CN103865556B - Device and method for producing mesophase-free medium-temperature modified asphalt - Google Patents
Device and method for producing mesophase-free medium-temperature modified asphalt Download PDFInfo
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- CN103865556B CN103865556B CN201210545373.8A CN201210545373A CN103865556B CN 103865556 B CN103865556 B CN 103865556B CN 201210545373 A CN201210545373 A CN 201210545373A CN 103865556 B CN103865556 B CN 103865556B
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Abstract
The invention discloses a mesophase-free medium-temperature modified asphalt production device, which comprises a secondary evaporator/main tower and reaction kettles connected with the secondary evaporator/main tower, wherein the secondary evaporator/main tower is connected with a plurality of normal-pressure reaction kettles connected in series through a gravity flow or a conveying pump; a stirrer is arranged in each reaction kettle, and a heating device is arranged beside each reaction kettle; the upper part of the reaction kettle is connected with an immersed cooler, the immersed cooler is connected with a gas-liquid separator, and the lower part of the gas-liquid separator is connected with a flash oil tank; the lower part of the reaction kettle is connected with an asphalt intermediate tank. The invention also provides a production method of the mesophase-free warm-modified asphalt, and the mesophase-free warm-modified asphalt is obtained by setting necessary control indexes. The medium-temperature modified asphalt without mesophase is obtained by reasonably setting commercial production devices and controlling the quality index of the medium-temperature asphalt, the medium-temperature asphalt is subjected to mild reaction at low temperature and normal pressure without blending flash oil, oil gas generated by the reaction is effectively recycled, and the effect of saving resources and energy is achieved.
Description
Technical field
The present invention relates to coal chemical technology, be specifically related to a kind of production equipment and production method of middle temperature modified pitch.
Background technology
Mid-temperature pitch softening temperature is low, but β resin content and coking value are all lower, transport in summer and long distance transportation inconvenience, and when Tan Su enterprise produces, exhaust gas volumn, loss, pollution are also large, and carbon product electric conductivity, intensity index are also poor; Modified pitch β resin content and coking value are all more satisfactory, modified pitch coking value is higher than 50%, Jiao that more bonds can be generated during roasting, but rheological property is deteriorated, need by heat-conducting oil heating to higher temperature during production, not only energy consumption is large, and when using close to or exceed heat conduction oil flash, bring potential safety hazard.
Present most of Graphite Electrodes manufacturing enterprise, in order to increase electrode lumber recovery, the physical strength improving electrode and electroconductibility, simultaneously in order to reduce energy consumption, reduce equipment failure, requires warm modified pitch (softening temperature SP90 ~ 100 DEG C) in use.This will be a trend, also meet the direction of energy-saving and emission-reduction.Do not have the enterprise of condition with allotment pitch yet, namely mix with the proportions of mid-temperature pitch by processing requirement with modified pitch, but this can bring the problem that before 360 DEG C, quantity of distillate is higher.
Design asphalt is as table 1.
The technical indicator of table 1 binder pitch
As seen from the above table, middle temperature modified pitch is except requiring that softening temperature is low, and other each index such as toluene insolubles content (TI), quinoline insolubles content (QI), coking value (CV) etc. need higher, close with modified pitch Indexes Comparison.
Owing to mutually restricting between each index during production pitch, while namely improving β-resin and CV, SP also can rise.According in the past and the knowhow of fraternal producer, in preparation, warm modified pitch generally adopts following steps: first coal tar is passed through vaporizer, by oil gas pre-evaporation, again prepare modified pitch through reactor, then return to join with flash oil and obtain middle temperature modified pitch, to reach high TI, QI, CV, the feature of low SP.But due to return join flash oil after can bring 360 DEG C before quantity of distillate high (volatile matter is high), contaminate environment during use, increases consumption.
Patent CN201010110449.5 discloses a kind of production method of middle temperature modified pitch, raw material first sends into tube furnace, generate high temperature tar, the high temperature tar generated sends into flash evaporator through main pipeline, separately be provided with a road secondary duct and lead directly to reaction tower, high temperature tar generates mid-temperature pitch through distillation, and then warm modified pitch in generating in reaction tower, and temperature of reaction is regulated by the add-on adjusting high temperature tar.The shortcoming of this invention is that high temperature tar mixes with modified pitch, and light ends is many, and coking value is low.CN201010110445.7 adopts compressive reaction and vacuum flashing equally, provides thermal source with high temperature tar, and before making 360 DEG C, quantity of distillate is higher.
CN200810038495.1 discloses the method for warm modified pitch in the production of a kind of two sections of series connection continuous pressure hot polymerizations, mid-temperature pitch obtains modified pitch by the polycondensation of two sections of cascade reaction still low-pressure heatings, wherein, carry out heating pre-scission reaction at first paragraph, carry out heating polycondensation fast at second segment, thus improve β value; Reacted material enters flashing tower, regulates the softening temperature of pitch at this.The shortcoming of this invention is that temperature of reaction is up to more than 390 DEG C, easy generation mesophase spherule (as accompanying drawing 2a), the generation of mesophase spherule can hinder coal-tar pitch to the infiltration in particles of aggregates micropore in kneading process, thus reduce the bonding strength of coal-tar pitch and solid carbon pledge material, be unfavorable for that the intensity of Carbon Materials improves.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is to provide a kind of without Existing in Improved Pitch Production System warm in mesophase spherule, provides a kind of without modified pitch production method warm in mesophase spherule simultaneously.
Technical scheme of the present invention is, a kind of without Existing in Improved Pitch Production System warm in mesophase spherule, the reactor comprising second evaporator or king-tower and be connected with second evaporator or king-tower, second evaporator or king-tower are connected with several normal-pressure reaction kettles of connecting by gravity flow or transferpump; Be provided with agitator in described reactor, each reactor is other is provided with heating unit;
Described reactor top is connected with immersion cooler, and described immersion cooler is connected with gas-liquid separator, and described gas-liquid separator bottom is connected with flash distillation oil groove;
Described reactor bottom is connected with pitch medial launder.
In air distillation technique, second evaporator is used for separate bitumen, and the inside only has several pieces of traverse baffles; In reduced pressure distillation process, do not have second evaporator, pitch is separated in king-tower, and there are tens blocks of column plates the inside.By being connected with reactor from stream mode in air distillation technique; In reduced pressure distillation process, king-tower is connected with reactor by transferpump.Flash distillation oil groove plays storage effect, for joining oil.
According to of the present invention without Existing in Improved Pitch Production System warm in mesophase spherule, preferably, described agitator is anchor frame.
According to of the present invention without Existing in Improved Pitch Production System warm in mesophase spherule, preferably, described reactor is 2-6.
Wherein, in a preferred embodiment, described reactor bottom is connected with pitch medial launder by an inverted-loop tube.The effect of inverted-loop tube keeps the constant liquid level in reactor.
Further, described gas-liquid separator is also connected with liquid seal can, and liquid seal can connects into loop via gas blower and described heating unit.That is, in this preferred version, the non-condensable gases obtained through gas-liquid separator can as the combustion material recycle of heating unit.Certainly, heating unit also can be connected with other fuel source systems.
Present invention also offers a kind of without modified pitch production method warm in mesophase spherule, the method comprises:
A, high temperature tar are through normal pressure or underpressure distillation, mid-temperature pitch is obtained in second evaporator or king-tower, softening temperature (SP) controls at 70 DEG C ~ 85 DEG C, and toluene insolubles content (TI) control >=12%, quinoline insolubles content (QI) control >=3%, coking value (CV) control >=45%;
B, mid-temperature pitch be several normal-pressure reaction kettles successively by connecting by gravity flow or transferpump, have agitator in reactor, and reactor is other is provided with heating unit.Temperature of reaction 360 DEG C ~ 380 DEG C, reaction times 5 ~ 15h, do not produced the middle temperature modified pitch of mesophase spherule, gained enters in pitch medial launder without modified pitch warm in mesophase spherule;
The oil gas that c, reaction produce is from the top of reactor through immersion cooler condensing cooling, then through gas-liquid separator, the liquid phase obtained enters flash distillation oil groove.
In accordance with the present production process, preferably, the heating raw of described heating unit is coal gas, electricity, high-temp waste gas or other heating agent.Make in reactor, to reach required temperature of reaction by heating and thermal insulation.
Wherein preferably, described agitator is anchor frame; Described reactor is 2-6.
Wherein, described reactor bottom is connected with pitch medial launder by an inverted-loop tube.
Further, the incoagulability gas obtained through immersion cooler condensing cooling after liquid seal can by perfect combustion in gas blower suction heating unit.That is, in this preferred version, the non-condensable gases obtained through gas-liquid separator can as the combustion material of heating unit, recycle.Certainly, heating unit also can be connected with other fuel source systems.The asphalt modifier non-condensable gases that the present invention obtains and the composition of coke-oven gas and calorific value comparative result see the following form 2.
Table 2 asphalt modifier non-condensable gas and coke-oven gas composition and calorific value
| Asphalt modifier non-condensable gas | Coke-oven gas | |
| H 2，mol% | 30.03 | 57.42 |
| CH 4，mol% | 47.18 | 26.63 |
| CO，mol% | 2.32 | 6.91 |
| CO 2，mol% | 1.89 | 2.67 |
| C nH m，mol% | 15.42 | 2.16 |
| H 2S，mol% | 2.11 | |
| Calorific value, MJ/m 3 | 32.66 | 20.16 |
The invention has the beneficial effects as follows: by controlling mid-temperature pitch quality index, then make its normal pressure gentleness reaction at low temperatures, must not return with flash oil and join, obtain not containing the middle temperature modified pitch of mesophase spherule.And the oil gas that reaction produces obtains effective recycling, reaches the effect of the energy that economizes on resources.The non-condensable gases produced, its calorific value, higher than coke-oven gas, is the fuel source of comparatively high-quality.
Accompanying drawing explanation
Fig. 1 is warm Existing in Improved Pitch Production System schema in the present invention.
In figure, 1-second evaporator or king-tower, 2-transferpump, 3-reactor, 4-agitator, 5-heating unit, 6-inverted-loop tube, 7-pitch medial launder, 8-water cooler, 9-vapour liquid separator, 10-flash distillation oil groove, 11-liquid seal can, 12-gas blower.
Fig. 2 is middle temperature modified pitch mesophase spherule comparison diagram.
Fig. 2 a is phasor in the middle of existing middle temperature modified pitch.Fig. 2 b is the middle phasor (mesophase spherule content is 0) of warm modified pitch in the present invention.
Embodiment
Embodiment 1
As shown in Figure 1, a kind of without Existing in Improved Pitch Production System warm in mesophase spherule, the reactor comprising king-tower and be connected with king-tower, king-tower 1 is connected with the normal-pressure reaction kettle 3 that several are connected by transferpump 2; Be provided with agitator 4 in described reactor 3, each reactor 3 is other is provided with heating unit 5; Reactor 3 top is connected with immersion cooler 8, and immersion cooler 8 is connected with gas-liquid separator 9, and described gas-liquid separator 9 bottom is connected with flash distillation oil groove 10; Reactor 3 bottom is connected with pitch medial launder 7 by an inverted-loop tube 6, and the effect of inverted-loop tube keeps the constant liquid level in reactor.
Described gas-liquid separator 9 is connected with liquid seal can 11, and liquid seal can 11 connects into loop via gas blower 12 and described heating unit 5.The non-condensable gases obtained through gas-liquid separator 9 can as the combustion material recycle of heating unit 5.
High temperature tar, through air distillation, discharges mid-temperature pitch from king-tower 1, and SP is 83 DEG C, and TI is 16%, QI is 5%, CV is 49%.Mid-temperature pitch is successively by the normal-pressure reaction kettle 3 of two series connection, and reactor 3 produces heat heating and thermal insulation by gas-fired, temperature of reaction first still 360 DEG C, the second still 365 DEG C, the total 6h of reaction times each 3h(), obtain middle temperature modified pitch.SP is 95 DEG C, and TI is 24%, QI is 6%, CV is 54%, without mesophase spherule, sees Fig. 2 b.Middle temperature modified pitch enters pitch medial launder 7 through inverted-loop tube 6.
The oil gas that reaction produces is through immersion cooler condensing cooling, then through gas-liquid separator, its liquid phase enters flash distillation oil groove, and incoagulability gas after liquid seal can by the perfect combustion of gas blower suction process furnace, provide pitch to react institute's heat requirement.
Embodiment 2
As shown in Figure 1, a kind of without Existing in Improved Pitch Production System warm in mesophase spherule, the reactor comprising second evaporator 1 and be connected with second evaporator 1, second evaporator 1 is connected with the normal-pressure reaction kettle 3 that several are connected by gravity flow; Be provided with agitator 4 in described reactor 3, each reactor 3 is other is provided with heating unit 5; Reactor 3 top is connected with immersion cooler 8, and immersion cooler 8 is connected with gas-liquid separator 9, and described gas-liquid separator 9 bottom is connected with flash distillation oil groove 10; Reactor 3 bottom is connected with pitch medial launder 7 by an inverted-loop tube 6, and the effect of inverted-loop tube keeps the constant liquid level in reactor.
Described gas-liquid separator 9 is connected with liquid seal can 11, and liquid seal can 11 is connected with coal gas system via gas blower 12.The non-condensable gases obtained through gas-liquid separator 9 can reclaim is used as him.
High temperature tar, through air distillation, discharges mid-temperature pitch from second evaporator 1, and SP is 80 DEG C, and TI is 15%, QI is 4.5%, CV is 48%.Mid-temperature pitch is successively by the normal-pressure reaction kettle of four series connection, and reactor passes through electrical heat tracing, temperature of reaction first still 365 DEG C, the second still 375 DEG C, the 3rd still 375 DEG C, the 4th still 365 DEG C, the total 8h of reaction times each 2h(), obtain middle temperature modified pitch.SP is 98 DEG C, and TI is 26%, QI is 6%, CV is 55%, without mesophase spherule.Middle temperature modified pitch enters pitch medial launder through inverted-loop tube.
The oil gas that reaction produces is through immersion cooler condensing cooling, then through gas-liquid separator, its liquid phase enters flash distillation oil groove, and incoagulability gas after liquid seal can by gas blower suction coal gas system.
Embodiment 3
High temperature tar, through air distillation, discharges mid-temperature pitch from second evaporator 1, and SP is 75 DEG C, and TI is 14%, QI is 4%, CV is 47%.Mid-temperature pitch is successively by the normal-pressure reaction kettle of three series connection, and reactor passes through high-temp waste gas heating and thermal insulation, temperature of reaction first still 375 DEG C, the second still 380 DEG C, the 3rd still 375 DEG C, the total 9h of reaction times each 3h(), obtain middle temperature modified pitch.SP is 93 DEG C, and TI is 27%, QI is 7%, CV is 54%, without mesophase spherule.Middle temperature modified pitch enters pitch medial launder through inverted-loop tube.
Other are with embodiment 2.
Embodiment 4
High temperature tar, through underpressure distillation, extracts mid-temperature pitch out with transferpump 2 from tar king-tower 1, and SP is 70 DEG C, and TI is 12%, QI is 3%, CV is 45%.Mid-temperature pitch is successively by two group reaction stills in parallel, and often group is three still series connection, and reactor is by superheated vapour heating and thermal insulation, first still 375 DEG C of every group reaction still, the second still 380 DEG C, the 3rd still 375 DEG C, the total 15h of reaction times each 5h(), obtain middle temperature modified pitch.SP is 97 DEG C, and TI is 28%, QI is 8%, CV is 56%, without mesophase spherule.
Other are with embodiment 1.
The present invention is by the reasonable setting of production equipment, and by controlling mid-temperature pitch quality index, make its normal pressure gentleness reaction at low temperatures, must not return with flash oil and join, obtain not containing the middle temperature modified pitch of mesophase spherule, the oil gas that reaction produces obtains effective recycling, reaches the effect of the energy that economizes on resources.
Claims (5)
1., without a modified pitch production method warm in mesophase spherule, it is characterized in that: the method comprises:
A, high temperature tar are through normal pressure or underpressure distillation, mid-temperature pitch is obtained in second evaporator/king-tower (1), softening temperature controls at 70 DEG C ~ 85 DEG C, and toluene insolubles content control >=12%, quinoline insolubles content control >=3%, coking value control >=45%;
B, mid-temperature pitch be several normal-pressure reaction kettles (3) successively by connecting by gravity flow or transferpump (2), have agitator (4) in reactor, and reactor (3) is other is provided with heating unit (5); Temperature of reaction 360 DEG C ~ 380 DEG C, reaction times 5 ~ 15h, is not produced the middle temperature modified pitch of mesophase spherule, and gained enters in pitch medial launder (7) without modified pitch warm in mesophase spherule;
The oil gas that c, reaction produce is from the top of reactor (3) through immersion cooler (8) condensing cooling, then through gas-liquid separator (9), the liquid phase obtained enters flash distillation oil groove (10); Described gas-liquid separator (9) is connected with liquid seal can (11), and liquid seal can (11) connects into loop via gas blower (12) and described heating unit (5).
2. according to claim 1 without modified pitch production method warm in mesophase spherule, it is characterized in that: the heating raw of described heating unit is coal gas, electricity, high-temp waste gas or other heating agent.
3. according to claim 1 without modified pitch production method warm in mesophase spherule, it is characterized in that: described agitator is anchor frame; Described reactor (3) is 2-6.
4. according to claim 1 without modified pitch production method warm in mesophase spherule, it is characterized in that: described reactor (3) bottom is connected with pitch medial launder (7) by an inverted-loop tube (6).
5. according to any one of Claims 1 to 4 without modified pitch production method warm in mesophase spherule, it is characterized in that: the incoagulability gas obtained through immersion cooler (8) condensing cooling after liquid seal can (11) by perfect combustion in gas blower (12) suction heating unit (5).
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804758B (en) * | 2015-04-09 | 2017-04-05 | 河南开炭新材料有限公司 | Heating flash evaporation holds the technique for pressing modified coal tar pitch |
| CN105331384B (en) * | 2015-11-23 | 2018-03-09 | 首钢水城钢铁（集团）有限责任公司 | A kind of modified coal tar pitch continuous process system and its method |
| CN109237493A (en) * | 2017-07-10 | 2019-01-18 | 宝武炭材料科技有限公司 | The processing unit and method of modified coal tar pitch reaction kettle flashed vapour |
| CN109251757A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | Method for producing mesophase-free asphalt by using reaction kettle |
| CN114540064A (en) * | 2022-03-04 | 2022-05-27 | 中冶焦耐(大连)工程技术有限公司 | Process and system for producing modified asphalt by combining direct heating kettle with modifying tower |
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| CN1970689A (en) * | 2006-12-13 | 2007-05-30 | 上海奥韦通工程技术有限公司 | Process for preparing modified asphalt |
| CN101289624A (en) * | 2008-06-03 | 2008-10-22 | 山西宏特煤化工有限公司 | Process for producing moderate temperature modified bitumen by continuously pressurizing and hot-polymerizing at two stages connected in series |
| CN102311747A (en) * | 2011-08-30 | 2012-01-11 | 河南宝舜化工科技有限公司 | Furnace-kettle type modified pitch production system and production process |
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| CN1970689A (en) * | 2006-12-13 | 2007-05-30 | 上海奥韦通工程技术有限公司 | Process for preparing modified asphalt |
| CN101289624A (en) * | 2008-06-03 | 2008-10-22 | 山西宏特煤化工有限公司 | Process for producing moderate temperature modified bitumen by continuously pressurizing and hot-polymerizing at two stages connected in series |
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| 武钢煤沥青发展对策和生产技术研究;李超;《中国优秀硕士学位论文全文数据库 工程科技I辑》;中国优秀硕士学位论文全文数据库 工程科技I辑;20100215;正文第9-10、14-15页及图2.7 * |
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Address after: 2004-2002 Weisan Road Chemical Office Building, Baoshan District, Shanghai Patentee after: Baowu Carbon Material Technology Co., Ltd. Address before: 2004-2002 Weisan Road Chemical Office Building, Baoshan District, Shanghai Patentee before: Chemical Co., Ltd. of Baoshan Iron and Steel Group, Shanghai |
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Address after: 200942 three chemical engineering office building, Baoshan Iron and steel factory, Shanghai, Baoshan District Patentee after: Baowu Carbon Technology Co.,Ltd. Address before: 200942 three chemical engineering office building, Baoshan Iron and steel factory, Shanghai, Baoshan District Patentee before: BAOWU CARBON MATERIAL TECHNOLOGY Co.,Ltd. |
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