CN1651367A - Method of extracting high purity acenaphthene from coat tar scrubbing oil - Google Patents
Method of extracting high purity acenaphthene from coat tar scrubbing oil Download PDFInfo
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- CN1651367A CN1651367A CN 200410044103 CN200410044103A CN1651367A CN 1651367 A CN1651367 A CN 1651367A CN 200410044103 CN200410044103 CN 200410044103 CN 200410044103 A CN200410044103 A CN 200410044103A CN 1651367 A CN1651367 A CN 1651367A
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Abstract
A process for extracting high-purity acenaphthene from the washing oil of tar includes such steps as single-tower vacuum rectifying to obtain acenaphthene fraction at 235-245 deg.C mixing it with organic solvent, and recrystallizing. Its purity is more than 99%.
Description
Technical field
The present invention relates to a kind of method of from coal tar wash oil, extracting the high purity acenaphthene in coal deep processing field.
Background technology
Acenaphthene is one of main component in the coal tar, accounts for 1.2%～1.8% in coal tar, and content belongs to the 3rd in washing oil, reaches 10.32%, and being is worth the kind of exploitation energetically.Acenaphthene is to separate in the coal tar wash oil and utilization product the earliest, and product processed is also many, is mainly used in synthetic dyestuff, particularly Gao Dang organic dye, bakelite, coating, synthetic resins, engineering plastics, rubber antioxidant etc.
At present, the currently known methods that extracts industrial acenaphthylene both at home and abroad from washing oil has aromatic hydrocarbon solvent crystallization process and high pressure crystal method, but there is the low and equipment complexity of the acenaphthene product content that is obtained respectively in its shortcoming, makes problems such as production cost height and organic solvent contaminate environment; And factories such as steel coke-oven plant, Anshan iron and steel plant are climbed by the domestic unit that utilizes the NAPTHALENE FLAKES. (INDUSTRIAL GRADE device to extract acenaphthene from washing oil, it adopts rectifying complete processings such as " twin furnace double tower " equipment or " three stoves, three towers " equipment, the acenaphthene product content that this method obtained is also very low, about 94%～96%, limited its exploitation in derived product.Can consult " utilizing the NAPTHALENE FLAKES. (INDUSTRIAL GRADE device from washing oil, to extract industrial acenaphthylene " " fuel and chemical industry ", 1989 the 2nd phases, Hu Dongsheng.
The application for a patent for invention " process for preparation of pure acenaphthene by gradually heating emulsification crystallization " of the Shu Ge of Beijing Coal Chemistry Inst., Coal Sciences General Inst. equality, application number is 97122009.3.The shortcoming of this processing method is that technological process is longer, need to use negatively charged ion, positively charged ion, both sexes, nonionogenic tenside and special emulsifying device, production process produces a large amount of waste water, as not handled, will certainly cause environmental pollution, in addition, to the acenaphthene content requirement of raw material acenaphthene cut higher (more than 79%).
Summary of the invention
The present invention proposes a kind of method of extracting the high purity acenaphthene from coal tar wash oil, it is characterized in that with the coal tar wash oil being raw material, the content of acenaphthene is 8%～15% in the washing oil, adopt single tower rectification under vacuum technology, use stuffing rectification column, filler is a stainless steel ripple filler, or stainless steel triangle filler, the theoretical plate number of packing tower is 45～60, the rectification under vacuum pressure-controlling is at 0.05～0.06MPa, control of reflux ratio is 10～20,235～245 ℃ of the extraction temperature of acenaphthene cut, the cut of acquisition acenaphthene content 65%～75% is a raw material with this cut, mix with organic solvent, the mass ratio of solvent and acenaphthene cut is 1～1.5: 1, and the solvent that is fit to comprises dehydrated alcohol or ethyl acetate etc., and mixture heating up to crystallization is all dissolved, slowly cool to 25～35 ℃ again, crystallization is separated out, and crystallization time 20～50min filters, obtain acenaphthene purity and reach product more than 99%, the mother liquor recycling use after the filtration.
The invention has the advantages that and adopt single tower rectification under vacuum technology, the extraction temperature is lower than atmospheric distillation technology, and energy expenditure is low, reduces the use of equipment, the rate of recovery height of acenaphthene cut; Adopt solvent extraction technology, preparation technology is simple, and is easy to operate, and solvent can be recycled, and energy consumption is low, product acenaphthene yield and content height, and production cost is low, can not produce problems such as contaminate environment.
Embodiment
For the effect of technology of the present invention is described better, be illustrated with specific examples below.Raw material washing oil, thick acenaphthene and dry back product acenaphthene adopt gas-chromatography to carry out content analysis.
Embodiment 1
The rectification under vacuum device is rectifying tower φ 30 * 1600mm, stainless steel triangle filler, 53 of stage number, still kettle is the 500ml there-necked flask, 400g coal tar wash oil (acenaphthene content 10.32%) is joined in the there-necked flask, and being evacuated to pressure is 0.053MPa, begins to be heated to backflow, after waiting to stablize 1～2h, beginning extraction cut, reflux ratio is 15, when recovered temperature reaches 235 ℃, begin to collect the acenaphthene cut, when temperature reaches 245 ℃, stop extraction, obtain the yellow acenaphthene crystallization of 52.0g, acenaphthene content 68.75%, acenaphthene yield 86.60% (is benchmark with acenaphthene in the raw material washing oil).
Get crystallization acenaphthene cut 10g, join in the 15ml dehydrated alcohol, be heated to the crystallization dissolving, slowly cool to 30 ℃ then, crystallization is separated out, and filters, with the crystallization of 5ml absolute ethanol washing, drying obtains high-purity acenaphthene product of 6.6g acenaphthene content 99.15%, acenaphthene yield 95.18%.
Embodiment 2
Other condition is constant, gets the 10ml ethyl acetate, behind the recrystallization, with 5ml ethyl acetate wash crystallization, drying, obtains the acenaphthene product of 5.8g acenaphthene content 99.03%, acenaphthene yield 83.55%.
Find out that from the foregoing description the advantage of utilizing this method to extract acenaphthene is that energy consumption is low, technology is simple, the rate of recovery height of acenaphthene cut, and the product content height, non-environmental-pollution reduces production cost.
Claims (4)
1. method of from coal tar wash oil, extracting the high purity acenaphthene, it is characterized in that with the coal tar wash oil being raw material, adopt single tower rectification under vacuum technology, use stuffing rectification column, theoretical plate number is 45～60, and the rectification under vacuum pressure-controlling is at 0.05～0.06MPa, control of reflux ratio is 10～20,235～245 ℃ of the extraction temperature of acenaphthene cut, the cut of acquisition acenaphthene content 65%～75% is a raw material with this cut, mix with organic solvent, mixture heating up to crystallization is all dissolved, slowly cool to 25～35 ℃ again, crystallization is separated out, crystallization time 20～50min, filter, obtain acenaphthene purity and reach product more than 99%, the mother liquor recycling use after the filtration.
2. the method for extracting the high purity acenaphthene from coal tar wash oil according to claim 1, the content that it is characterized in that acenaphthene in the raw material washing oil is 8%～15%.
3. the method for extracting the high purity acenaphthene from coal tar wash oil according to claim 1 is characterized in that described packing tower filler is a stainless steel ripple filler, or stainless steel triangle filler.
4. the method for extracting the high purity acenaphthene from coal tar wash oil according to claim 1 is characterized in that described organic solvent comprises dehydrated alcohol or ethyl acetate, dehydrated alcohol preferably, and the mass ratio of solvent and acenaphthene cut is 1～1.5: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100441034A CN100336788C (en) | 2004-12-07 | 2004-12-07 | Method of extracting high purity acenaphthene from coat tar scrubbing oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100441034A CN100336788C (en) | 2004-12-07 | 2004-12-07 | Method of extracting high purity acenaphthene from coat tar scrubbing oil |
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| CN1651367A true CN1651367A (en) | 2005-08-10 |
| CN100336788C CN100336788C (en) | 2007-09-12 |
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| CNB2004100441034A Expired - Fee Related CN100336788C (en) | 2004-12-07 | 2004-12-07 | Method of extracting high purity acenaphthene from coat tar scrubbing oil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100473631C (en) * | 2006-03-29 | 2009-04-01 | 宝山钢铁股份有限公司 | Process for purifying biphenyl |
| CN101182277B (en) * | 2007-12-14 | 2010-04-14 | 鞍钢股份有限公司 | Method for extracting biphenyl from middle washing oil |
| CN102267858A (en) * | 2010-06-03 | 2011-12-07 | 鞍钢集团工程技术有限公司 | Method and apparatus for producing industrial acenaphthene from wash oil of coal tar |
| CN101665402B (en) * | 2008-09-01 | 2013-03-13 | 鞍钢股份有限公司 | Method for preparing refined fluorene |
| CN109438164A (en) * | 2018-12-06 | 2019-03-08 | 南京师范大学 | The device and method for extracting acenaphthene and acenaphthylene in LCO double ring arene |
| 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2606256B2 (en) * | 1988-02-24 | 1997-04-30 | 日本鋼管株式会社 | Method for producing acenaphthene |
| JP2560397B2 (en) * | 1988-03-08 | 1996-12-04 | 日本鋼管株式会社 | Process for producing acenaphthene, dibenzofuran and fluorene |
| 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 |
| CN1062292C (en) * | 1997-12-15 | 2001-02-21 | 煤炭科学研究总院北京煤化学研究所 | Process for preparation of pure acenaphthene by gradually heating emulsification crystallization |
-
2004
- 2004-12-07 CN CNB2004100441034A patent/CN100336788C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100473631C (en) * | 2006-03-29 | 2009-04-01 | 宝山钢铁股份有限公司 | Process for purifying biphenyl |
| CN101182277B (en) * | 2007-12-14 | 2010-04-14 | 鞍钢股份有限公司 | Method for extracting biphenyl from middle washing oil |
| CN101665402B (en) * | 2008-09-01 | 2013-03-13 | 鞍钢股份有限公司 | Method for preparing refined fluorene |
| CN102267858A (en) * | 2010-06-03 | 2011-12-07 | 鞍钢集团工程技术有限公司 | Method and apparatus for producing industrial acenaphthene from wash oil of coal tar |
| CN109438164A (en) * | 2018-12-06 | 2019-03-08 | 南京师范大学 | The device and method for extracting acenaphthene and acenaphthylene in LCO double ring arene |
| 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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| Publication number | Publication date |
|---|---|
| CN100336788C (en) | 2007-09-12 |
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