CN102965135B - Purification method for coal tar maltha - Google Patents
Purification method for coal tar maltha Download PDFInfo
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- CN102965135B CN102965135B CN201210425287.3A CN201210425287A CN102965135B CN 102965135 B CN102965135 B CN 102965135B CN 201210425287 A CN201210425287 A CN 201210425287A CN 102965135 B CN102965135 B CN 102965135B
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Abstract
A purification method for coal tar maltha aims to save energy and improve grade of coal asphalt raw material. The method provided by the invention comprises the steps of: conducting rough machining on the coal tar, cutting coal tar pitch with a softening point of 30-40 DEG C, and sending into a bulkhead type coal tar pitch extraction column for extraction; respectively heating an aliphatic extraction solvent and an aromatic extraction solvent to 110-250 DEG C; taking 0.5-1 part of an aliphatic solvent and 3-5 parts of an aromatic solvent, and mixing the two into an extractant by a static mixer; thoroughly stirring and mixing the extractant and coal tar pitch by a proportion of 1:0.5-1.3 with the static mixer, and adding the mixture from the upper part of the bulkhead type coal tar pitch extraction column; discharging the sulfur nitrogen compound in coal tar pitch and combined with the extractant from bottom of the extraction column, so as to purify coal tar pitch by removal of sulfur compounds; and discharging the coal tar pitch from the middle part of the bulkhead type coal tar pitch extraction column.
Description
Technical field
The present invention relates to a kind of coal tar soft asphalt purifying method.
Background technology
Coal tar soft asphalt is the main raw material of producing needle coke, and the quality of needle coke, cost and raw material are in close relations.In existing needle coke production technique, coal tar soft asphalt all needs to carry out purifying treatment conventionally, and existing purification process mainly contains vacuum distilling separating technology, centrifugal separation process, polymerization modifying process etc.Although vacuum distilling separating technology technique is simple, raw material productive rate is low.Centrifugal separation process refining effect is general, can raw material productive rate moderate, but investment is large.And polymerization modifying process is to utilize vacuum flashing-polymeric kettle polycondensation upgrading to form, facility investment is many.At present, nippon and mitsubishi chemical industry company have adopted the needle coke production technique of solvent treatment → delayed coking → calcining, but because of technical some the reason scale of solvent treatment always little.Domestic many enterprises have also expanded the needle coke working system of solvent treatment → delayed coking → calcining on original technique basis, but see in quality, the needle coke quality product of producing is still unstable, not yet reaches the level requirement that Japanese enterprises is produced ultra-high power graphite electrode.
Summary of the invention
The present invention seeks to overcome the deficiency of above-mentioned existing solvent treatment technology, the coal tar soft asphalt purifying method of a kind of effectively save energy, raising coal tar pitch raw material grade is provided.
The inventive method is:
(1) meet the coal tar of smelting mark YB/T5075-2010 standard, after the conventional means processing such as a tower normal decompression technique roughing, cut softening temperature and be the coal-tar pitch of 30-40 ℃, this coal-tar pitch is sent into partition wall type coal-tar pitch extraction tower by the reciprocation pump of the resistance to viscosity of heatproof;
(2) by reboiler, aliphatics, aromatic series extraction solvent are heated to respectively to 110-250 ℃.
Described aliphatics extraction solvent refers to any one or several arbitrary proportion mixture in the fatty compoundss such as kerosene, solar oil, 280# solvent oil, N-methylacetamide, N-Methyl pyrrolidone;
Described aromatic series extraction solvent refers to containing any one or several arbitrary proportion mixture in the aromatics such as the naphtalene oil of dibenzofuran, carbazole, benzo-thiophene, washing oil, carbolineum;
(3) according to weight unit part, get respectively 0.5~1 part of aliphatics extraction solvent and through static mixer, be mixed into extraction agent with 3~5 parts of aromatic series extraction solvents.
(4) by extraction agent and the weight ratio of coal-tar pitch, be that mix with coal-tar pitch extraction agent 1:0.5~1.3 through static mixer, after being fully uniformly mixed, from partition wall type coal-tar pitch extraction tower top, add; The compounds such as the sulphur nitrogen in coal-tar pitch are discharged after being combined with extraction agent at the bottom of extraction tower, and the coal-tar pitch removing after the compounds such as sulphur nitrogen is purified, and from partition wall type coal-tar pitch extraction tower middle part, discharge.
The refining coal pitch of making according to above-mentioned steps can be used for producing coal-based needle coke product.
The present invention directly sends into heated bitumen partition wall type coal-tar pitch extraction tower, and it has desulfurization, denitrogenation, de-quinoline insolubles, removes heavy metal a small amount of in pitch, and as vanadium, lead, aluminium, sodium etc., and molecule cutting reduces the effect of coal-tar pitch studies on asphaltene content.By coal tar fractional distillation and coal-tar pitch purify in conjunction with, effectively save energy, raising coal tar pitch raw material grade; Heated bitumen after coal tar fractional distillation lateral line discharging at the bottom of secondary tower is directly sent into partition wall type coal-tar pitch extraction tower, and its advantage is in a tower, to complete extraction and separated from solvent.By boiling range, density phase-splitting, can obtain needle coke and greying dipping agent bitumen, contribute to simplify coal-tar pitch cooling forming, reheat and dissolve purification process etc.; When aromatic solvent dissolves after coal-tar pitch, utilize in aliphatics ketone group, amido, sulphur carbon back and coal-tar pitch aromatic heterocycle as the affinity of dibenzofuran, carbazole, benzo-thiophene, by azeotropic extraction, dibenzofuran, carbazole, benzo-thiophene etc. are separated with the coal-tar pitch of extracting phase at extraction phase with extraction agent, and then solvent recycle and reuse by distillation.
Embodiment
Equipment used static mixer of the present invention, partition wall type coal-tar pitch extraction tower and auxiliary facility, be universal or standard equipment.
Embodiment mono-: the implementation step of the inventive method is:
The coal tar that meets smelting mark YB/T5075-2010 standard, with after conventional means processing, cuts softening temperature and is the coal-tar pitch of 30-40 ℃, and this coal-tar pitch is sent into partition wall type coal-tar pitch extraction tower by the reciprocation pump of the resistance to viscosity of heatproof;
Technical grade N-methylacetamide and tar one tower are cut out to naphtalene oil and by reboiler, be heated to respectively 110-250 ℃.
Technical grade N-methylacetamide or tar one tower are cut out to naphtalene oil and according to weight ratio 1:5, through static mixer, be mixed into extraction agent.
Extraction agent is mixed through static mixer for 1:1 by weight with coal-tar pitch, after being fully uniformly mixed, from partition wall type coal-tar pitch extraction tower top, add; The compounds such as the sulphur nitrogen in coal-tar pitch are discharged after being combined with extraction agent at the bottom of extraction tower, and coal-tar pitch is purified after removing the compounds such as sulphur nitrogen, from partition wall type coal-tar pitch extraction tower middle part, discharge.
According to above-mentioned steps, purify later coal-tar pitch, quinoline insolubles content is less than 0.5%.It is the raw material of making senior carbon materials.
Embodiment bis-: the implementation step of the inventive method is:
The coal tar that meets smelting mark YB/T5075-2010 standard, with after normal pressure one tower process processing, cuts softening temperature and is the coal-tar pitch of 30-40 ℃, and this coal-tar pitch is sent into partition wall type coal-tar pitch extraction tower by the reciprocation pump of the resistance to viscosity of heatproof;
200# solvent oil and tar one tower are cut out to washing oil and by reboiler, be heated to respectively 110-250 ℃.
200# solvent oil or tar one tower are cut out to washing oil and according to weight ratio 1:5.5, through static mixer, be mixed into extraction agent.
Extraction agent is mixed through static mixer for 1:1.05 by weight with coal-tar pitch, after being fully uniformly mixed, from partition wall type coal-tar pitch extraction tower top, add; The compounds such as the sulphur nitrogen in coal-tar pitch are discharged after being combined with extraction agent at the bottom of extraction tower, and coal-tar pitch is purified after removing the compounds such as sulphur nitrogen, from partition wall type coal-tar pitch extraction tower middle part, discharge.
According to above-mentioned steps, purify later coal-tar pitch, quinoline insolubles content little with in 0.3%.It is the raw material of making senior carbon materials.
Claims (1)
1. a coal tar soft asphalt purifying method, is characterized in that:
(1) coal tar is after a tower normal decompression technique roughing, cut softening temperature and be the coal-tar pitch of 30-40 ℃, this coal-tar pitch is sent into partition wall type coal-tar pitch extraction tower by the reciprocation pump of the resistance to viscosity of heatproof and is extracted, and described coal tar meets smelting mark YB/T5075-2010 standard;
(2) by reboiler, aliphatics, aromatic series extraction solvent are heated to respectively to 110-250 ℃;
Described aliphatics extraction solvent refers to any one or several arbitrary proportion mixture in the fatty compoundss such as kerosene, solar oil, 280# solvent oil, N-methylacetamide, N-Methyl pyrrolidone;
Described aromatic series extraction solvent refers to containing any one or several arbitrary proportion mixture in the aromatics such as the naphtalene oil of dibenzofuran, carbazole, benzo-thiophene, washing oil, carbolineum;
(3) according to weight unit part, get respectively 3~5 parts of 0.5~1 part of aliphatics extraction solvent and aromatic series extraction solvents, through static mixer, be mixed into extraction agent;
(4) ratio that is 1:0.5~1.3 in the weight ratio of extraction agent and coal-tar pitch after static mixer is fully uniformly mixed, adds extraction agent and coal-tar pitch from partition wall type coal-tar pitch extraction tower top; Sulfur-nitrogen compound in coal-tar pitch is discharged from this extraction tower bottom after being combined with extraction agent, and coal-tar pitch is purified after removing sulfur-nitrogen compound, from partition wall type coal-tar pitch extraction tower middle part, discharges.
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CN104193063B (en) * | 2014-09-16 | 2016-01-27 | 王茜茜 | A kind of tar and waste water treatment unit preparing pitch |
CN105734723A (en) * | 2016-03-25 | 2016-07-06 | 山东瑞城宇航碳材料有限公司 | Method for manufacturing ultrahigh-modulus graphite fiber continuous filament from coal tar |
CN106753545A (en) * | 2016-12-08 | 2017-05-31 | 辽宁石油化工大学 | A kind of process of coal tar processing modification |
CN111218294B (en) * | 2018-11-27 | 2021-07-23 | 宝武炭材料科技有限公司 | Method for purifying quinoline insoluble coal-series asphalt with high softening point and high softening point |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101289625A (en) * | 2008-06-03 | 2008-10-22 | 山西宏特煤化工有限公司 | Production process of dipping agent bitumen |
CN101531909A (en) * | 2009-04-09 | 2009-09-16 | 中钢集团鞍山热能研究院有限公司 | Continuous sedimentation process for production of needle coke |
CN101824329A (en) * | 2010-05-17 | 2010-09-08 | 朱兴建 | Novel process for eliminating quinoline insoluble substances in coal tar medium temperature pitch |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101289625A (en) * | 2008-06-03 | 2008-10-22 | 山西宏特煤化工有限公司 | Production process of dipping agent bitumen |
CN101531909A (en) * | 2009-04-09 | 2009-09-16 | 中钢集团鞍山热能研究院有限公司 | Continuous sedimentation process for production of needle coke |
CN101824329A (en) * | 2010-05-17 | 2010-09-08 | 朱兴建 | Novel process for eliminating quinoline insoluble substances in coal tar medium temperature pitch |
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