CN103173235A - Low-energy-consumption removal method of quinoline insolubles in asphalt - Google Patents
Low-energy-consumption removal method of quinoline insolubles in asphalt Download PDFInfo
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- CN103173235A CN103173235A CN2013101003873A CN201310100387A CN103173235A CN 103173235 A CN103173235 A CN 103173235A CN 2013101003873 A CN2013101003873 A CN 2013101003873A CN 201310100387 A CN201310100387 A CN 201310100387A CN 103173235 A CN103173235 A CN 103173235A
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- washing oil
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- quinoline insolubles
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Abstract
The invention discloses a low-energy-consumption removal method of quinoline insolubles in asphalt and belongs to the technical field of removal of quinoline insolubles in the asphalt. The low-energy-consumption removal method comprises the following steps of: preparing a flocculant solution containing ethylene glycol or propylene glycol, water and aluminium polychlorid, and an asphalt/gas absorber oil mixture solution, mixing the flocculant solution and the asphalt/gas absorber oil mixture solution, then carrying out centrifugal separation to extract a supernatant, and distilling the ethylene glycol, the propylene glycol and gas absorber oil from the supernatant to obtain refined asphalt. The low-energy-consumption removal method has the advantages and effects that: as a flocculating mechanism is adopted, the technological time spent in the process of removing the quinoline insolubles in the asphalt is saved in comparison with the traditional solvent sedimentation method, and therefore the energy consumption is reduced. The mass content of the quinoline insolubles in the refined asphalt treated by using the method is 0.3-0.6 percent.
Description
Technical field
The present invention relates to the less energy-consumption removal methods of quinoline insolubles in a kind of pitch, belong to the pitch quinoline insolubles and remove technical field.
Background technology
Quinoline insolubles in pitch is the carbon particles about a kind of 1 μ m, if its mass content in pitch surpasses 1%, will significantly reduce the mesophase pitch that uses pitch to go out as raw material production, the quality of needle coke, when therefore related products is produced, requirement must remove the quinoline insolubles in pitch, and its mass content is reduced to below 0.8%.The way of present industrial comparative maturity is to use single solvent or solvent pairs to mix settling process, the method removal effect is good, but need the long settling time (general 5 ~ 24h), because settling process need to be incubated operation, therefore need the external world that energy is provided, the long treatment time directly causes energy consumption to strengthen, and finally improves product cost.The present invention relates to the less energy-consumption removal methods of quinoline insolubles in pitch, the method utilizes the alcohol-water mixture molecule that will flocculate to introduce asphalt system, utilize flocculation mechanism significantly to dwindle the time that removes quinoline insolubles, thereby reduce energy consumption, improve the economic benefit of product.
Summary of the invention
The invention provides the less energy-consumption removal methods of quinoline insolubles in a kind of pitch, the method operating time is short, and energy consumption is low.
The present invention realized by the following technical programs, and the less energy-consumption removal methods of quinoline insolubles in a kind of pitch is characterized in that comprising following process:
(1) under room temperature, a kind of in polymerize aluminum chloride and deionized water and ethylene glycol and propylene glycol is in mass ratio (1 ~ 1.5): (7 ~ 15): after mix (55 ~ 100), through the stirring solution that obtains flocculating;
(2) adding quality in the pending pitch is the washing oil of 1.5 ~ 2.5 times, obtains pitch and washing oil mixed solution in a temperature 80-95 ℃ stirring;
(3) in the pitch and washing oil mixed solution of step (2) system, adding quality is the flocculation solution through step (1) system of 0.3 ~ 0.6 times of the asphalt quality in this pitch and washing oil mixed solution, obtain primary treatment liquid after stirring 0.5 ~ 1.5h under temperature 80-105 ℃ constant temperature, be centrifugal layering under 1500 ~ 2000r/min with this primary treatment liquid at rotating speed, collect upper strata liquid as secondary treatment liquid, collect lower floor and be enriched with the viscous fluid of quinoline insolubles as by product;
(4) with step (3) secondary treatment liquid distill out ethylene glycol or propylene glycol under normal pressure and temperature 190-205 ℃; Distill out washing oil again under temperature 280-300 ℃, reclaim ethylene glycol or propylene glycol and washing oil and recycle; The remaining substrate of distillation is refined asphaltic bitumen.
Advantage of the present invention and effect are as follows: present method is owing to adopting flocculation mechanism, and the conventional solvent of comparing settling process is saved the process time during quinoline insolubles in removing pitch, thereby reduced energy consumption.Refined asphaltic bitumen after present method is processed, its quinoline insolubles mass content is 0.3 ~ 0.6%.
Embodiment
Embodiment 1
(1) under room temperature with 100g polymerize aluminum chloride (solid, GB/T 22627-2008), after 1000g deionized water, 8000g ethylene glycol mix, stir 2 h, obtain the solution that flocculates;
(2) add 2000g washing oil (GB/T 24217-2009) in the pending pitch of 1000g (quinoline insolubles mass content 4.7%), be warming up to 95 ℃ after constant temperature obtain pitch/washing oil mixed solution after stirring 1h;
(3) add 600g flocculation solution in above-mentioned pitch/washing oil mixed solution, stir 1h under 105 ℃ of constant temperature and obtain primary treatment liquid, with the layering after centrifugal 45min under rotating speed 2000r/min of this treatment solution, the upper strata is secondary treatment liquid, lower floor is the black liquor that is enriched with quinoline insolubles of thickness, this liquid can be as the raw material of other field, as producing binding agent;
(4) secondary treatment liquid is distilled out ethylene glycol under 200-205 ℃, distill out washing oil under 280-300 ℃, ethylene glycol and washing oil are recycled, and the remaining substrate of distillation is the refined asphaltic bitumen after processing, and the refined asphaltic bitumen quality is 600g, quinoline insolubles content 0.3%.
Embodiment 2
(1) under room temperature with the 150g polymerize aluminum chloride, the 700g deionized water after the 5500g mixed with propylene glycol, stirs 2 h, obtains the solution that flocculates;
(2) add the 1500g washing oil in the pending pitch of 1000g, be warming up to 80 ℃ after constant temperature obtain pitch/washing oil mixed solution after stirring 1.5h;
(3) add 300g flocculation solution in above-mentioned pitch/washing oil mixed solution, stir 1.5h under 95 ℃ of constant temperature and obtain primary treatment liquid, with the layering after centrifugal 30min under rotating speed 2000r/min of this treatment solution, the upper strata is secondary treatment liquid, lower floor is the black liquor that is enriched with quinoline insolubles of thickness, this liquid can be as the raw material of other field, as producing binding agent;
(4) secondary treatment liquid is distilled out propylene glycol under 190-200 ℃, distill out washing oil under 280-300 ℃, propylene glycol and washing oil are recycled, and the remaining substrate of distillation is the refined asphaltic bitumen after processing, and the refined asphaltic bitumen quality is 700g, quinoline insolubles content 0.6%.
Embodiment 3
(1) under room temperature with the 100g polymerize aluminum chloride, the 1500g deionized water after the 10000g mixed with propylene glycol, stirs 2 h, obtains the solution that flocculates;
(2) add the 2500g washing oil in the pending pitch of 1000g, be warming up to 95 ℃ after constant temperature obtain pitch/washing oil mixed solution after stirring 1.5h;
(3) add 500g flocculation solution in above-mentioned pitch/washing oil mixed solution, stir 0.5h under 105 ℃ of constant temperature and obtain primary treatment liquid, with the layering after centrifugal 15min under rotating speed 1500r/min of this treatment solution, the upper strata is secondary treatment liquid, lower floor is the black liquor that is enriched with quinoline insolubles of thickness, this liquid can be as the raw material of other field, as producing binding agent;
(4) secondary treatment liquid is distilled out propylene glycol under 190-200 ℃, distill out washing oil under 280-300 ℃, propylene glycol and washing oil are recycled, and the remaining substrate of distillation is the refined asphaltic bitumen after processing, the refined asphaltic bitumen quality is 615g, quinoline insolubles content 0.4%.
Embodiment 4
(1) under room temperature with the 130g polymerize aluminum chloride, after 1200g deionized water, 7000g ethylene glycol mix, stir 2 h, obtain the solution that flocculates;
(2) add the 2000g washing oil in the pending pitch of 1000g, be warming up to 80 ℃ after constant temperature obtain pitch/washing oil mixed solution after stirring 1.5h;
(3) add 500g flocculation solution in above-mentioned pitch/washing oil mixed solution, stir 1h under 90 ℃ of constant temperature and obtain primary treatment liquid, with the layering after centrifugal 45min under rotating speed 2000r/min of this treatment solution, the upper strata is secondary treatment liquid, lower floor is the black liquor that is enriched with quinoline insolubles of thickness, this liquid can be as the raw material of other field, as producing binding agent;
(4) secondary treatment liquid is distilled out ethylene glycol under 200-205 ℃, distill out washing oil under 280-300 ℃, ethylene glycol and washing oil are recycled, and the remaining substrate of distillation is the refined asphaltic bitumen after processing, the refined asphaltic bitumen quality is 550g, quinoline insolubles content 0.3%.
Embodiment 5
(1) under room temperature with the 140g polymerize aluminum chloride, after 1100g deionized water, 5500g ethylene glycol mix, stir 2 h, obtain the solution that flocculates;
(2) add the 1700g washing oil in the pending pitch of 1000g, be warming up to 85 ℃ after constant temperature obtain pitch/washing oil mixed solution after stirring 1.5h;
(3) add 400g flocculation solution in above-mentioned pitch/washing oil mixed solution, stir 1h under 95 ℃ of constant temperature and obtain primary treatment liquid, with the layering after centrifugal 30min under rotating speed 1500r/min of this treatment solution, the upper strata is secondary treatment liquid, lower floor is the black liquor that is enriched with quinoline insolubles of thickness, this liquid can be as the raw material of other field, as producing binding agent;
(4) secondary treatment liquid is distilled out ethylene glycol under 200-205 ℃, distill out washing oil under 280-300 ℃, ethylene glycol and washing oil are recycled, and the remaining substrate of distillation is the refined asphaltic bitumen after processing, the refined asphaltic bitumen quality is 615g, quinoline insolubles content 0.4%.
Embodiment 6
(1) under room temperature with the 100g polymerize aluminum chloride, the 900g deionized water after the 6500g mixed with propylene glycol, stirs 2 h, obtains the solution that flocculates;
(2) add the 2000g washing oil in the pending pitch of 1000g, be warming up to 90 ℃ after constant temperature obtain pitch/washing oil mixed solution after stirring 1.5h;
(3) add 460g flocculation solution in above-mentioned pitch/washing oil mixed solution, stir 1.5h under 105 ℃ of constant temperature and obtain primary treatment liquid, with the layering after centrifugal 15min under rotating speed 2000r/min of this treatment solution, the upper strata is secondary treatment liquid, lower floor is the black liquor that is enriched with quinoline insolubles of thickness, this liquid can be as the raw material of other field, as producing binding agent;
(4) secondary treatment liquid is distilled out propylene glycol under 190-200 ℃, distill out washing oil under 280-300 ℃, propylene glycol and washing oil are recycled, and the remaining substrate of distillation is the refined asphaltic bitumen after processing, the refined asphaltic bitumen quality is 705g, quinoline insolubles content 0.6%.
Comparative example with embodiment 1:
(1) add 1300g washing oil (GB/T 24217-2009) and 1300g kerosene (GB 253-2008) in the pending pitch of 1000g (quinoline insolubles mass content 4.7%), after stirring 1h under 105 ℃, be warming up to 115 ℃ of standing 6h of constant temperature and obtain mixed solution;
(2) with mixed solution at normal pressure, 270-300 ℃ of lower Distillation recovery washing oil, kerosene, the distillation substrate is the refined asphaltic bitumen after processing, the refined asphaltic bitumen quality is 600g, quinoline insolubles content is 0.3%.
This comparative example's power consumption is apparently higher than embodiment 1.
Claims (1)
1. the less energy-consumption removal methods of quinoline insolubles in a pitch is characterized in that comprising following process:
(1) under room temperature, a kind of in polymerize aluminum chloride and deionized water and ethylene glycol and propylene glycol is in mass ratio (1 ~ 1.5): (7 ~ 15): after mix (55 ~ 100), through the stirring solution that obtains flocculating;
(2) adding quality in the pending pitch is the washing oil of 1.5 ~ 2.5 times, obtains pitch and washing oil mixed solution in a temperature 80-95 ℃ stirring;
(3) in the pitch and washing oil mixed solution of step (2) system, adding quality is the flocculation solution through step (1) system of 0.3 ~ 0.6 times of the asphalt quality in this pitch and washing oil mixed solution, obtain primary treatment liquid after stirring 0.5 ~ 1.5h under temperature 80-105 ℃ constant temperature, be centrifugal layering under 1500 ~ 2000r/min with this primary treatment liquid at rotating speed, collect upper strata liquid as secondary treatment liquid, collect lower floor and be enriched with the viscous fluid of quinoline insolubles as by product;
(4) with step (3) secondary treatment liquid distill out ethylene glycol or propylene glycol under normal pressure and temperature 190-205 ℃; Distill out washing oil again under temperature 280-300 ℃, reclaim ethylene glycol or propylene glycol and washing oil and recycle; The remaining substrate of distillation is refined asphaltic bitumen.
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| CN201310100387.3A CN103173235B (en) | 2013-03-27 | 2013-03-27 | Low-energy-consumption removal method of quinoline insolubles in asphalt |
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| CN201310100387.3A CN103173235B (en) | 2013-03-27 | 2013-03-27 | Low-energy-consumption removal method of quinoline insolubles in asphalt |
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| CN103173235B CN103173235B (en) | 2014-06-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110317624A (en) * | 2019-08-08 | 2019-10-11 | 平顶山东晟高科实业有限公司 | A kind of method of pitch removing QI |
Citations (5)
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|---|---|---|---|---|
| EP1130077A2 (en) * | 2000-03-01 | 2001-09-05 | Repsol Petroleo S.A. | Highly aromatic petroleum pitches, their preparation and use in the manufacture of electrodes |
| CA2428995A1 (en) * | 2003-05-16 | 2004-11-16 | Speros E. Moschopedis | Separation of asphaltenes from bitumen and heavy oils using a metal salt catalyst |
| CN101294089A (en) * | 2007-04-25 | 2008-10-29 | 淄博矿业集团有限责任公司 | Method for producing coal tar pitch |
| CN101787298A (en) * | 2009-01-23 | 2010-07-28 | 北京石油化工学院 | Coal art pitch purification method |
| CN101787299A (en) * | 2010-03-01 | 2010-07-28 | 上海尚元化工工程技术有限公司 | Method for extracting, producing and purifying pitch with mixed solvent |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1130077A2 (en) * | 2000-03-01 | 2001-09-05 | Repsol Petroleo S.A. | Highly aromatic petroleum pitches, their preparation and use in the manufacture of electrodes |
| CA2428995A1 (en) * | 2003-05-16 | 2004-11-16 | Speros E. Moschopedis | Separation of asphaltenes from bitumen and heavy oils using a metal salt catalyst |
| CN101294089A (en) * | 2007-04-25 | 2008-10-29 | 淄博矿业集团有限责任公司 | Method for producing coal tar pitch |
| CN101787298A (en) * | 2009-01-23 | 2010-07-28 | 北京石油化工学院 | Coal art pitch purification method |
| CN101787299A (en) * | 2010-03-01 | 2010-07-28 | 上海尚元化工工程技术有限公司 | Method for extracting, producing and purifying pitch with mixed solvent |
Non-Patent Citations (2)
| Title |
|---|
| 曾舟林等: "煤焦油中喹啉不溶物的分离方法", 《洁净煤技术》, vol. 18, no. 2, 25 April 2012 (2012-04-25), pages 56 - 59 * |
| 薛改凤等: "絮凝剂和溶剂对煤焦油净化效果", 《炭素技术》, no. 1, 28 February 1997 (1997-02-28), pages 17 - 20 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110317624A (en) * | 2019-08-08 | 2019-10-11 | 平顶山东晟高科实业有限公司 | A kind of method of pitch removing QI |
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