CN101220284A - Method for producing electrode impregnation asphalt - Google Patents

Method for producing electrode impregnation asphalt Download PDF

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Publication number
CN101220284A
CN101220284A CNA200710158909XA CN200710158909A CN101220284A CN 101220284 A CN101220284 A CN 101220284A CN A200710158909X A CNA200710158909X A CN A200710158909XA CN 200710158909 A CN200710158909 A CN 200710158909A CN 101220284 A CN101220284 A CN 101220284A
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China
Prior art keywords
pitch
solvent
temperature
mid
heating
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CNA200710158909XA
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Chinese (zh)
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CN101220284B (en
Inventor
王萍
李健
王晓楠
姚君
马晨阳
宋亚楠
田晓露
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Angang Steel Co Ltd
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Angang Steel Co Ltd
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Publication of CN101220284B publication Critical patent/CN101220284B/en
Expired - Fee Related legal-status Critical Current
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Abstract

A preparation method of an electrode impregnation pitch adopts the medium temperature pitch as the raw material and the dephenollized phenol oil as the solvent which passes three processing steps of thermal dissolving, vacuum filtrating and solvent distillation recycling so as to remove the quinoline insoluble matter in the medium temperature pitch, thus leading the weight of quinoline insoluble matter to be less than 0.1 percent of the electrode impregnation pitch product. The yield of the electrode impregnation pitch of the invention can reach more than 80 percent. The used dephenollized phenol oil can be reused and the filter cake can be processed as the heavy asphalt. The whole process needs less equipment and less working procedure with easy control, simple technique and good effect. The invention has an effective method of processing the coal tar pitch can produce 4,000 tons of the electrode impregnation pitches, supposing with the annual process of 5,000 tons of the medium temperature pitch.

Description

A kind of preparation method of electrode impregnating pitch
Technical field
The invention belongs to coal chemical technology, relate in particular to a kind of method of utilizing mid-temperature pitch to produce the electrode impregnating pitch.
Background technology
The preparation method of electrode impregnating pitch has coal tar, viscid bitumen, mid-temperature pitch etc. by the raw materials for production branch.By the production method branch have that coal tar filtration method, coal-tar solvent extraction process, coal tar (viscid bitumen) hot polymerization are legal, coal-tar pitch solvent settling process, mid-temperature pitch solvent filter method.The key that adopts mid-temperature pitch to produce the production of electrode impregnating pitch is to remove quinoline insolubles content, remove quinoline insolubles method have following several.
Standing sedimentation separates: mainly rely on gravity settling to separate impurities.Present method characteristics are that investment is little, technology is simple, but decontamination effect improving is poor.
Centrifugation: use that supercentrifuge is centrifugal to remove primary quinoline insolubles, this appliance arrangement is huge, and metal is wasteful, the energy consumption height.
Thermosol filters: at first melt the material coarse filtration in still, the coarse filtration still is furnished with process furnace, pressurizing valve, blow-off valve; Adopt high-efficiency filtering material that the raw material of coarse filtration is entered smart filter still then and filter, this method good purification, technology is simple, but filter screen is required harsh.
Solvent extraction: carry out solvent extraction after adding solvent, this method investment is little, good purification, but solvent load is big, and yield is low.
The production of China's electrode impregnating pitch at present still is in the Development and Trial stage, and the method for producing the electrode impregnating pitch with mid-temperature pitch does not still realize industrialization.Therefore by retrieval, identical with the present invention or akin patent documentation of Shang Weijian and relevant document announcement.
Summary of the invention
The purpose of this invention is to provide a kind of reduced investment, instant effect, technology is simple, and the quinoline in the energy effective elimination mid-temperature pitch is not tolerant, thereby obtains the method for high-quality electrode impregnating pitch.
For this reason, the technical solution that the present invention taked is:
The preparation method of electrode impregnating pitch of the present invention, the employing mid-temperature pitch is a raw material, with the removal phenol carbolic oil is solvent, reclaims three processing removing the quinoline insolubles in the mid-temperature pitch through heating for dissolving, vacuum filtration, solvent distillation, thereby makes electrode impregnating pitch product.Its concrete operations step is:
1, heating for dissolving: mid-temperature pitch is mixed post-heating with the removal phenol carbolic oil solvent by 1: 2~5, keep solvent temperature between 70 ℃~110 ℃, and be continuously stirring to mid-temperature pitch and all be dissolved in the removal phenol carbolic oil solvent; Take little fire heating then, dissolve after 10~30 minutes, stop heating;
2, vacuum filtration: after hot mixing solutions at room temperature is cooled to 15~45 ℃, slowly pour in the funnel of mounted in advance vacuum filtration device, carry out vacuum filtration while pour into, the filtrate behind the suction filtration is poured in the Copper Pot;
3, the solvent distillation is reclaimed: the filtrate in the Copper Pot is distilled under the mode of decompression, distill whole temperature and remain on 160 ℃~230 ℃, distillate is solvent, and is reusable; The sample of pouring out at the bottom of the kettle of distillation back is the electrode impregnating pitch.And quinoline insolubles weight is less than 0.1% in the electrode impregnating pitch.
The beneficial effect of the preparation method of electrode impregnating pitch of the present invention is:
The one, recovery rate height, mid-temperature pitch are handled its electrode impregnating pitch productive rate of back and can be reached more than 80%; The 2nd, the utilization ratio height uses removal phenol carbolic oil solvent later all to reclaim and reuses, and the filter cake that is produced after filtering can be used as heavy bitumen and handles; The 3rd, the processing efficiency height, the whole process of production required equipment is few, and processing method is easy to grasp and control, and operation is few, and is effective; The 4th, comprehensive benefit is considerable, coal-tar pitch is an isolated bulk product in the coal tar course of processing, account for 50~60% of coal tar total amount, with 5000 tons of mid-temperature pitches of year processing, productive rate is 80% calculating, just can produce 4000 tons of electrode impregnating pitches every year, for an effective way has been found out in the processing of coal-tar pitch.
Embodiment
The invention will be further described below in conjunction with embodiment.
The preparation method of electrode impregnating pitch of the present invention, selecting mid-temperature pitch for use is raw material, with the removal phenol carbolic oil is solvent, reclaims three processing through heating for dissolving, vacuum filtration, solvent distillation, thereby produces quinoline insolubles weight less than 0.1% electrode impregnating pitch product.
Embodiment 1:
With mid-temperature pitch and removal phenol carbolic oil solvent mixed by 1: 2, after the mixing mixture is heated, and uninterrupted the stirring, keep solvent temperature at 110 ℃, mid-temperature pitch all is dissolved in the removal phenol carbolic oil solvent; Take little fire heating then, dissolve after 10 minutes, stop heating.
After hot mixing solutions at room temperature is cooled to 15 ℃, slowly pour in the funnel of mounted in advance vacuum filtration device, carry out vacuum filtration while pour into, the filtrate behind the suction filtration is poured in the Copper Pot.
Filtrate in the Copper Pot is distilled under the mode of decompression, and distilling whole temperature is 230 ℃.Distillate is the removal phenol carbolic oil solvent, reclaims so that reuse.The sample of pouring out at the bottom of the kettle of distillation back can obtain quinoline insolubles weight less than 0.1% electrode impregnating pitch.
Embodiment 2:
With mid-temperature pitch and removal phenol carbolic oil solvent mixed by 1: 5, after the mixing mixture is heated, and uninterrupted the stirring, keep solvent temperature at 70 ℃, mid-temperature pitch all is dissolved in the removal phenol carbolic oil solvent; Take little fire heating then, dissolve after 30 minutes, stop heating.
After hot mixing solutions at room temperature is cooled to 45 ℃, slowly pour in the funnel of mounted in advance vacuum filtration device, carry out vacuum filtration while pour into, the filtrate behind the suction filtration is poured in the Copper Pot.
Filtrate in the Copper Pot is distilled under the mode of decompression, and distilling whole temperature is 160 ℃.Distillate is the removal phenol carbolic oil solvent, reclaims so that reuse.The sample of pouring out at the bottom of the kettle of distillation back can obtain quinoline insolubles weight less than 0.1% electrode impregnating pitch.

Claims (2)

1. the preparation method of an electrode impregnating pitch, the employing mid-temperature pitch is a raw material, it is characterized in that, and with the removal phenol carbolic oil solvent, reclaim three processing removing the quinoline insolubles in the mid-temperature pitch through heating for dissolving, vacuum filtration, solvent distillation, thereby make electrode impregnating pitch product; Its concrete operations step is:
(1), heating for dissolving: mid-temperature pitch is mixed post-heating with the removal phenol carbolic oil solvent by 1: 2~5, keep solvent temperature between 70 ℃~110 ℃, and be continuously stirring to mid-temperature pitch and all be dissolved in the removal phenol carbolic oil solvent; Take little fire heating then, dissolve after 10~30 minutes, stop heating;
(2), vacuum filtration: after hot mixing solutions at room temperature is cooled to 15~45 ℃, slowly pour in the funnel of mounted in advance vacuum filtration device, carry out vacuum filtration while pour into, the filtrate behind the suction filtration is poured in the Copper Pot;
(3), the solvent distillation is reclaimed: the filtrate in the Copper Pot is distilled under the mode of decompression, distill whole temperature and remain on 160 ℃~230 ℃, distillate is solvent, and is reusable; The sample of pouring out at the bottom of the kettle of distillation back is the electrode impregnating pitch.
2. the preparation method of electrode impregnating pitch according to claim 1 is characterized in that, quinoline insolubles weight is less than 0.1% in the described electrode impregnating pitch.
CN200710158909XA 2007-12-14 2007-12-14 Method for producing electrode impregnation asphalt Expired - Fee Related CN101220284B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN200710158909XA CN101220284B (en) 2007-12-14 2007-12-14 Method for producing electrode impregnation asphalt

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN200710158909XA CN101220284B (en) 2007-12-14 2007-12-14 Method for producing electrode impregnation asphalt

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CN101220284A true CN101220284A (en) 2008-07-16
CN101220284B CN101220284B (en) 2010-12-08

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101445740A (en) * 2009-01-04 2009-06-03 北京石油化工学院 A preparation method of dipping agent pitch
CN101787298A (en) * 2009-01-23 2010-07-28 北京石油化工学院 Coal art pitch purification method
CN101880542A (en) * 2010-06-24 2010-11-10 山西潞安环保能源开发股份有限公司 Method for removing organic sulfur in coal pitch
CN104031669A (en) * 2013-03-07 2014-09-10 神华集团有限责任公司 Electrode pitch and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101445740A (en) * 2009-01-04 2009-06-03 北京石油化工学院 A preparation method of dipping agent pitch
CN101787298A (en) * 2009-01-23 2010-07-28 北京石油化工学院 Coal art pitch purification method
CN101787298B (en) * 2009-01-23 2014-05-28 北京石油化工学院 Coal art pitch purification method
CN101880542A (en) * 2010-06-24 2010-11-10 山西潞安环保能源开发股份有限公司 Method for removing organic sulfur in coal pitch
CN101880542B (en) * 2010-06-24 2013-01-23 山西潞安环保能源开发股份有限公司 Method for removing organic sulfur in coal pitch
CN104031669A (en) * 2013-03-07 2014-09-10 神华集团有限责任公司 Electrode pitch and preparation method thereof

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