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CN105131999A - Technology and device for single furnace single kettle production of modified asphalt - Google Patents

Technology and device for single furnace single kettle production of modified asphalt Download PDF

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Publication number
CN105131999A
CN105131999A CN201510500851.7A CN201510500851A CN105131999A CN 105131999 A CN105131999 A CN 105131999A CN 201510500851 A CN201510500851 A CN 201510500851A CN 105131999 A CN105131999 A CN 105131999A
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China
Prior art keywords
reactor
pitch
oil
asphalt
reaction kettle
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Pending
Application number
CN201510500851.7A
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Chinese (zh)
Inventor
杨浩
叶煌
姜秋
孙虹
单春华
贾骞
薛海凤
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Acre Coking and Refractory Engineering Consulting Corp MCC
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Acre Coking and Refractory Engineering Consulting Corp MCC
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Priority to CN201510500851.7A priority Critical patent/CN105131999A/en
Publication of CN105131999A publication Critical patent/CN105131999A/en
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Abstract

The present invention relates to a technology and device for single furnace single kettle production of modified asphalt, bitumen come from a tar distillation apparatus and reaction kettle heating furnace outlet asphalt are mixed in a mixer, then together enter into a reaction kettle for thermal cracking and thermal polymerization reaction to produce beta- resin and alpha- resin; reaction kettle bottom asphalt is extracted out by an asphalt circulation pump, and most of the reaction kettle bottom asphalt is sent into a reaction kettle heating furnace for heating cycle to back to the reaction kettle, a small portion of the reaction kettle bottom asphalt and pyrolysis gas come from the reaction kettle top respectively enter a flash evaporation column for flash evaporation steam stripping; modified asphalt collected from the flash evaporation column bottom enters into an asphalt molding unit after heat exchange and cooling. By use of the method for shortening the technical process, equipment and piping coking and clogging probability can be effectively reduced, through comprehensive regulation of the reaction temperature, reaction pressure and residence time within the reaction kettle, resin transformation control can be achieved, requirements for production of an asphalt product required by an indicator can be met, investment is low, energy consumption is low, and environmental protection effect is good.

Description

Single stove list still produces technique and the device of modified pitch
Technical field
The present invention relates to modified pitch production technical field in coking engineering projects field, particularly relate to a kind of employing diamond heating, in a reactor, technique and the device of modified pitch produced by single stove list still of continuous seepage modified pitch.
Background technology
Coal-tar pitch, mainly for the preparation of Graphite Electrodes, the anode of aluminium metallurgy, the electrode carbon cellulosic material of Electric furnace steel making, also can be used for making carbon black and using as fuel.Along with the development of Chinese large-sized aluminium cell and large-capacity high-power direct current electric arc furnace, large size prebaked anode and superpower ultra-high power graphite electrode are had higher requirement, for the requirement also corresponding raising of the asphalt quality of the high-grade carbon material goods of this two class of production, namely need to adopt modified pitch.
The modification technology of pitch refers to the hot cracked and heat polymerization of pitch, the QI in pitch meet increase within the scope of index request, increase β resin content as far as possible, thus obtain the modified pitch meeting quality index and require.
The method for modifying of current pitch mainly contains: vacuum flashing method, normal pressure thermal polymerization method and pressurization thermal polymerization method.Wherein thermal polymerization method is divided into again autoclave thermal polymerization method and tube furnace thermal polymerization method.Tube furnace thermal polymerization method can be described as the technique of current reasonable production modified pitch, and the modified pitch product index adjustability produced is large, can meet the requirement of different user.
Current tube furnace thermal polymerization method adopts the pitch of about 360 DEG C come from tar distillation device to be raw material, it enters pitch reactor after mixing with the first reactor furnace outlet circulation pitch, the temperature of reaction of the first reactor is at about 370 DEG C, and reaction pressure is 0.3MPa.Bottom reactor, pitch is extracted out through pitch recycle pump, major part delivers to the first diamond heating circulation, after small portion mixes with the second reactor bottom cycle pitch, send into the second tube furnace stove by pitch recycle pump to heat, after heating, pitch sends into the second reactor, the temperature of reaction of the second reactor is at about 390 DEG C, and reaction pressure is 0.3MPa.Flashing tower delivered to by second Polycondensation Reactor and Esterification Reactor small portion pitch and reactor top splitting gas, and the superheated vapour amount injected by adjustment, regulates the softening temperature of modified pitch.
Tube furnace thermal polymerization method achieves the continuous seepage of pitch, and stable, and can control respectively the content of α resin and β resin, quality product is high, and adjustability is large.But because technical process is long, inevitably result in blockage to e-quipment and pipe, need stop work processes coking material.
Summary of the invention
The invention provides the technique that modified pitch produced by a kind of single stove list still, adopt the method for shortened process, effectively reduce the probability of equipment and pipeline coking, blocking, simultaneously by comprehensive adjustment reactor interior reaction temperature, reaction pressure and the residence time, realize the control to resin transitions, meet the needs of the modified pitch product producing a certain index request; Low, the less energy consumption of its investment, environment protecting is good; Invention also provides the device for realizing this technique.
In order to achieve the above object, the present invention realizes by the following technical solutions:
The technique of modified pitch produced by single stove list still, comprises the steps:
1) pitch without cooling that tar distillation device is next, after mixing in a mixer, together enters in reactor and thermo-cracking and heat polymerization occurs, and generate β resin and α resin with the outlet pitch of reactor process furnace;
2) reactor is by the heat supply of reactor process furnace, and temperature controls between 380 ~ 410 DEG C, and pressure is by nitrogen regulable control between 0 ~ 0.4MPa, and the residence time of mix asphalt in reactor controls at 6 ~ 10h;
3) bottom reactor, pitch is extracted out through pitch recycle pump, and major part is delivered to reactor process furnace and get back to reactor after heating cycle, and the splitting gas that small portion and reactor eject enters flashing tower respectively and carries out flash distillation stripping; Temperature in flashing tower is between 350 ~ 450 DEG C, and pressure is between 50 ~ 110KPa.a;
4) the flash oil vapour that steams of flash distillation tower top and vapour mixture together enter flash oil condensing water cooler, deliver to oil-water separation tank and carry out oily water separation after condensing cooling;
5) oil-water separation tank top dispersing gas is delivered in exhaust washing column through flue gas Washers, sprays, then send reactor process furnace to burn in exhaust washing column with circulating washing oil; Cleaning oil groove adopts steam heating, and regularly injects new washing oil;
6) the modified pitch product of extraction at the bottom of flashing tower pumps out through pitch extraction, after heat exchange cooling, enter asphalt moulding unit.
In reactor, by comprehensive adjustment reactor interior reaction temperature, reaction pressure and the residence time of pitch in reactor, produce the modified pitch product of different index request.
In flashing tower, the superheated vapour amount injected by adjustment produces the modified pitch product that different softening point requires.
The device of the technique of modified pitch is produced for realizing single stove list still, comprise reactor, reactor process furnace, flashing tower, oil-water separation tank, exhaust washing column and cleaning oil groove, the upper feed inlet of described reactor connects mixing tank, and mixing tank connects the pitch discharge port of tar distillation device and the bottom pitch discharge port of reactor process furnace respectively; The bottom discharge mouth of reactor is by the pitch recycle pump top bitumen feed mouth of ligation still process furnace and the upper feed inlet of flashing tower respectively; The top splitting gas outlet of reactor connects the middle part opening for feed of flashing tower; Finished product discharge port at the bottom of flashing tower is connected the opening for feed of asphalt moulding unit through pitch extraction pump after interchanger; The flash oil vapour at flashing tower top and vapour mixture outlet connect oil-water separation tank after condensate cooler; The top dispersing gas outlet of oil-water separation tank connects exhaust washing column through flue gas Washers, is connected, the inlet mouth bottom air outlet, top ligation still process furnace bottom exhaust washing column with cleaning oil groove.
Described reactor process furnace is tubular oven.
Circulating washing oil flusher is established on described exhaust washing column top, and establish steam heater in cleaning oil groove, new washing oil opening for feed is established at top.
Compared with prior art, the invention has the beneficial effects as follows:
1) method of shortened process is adopted, effectively reduce the probability of equipment and pipeline coking, blocking, simultaneously by comprehensive adjustment reactor interior reaction temperature, reaction pressure and the residence time, realize the control to resin transitions, meet the needs of the modified pitch product producing a certain index request;
2) change single stove list still into by the two still of twin furnace to produce, the occupation of land related to, structure steel fabrication and installation, equipment purchase, pipeline, instrument installation costs all significantly reduce, therefore less investment; The public auxiliary consumption such as coal gas during production, nitrogen, power consumption also reduce thereupon, therefore energy consumption reduces;
3) the present invention adopts closed circulatory system, does not have harmful substances and arranges outward, and environment protecting is good.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
In figure: 1. reactor 2. pitch recycle pump 3. mixing tank 4. reactor process furnace 5. flashing tower 6. flash oil condensing water cooler 7. oil-water separation tank 8. cleans oil groove 9. and is vented washing column 10. flue gas Washers 11. pitch extraction pump 12. interchanger
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further:
Seeing Fig. 1, is process flow sheet of the present invention, and the technique of modified pitch produced by single stove list still of the present invention, comprises the steps:
1) pitch without cooling that tar distillation device is next, after mixing, together enters in reactor 1 and thermo-cracking and heat polymerization occurs, and generate β resin and α resin with the outlet pitch of reactor process furnace 4 in mixing tank 3;
2) reactor 1 is by reactor process furnace 4 heat supply, and temperature controls between 380 ~ 410 DEG C, and pressure is by nitrogen regulable control between 0 ~ 0.4MPa, and the residence time of mix asphalt in reactor 1 controls at 6 ~ 10h;
3) bottom reactor 1, pitch is extracted out through pitch recycle pump 2, and major part is delivered to reactor process furnace 4 after heating cycle, got back to reactor 1, and the splitting gas that small portion and reactor 1 eject enters flashing tower 5 respectively and carries out flash distillation stripping; Temperature in flashing tower 5 is between 350 ~ 450 DEG C, and pressure is between 50 ~ 110KPa.a;
4) flashing tower 5 pushes up the flash oil vapour that steams and vapour mixture together enters flash oil condensing water cooler 6, delivers to oil-water separation tank 7 and carry out oily water separation after condensing cooling;
5) oil-water separation tank 7 top dispersing gas is delivered in exhaust washing column 9 through flue gas Washers 10, sprays, then send reactor process furnace 4 to burn in exhaust washing column 9 with circulating washing oil; Cleaning oil groove 8 adopts steam heating, and regularly injects new washing oil;
6) the modified pitch product of extraction at the bottom of flashing tower is sent through pitch extraction pump 11, after heat exchange cooling, enter asphalt moulding unit.
In reactor 1, by comprehensive adjustment reactor 1 interior reaction temperature, reaction pressure and the residence time of pitch in reactor 1, produce the modified pitch product of different index request.
In flashing tower 5, the superheated vapour amount injected by adjustment produces the modified pitch product that different softening point requires.
The device of the technique of modified pitch is produced for realizing single stove list still, comprise reactor 1, reactor process furnace 4, flashing tower 5, oil-water separation tank 7, exhaust washing column 9 and cleaning oil groove 10, the upper feed inlet of described reactor 1 connects mixing tank 3, and mixing tank 3 connects the pitch discharge port of tar distillation device and the bottom pitch discharge port of reactor process furnace 4 respectively; The bottom discharge mouth of reactor 1 is by the pitch recycle pump 2 top bitumen feed mouth of ligation still process furnace 4 and the upper feed inlet of flashing tower 5 respectively; The top splitting gas outlet of reactor 1 connects the middle part opening for feed of flashing tower 5; Finished product discharge port at the bottom of flashing tower is connected the opening for feed of asphalt moulding unit through pitch extraction pump 11 after interchanger 12; The flash oil vapour at flashing tower 5 top and vapour mixture outlet connect oil-water separation tank 7 after flash oil condensing water cooler 6; The top dispersing gas outlet of oil-water separation tank 7 connects exhaust washing column 9 through flue gas Washers 10, is connected, the inlet mouth bottom air outlet, top ligation still process furnace 4 bottom exhaust washing column 9 with cleaning oil groove 8.
Described reactor process furnace 4 is tubular oven.
Circulating washing oil flusher is established on described exhaust washing column 9 top, and establish steam heater in cleaning oil groove 8, new washing oil opening for feed is established at top.
During aluminium anode, aluminium negative electrode and steel-making pole produce, pitch used is mainly cakingagent.And main in pitch what play cohesive action is β resin, β resin is the solvable and Middle molecule aromatic polymer that benzene (toluene) is insoluble of quinoline, is the close-burning component of authentic representative.When carrying out heat to pitch, at high temperature there is thermo-cracking and heat polymerization in the aromatic hydrocarbon molecule in pitch, in pitch, a part for original β component can be converted into α component, the γ component of benzene (toluene) solvend is converted into β component (secondary β resin), and its transforming degree increases with the rising of Heating temperature and the prolongation in reaction times.
In reaction pressure raising situation, Reaction time shorten, thermal polycondensation is strengthened, and thermolysis weakens, and β resin content can be made obviously to increase.In a reactor, orthogonal experiment is done to temperature of reaction, reaction pressure and the residence time three key elements, a suitable reaction conditions can be found to realize the transformation between resin, thus produce the modified pitch product of a certain index request.Therefore a completely available reactor replaces two reactors.
The present invention with tar distillation device come pitch for main raw material, thermo-cracking and heat polymerization occur in reactor 1, and generate β resin and α resin, heat is supplied by reactor process furnace 4.The temperature of reactor 1 controls between 380 ~ 410 DEG C, and pressure-controlling is between 0 ~ 0.4MPa, and the reaction times is about 6 ~ 10h, can control β resin content and QI index by the above processing parameter of comprehensive adjustment.

Claims (6)

1. the technique of modified pitch produced by single stove list still, it is characterized in that, comprise the steps:
1) pitch without cooling that tar distillation device is next, after mixing in a mixer, together enters in reactor and thermo-cracking and heat polymerization occurs, and generate β resin and α resin with the outlet pitch of reactor process furnace;
2) reactor is by the heat supply of reactor process furnace, and temperature controls between 380 ~ 410 DEG C, and pressure is by nitrogen regulable control between 0 ~ 0.4MPa, and the residence time of mix asphalt in reactor controls at 6 ~ 10h;
3) bottom reactor, pitch is extracted out through pitch recycle pump, and major part is delivered to reactor process furnace and get back to reactor after heating cycle, and the splitting gas that small portion and reactor eject enters flashing tower respectively and carries out flash distillation stripping; Temperature in flashing tower is between 350 ~ 450 DEG C, and pressure is between 50 ~ 110KPa.a;
4) the flash oil vapour that steams of flash distillation tower top and vapour mixture together enter flash oil condensing water cooler, deliver to oil-water separation tank and carry out oily water separation after condensing cooling;
5) oil-water separation tank top dispersing gas is delivered in exhaust washing column through flue gas Washers, sprays, then send reactor process furnace to burn in exhaust washing column with circulating washing oil; Cleaning oil groove adopts steam heating, and regularly injects new washing oil;
6) the modified pitch product of extraction at the bottom of flashing tower pumps out through pitch extraction, after heat exchange cooling, enter asphalt moulding unit.
2. the technique of modified pitch produced by single stove list still according to claim 1, it is characterized in that, in reactor, by comprehensive adjustment reactor interior reaction temperature, reaction pressure and the residence time of pitch in reactor, produce the modified pitch product of different index request.
3. the technique of modified pitch produced by single stove list still according to claim 1, it is characterized in that, in flashing tower, the superheated vapour amount injected by adjustment produces the modified pitch product that different softening point requires.
4. the device of the technique of modified pitch is produced for realizing single stove list still according to claim 1, it is characterized in that, comprise reactor, reactor process furnace, flashing tower, oil-water separation tank, exhaust washing column and cleaning oil groove, the upper feed inlet of described reactor connects mixing tank, and mixing tank connects the pitch discharge port of tar distillation device and the bottom pitch discharge port of reactor process furnace respectively; The bottom discharge mouth of reactor is by the pitch recycle pump top bitumen feed mouth of ligation still process furnace and the upper feed inlet of flashing tower respectively; The top splitting gas outlet of reactor connects the middle part opening for feed of flashing tower; Finished product discharge port at the bottom of flashing tower is connected asphalt moulding unit feed mouth through pitch extraction pump after interchanger; The flash oil vapour at flashing tower top and vapour mixture outlet connect oil-water separation tank after condensate cooler; The top dispersing gas outlet of oil-water separation tank connects exhaust washing column through flue gas Washers, is connected, the inlet mouth bottom air outlet, top ligation still process furnace bottom exhaust washing column with cleaning oil groove.
5. the device of modified pitch produced by single stove list still according to claim 4, and it is characterized in that, described reactor process furnace is tubular oven.
6. the device of modified pitch produced by single stove list still according to claim 4, and it is characterized in that, circulating washing oil flusher is established on described exhaust washing column top, and establish steam heater in cleaning oil groove, new washing oil opening for feed is established at top.
CN201510500851.7A 2015-08-14 2015-08-14 Technology and device for single furnace single kettle production of modified asphalt Pending CN105131999A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108315036A (en) * 2018-02-28 2018-07-24 黄骅市信诺立兴精细化工股份有限公司 The production technology of coalite tar heavy constituent production modified coal tar pitch in a kind of utilization
CN108641740A (en) * 2018-05-31 2018-10-12 山西豪仑科化工有限公司 A kind of modified coal tar pitch and preparation method and application by alternating temperature production of pressurizeing
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
CN110813951A (en) * 2019-10-28 2020-02-21 鞍钢股份有限公司 Method for cleaning coking materials in modified asphalt production system by using wash oil
CN113817491A (en) * 2021-10-08 2021-12-21 辽宁宝来生物能源有限公司 Special apparatus for producing of mesophase pitch
CN114164013A (en) * 2021-12-20 2022-03-11 祥峰科技有限公司 Modified asphalt preparation system

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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
CN204939397U (en) * 2015-08-14 2016-01-06 中冶焦耐工程技术有限公司 The device of modified pitch produced by single stove list still

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US4096056A (en) * 1976-10-21 1978-06-20 Witco Chemical Corporation Method of producing an impregnating petroleum pitch
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
CN204939397U (en) * 2015-08-14 2016-01-06 中冶焦耐工程技术有限公司 The device of modified pitch produced by single stove list still

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN108315036A (en) * 2018-02-28 2018-07-24 黄骅市信诺立兴精细化工股份有限公司 The production technology of coalite tar heavy constituent production modified coal tar pitch in a kind of utilization
CN108641740A (en) * 2018-05-31 2018-10-12 山西豪仑科化工有限公司 A kind of modified coal tar pitch and preparation method and application by alternating temperature production of pressurizeing
CN110813951A (en) * 2019-10-28 2020-02-21 鞍钢股份有限公司 Method for cleaning coking materials in modified asphalt production system by using wash oil
CN110813951B (en) * 2019-10-28 2021-05-28 鞍钢股份有限公司 Method for cleaning coking materials in modified asphalt production system by using wash oil
CN113817491A (en) * 2021-10-08 2021-12-21 辽宁宝来生物能源有限公司 Special apparatus for producing of mesophase pitch
CN113817491B (en) * 2021-10-08 2022-05-13 辽宁宝来生物能源有限公司 Special apparatus for producing of mesophase pitch
CN114164013A (en) * 2021-12-20 2022-03-11 祥峰科技有限公司 Modified asphalt preparation system

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