原理工大学 | Method for selectively separating anthracene from condensed ring aromatic compound |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1233710C (en) | Method for recycling colvent utilized in producting polyphenylene sulfide | |
| CN1121103A (en) | Method of refining anthracene, phenanthrene and carbazole | |
| CN106929160B (en) | Method for refining vegetable oil wax | |
| CN111099990B (en) | Recycling method of long carbon chain dicarboxylic acid refined crystallization mother liquor | |
| CN108570558A (en) | The method that copper is recycled from organosilicon slag slurry | |
| CN1958596A (en) | Method for extracting cholesterol from lanoline | |
| KR100371759B1 (en) | Process for producing (meth)acrylic acid | |
| CN101182278B (en) | Method for purifying refined fluorene by crystallizing process | |
| CN102827681A (en) | Waste hydraulic oil regeneration technology | |
| CN1061420A (en) | A kind of process for recovery and regeneration of waste plastics | |
| US4482766A (en) | Production of fatty alcohol with recovery thereof from the hydrogenation catalyst | |
| EP0015116B1 (en) | Process for the production of fatty acid soaps from sludge by extraction and subsequent saponifying | |
| CN1050356C (en) | Process for preparing sodium (or potassium) L-ascorbate | |
| CN212315539U (en) | Recovery device of elemental sulfur in sulfur-containing hydrometallurgy slag | |
| CN1049688C (en) | Method for treatment of alpha, omega dibasic acid fermentation liquor | |
| JP2003292987A (en) | Process for upgradation and bleaching of crude rice bran wax | |
| CN1332145A (en) | Benzoic acid recovering process for terephthalic acid oxygenating residue | |
| US3931258A (en) | Recovery of sugar cane wax | |
| CN100575343C (en) | Process for refining carbazole | |
| CN1482064A (en) | Method of preparing anhydrous aluminium chloride | |
| CN112745214A (en) | Method for separating and purifying sodium formate from pentaerythritol mother liquor by adopting solid phase extraction-elution crystallization method | |
| CN1110329A (en) | Method for recovering extractant from interfacial flocculate produced during the extraction of copper by LIX | |
| JPH06200289A (en) | Method for purifying natural crude wax | |
| CN212128044U (en) | Brominated SBS refining system | |
| RU2185225C2 (en) | Method of separation of solution from solids for process products |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication |