CN103977591B - A kind of scraper plate rectifying column refining for adiponitrile and adiponitrile process for refining - Google Patents
A kind of scraper plate rectifying column refining for adiponitrile and adiponitrile process for refining Download PDFInfo
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- CN103977591B CN103977591B CN201410236384.7A CN201410236384A CN103977591B CN 103977591 B CN103977591 B CN 103977591B CN 201410236384 A CN201410236384 A CN 201410236384A CN 103977591 B CN103977591 B CN 103977591B
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Abstract
A kind of scraper plate rectifying column refining for adiponitrile, comprise tower body, liquid tremie pipe, packing layer is comprised in described tower body, board-like layer, also comprise scraper evaporator, Matter Transfer mouth, liquid-phase outlet, circulating pump, described scraper evaporator is seal-installed on tower body outside, below last block column plate of board-like layer, described Matter Transfer mouth is outside at board-like layer position tower body, liquid-phase outlet is bottom tower body, Matter Transfer mouth is connected by circulating pump with liquid-phase outlet, the invention has the beneficial effects as follows: the present invention adopts special tower structure, the method of Crystallization Separation is adopted to be separated with other dissolved impurities adiponitrile, adiponitrile product has been reclaimed to greatest extent while obtaining highly purified adiponitrile product.Effectively avoid the problem of traditional rectifier bottoms coking and blocking, improve product purity, reclaim adiponitrile product to greatest extent.
Description
Technical field
The invention belongs to chemical production technology equipment technical field, relate to a kind of scraper plate rectifying column refining for adiponitrile and adiponitrile process for refining particularly.
Background technology
The rectifying column used in existing production adiponitrile process comprises tower body, some layers of column plate are had in tower body, products export is arranged at tower body top, there is feed(raw material)inlet tower body middle and upper part, tower body above feed(raw material)inlet there is reflux inlet, there are Matter Transfer heating exit and Matter Transfer heated inlet at the bottom of tower, at the bottom of tower, also have heavy constituent outlet, between the ground floor column plate (i.e. basecoat column plate) and second layer column plate of tower body, be provided with circulation heavy constituent entrance.Shortcoming is: during production, partial material at the bottom of tower is delivered to ground floor column plate circulate, because the material composition of ground floor column plate changes, heavy constituent increases, the heavy constituent on each layer column plate is above caused also to change, the heavy constituent content in overhead is finally made to increase, poor product quality.
In adiponitrile production process, the mode of separation and purification many employings rectifying of adiponitrile is carried out, and the operation of adiponitrile treating column is very difficult, the easy coking of adiponitrile treating column materials at bottom of tower, crystallization goes out heat exchanger at the bottom of the auxiliary agent blocking tower in product affects normal production process.The thin film evaporation of existing heat sensitive material and the coupled system of distillation system, without circulating pump at the bottom of rectifying tower, if misoperation still can cause the coking of materials at bottom of tower and the precipitation of solid matter, traditional evaporation mode is disposable evaporation, and disengagement area is limited, make material evaporation incomplete, rectifying rate is low; After gas-liquid separation process, still can produce entrainment, separation degree is affected.As shown in Figure 1, refine adiponitrile with traditional process, the component wherein at the bottom of rectifying column 1 tower needs strict control, and not so in adiponitrile, dissolved impurity can because at the bottom of misoperation blocking tower, cause parking; Component at the bottom of No. two rectifying column 2 towers needs strict control, and at the bottom of No. two rectifying column 2 towers in containing non-crystallizable precipitation at the bottom of the tower of a certain amount of adiponitrile composition guarantee No. two rectifying columns 2, the waste of adiponitrile must be caused.
Summary of the invention
The present invention is for better to solve the problems of the technologies described above, adopt scraper plate rectifying column, remove by the method for crystallization the solid impurity be dissolved in adiponitrile, and got rid of by the solid that reaction generates by rotary slagging coutrol system, can be separated and obtain highly purified adiponitrile product.The concrete technical scheme adopted is as follows:
For the scraper plate rectifying column that adiponitrile is refining, comprise tower body, liquid tremie pipe, comprise packing layer, board-like layer in described tower body, packing layer is above board-like layer, and material inlet is in the packing layer bottom of described tower body, and gaseous phase outlet is at the top of tower body, last block column plate of described board-like layer is drawn liquid tremie pipe vertically downward, described scraper plate rectifying column also comprises scraper evaporator, Matter Transfer mouth, liquid-phase outlet, circulating pump, described scraper evaporator comprises transmission device, evaporator tube, external heating jacket, scraper plate bracing ring, scraper plate, feed opening, solid baffle, concave shape gas baffle, described evaporator tube is seal-installed on tower body outside, below last block column plate of board-like layer, evaporator tube lower end arranges feed opening, feed opening adopts blind plate sealing, external overall installs external heating jacket, scraper plate is fixed on scraper plate bracing ring, be installed on evaporator tube inside, and be connected with the transmission device of outside, solid baffle is installed on evaporator tube and tower body junction inner lower, concave shape gas baffle is installed on evaporator tube and tower body junction upper inside, described Matter Transfer mouth is outside at board-like layer position tower body, and liquid-phase outlet is bottom tower body, and Matter Transfer mouth is connected by circulating pump with liquid-phase outlet.
Do not set up circulation at the bottom of traditional scraper plate rectifying column coupled system tower, the retention time of material of easy coking and polymerization is long, arranges after liquid-phase outlet at the bottom of tower and Matter Transfer mouth set up circulation, reduces the time of staying of easy polymer material.
Described scraper evaporator at least comprises an entrance, is installed on tower body outside with horizontal type structure, also comprises and mends nitrogen mouth; be installed on feed opening place, feed opening place increases mends nitrogen mouth, opens during feed opening blanking; during system shutdown, nitrogen protection use is carried out to system, ensure the stability of system.
Described liquid tremie pipe horizontal segment is the shortest, and liquid tremie pipe vertical section and tower body keep the shortest safe distance.Described scraper plate arranges in the shape of a spiral.Be separated by 120 ° between described scraper plate and scraper plate, between adjacent often group scraper plate, rotate 60 ° successively.
The full chuck of evaporator tube, evaporator tube and tower body portion increase concave shape gas baffle; The built-in solid baffle of evaporator tube; Evaporator tube rotary slagging coutrol feed opening place also needs external heating jacket to protect, and feed opening adopts blind plate sealing.Heating medium temperature in scraper evaporator external heating jacket is elevated to 200-280 DEG C, then Produced Liquid in the middle part of tower is entered scraper evaporator, and helical flight is opened, and pushes solid material slag to deslagging feed opening.
Described scraper plate rectifying column is used to carry out the refining technique of adiponitrile, thick adiponitrile upstream device come introduces scraper plate rectifying column, along with the carrying out of rectifying, on column plate, material concentration there occurs change, have solid matter crystallization on board-like layer column plate, thick adiponitrile material liquid is introduced easy crystallization column plate, and the material of this column plate is caused scraper evaporator by liquid tremie pipe, by rotary slagging coutrol system, solid matter is entered feed opening, the gas phase formed in tapping process enters upper strata and continues rectifying, and use circulating pump to make to set up Matter Transfer at the bottom of tower and between board-like layer by Matter Transfer mouth and liquid-phase outlet, in operation, at scraper plate rectifying column top extraction high-purity adiponitrile product, scraper plate rectifier bottoms draws the adiponitrile product containing a small amount of heavy constituent, enter subordinate's rectifying column through buffering and carry out rectifying, the high-purity adiponitrile product of subordinate's rectifying column top extraction, extraction heavy constituent in bottom reclaims.
The operating pressure of described scraper evaporator is 1KPaA-50KPaA, and operating temperature is 200-280 DEG C, and rotating speed is 60 ~ 240r/min.
Open during feed opening blanking and mend nitrogen mouth, nitrogen protection is carried out to system.
The present invention is different from traditional thin film evaporator, vertically horizontal scraper evaporator has been made into by traditional, and be provided with gas and solid baffle at scraper evaporator and rectifying column tower body junction, the solid produced in production process is separated thoroughly with adiponitrile, arranging of gas baffle effectively avoids entrainment, by rotary slagging coutrol system by the solid impurity composition removing in adiponitrile, avoid at the bottom of the stage of rectification crystallization impurity blocking rectifying tower in adiponitrile product purification purification process, effectively protect filler at the bottom of tower and reboiler, and at the bottom of scraper plate evaporating column tower, add circulating pump, make containing adiponitrile Matter Transfer, add the reliability and stability of operation, reclaimed adiponitrile product to greatest extent simultaneously, and obtaining purity is high-purity adiponitrile product.
The invention has the beneficial effects as follows: the present invention adopts special tower structure, adopt the method for Crystallization Separation to be separated with other dissolved impurities adiponitrile, while obtaining highly purified adiponitrile product, reclaimed adiponitrile product to greatest extent.Effectively avoid the problem of traditional rectifier bottoms coking and blocking, improve product purity, reclaim adiponitrile product to greatest extent.
Accompanying drawing explanation
Fig. 1 is traditional rectifying column process chart
Fig. 2 is scraper plate rectifying column adiponitrile process for refining flow chart of the present invention
Fig. 3 is scraper plate rectifying tower structure schematic diagram of the present invention
Fig. 4 is scraper evaporator scraper plate arrangement mode figure of the present invention
Fig. 5 is scraper evaporator scraper plate fixed form figure of the present invention
Marginal data: 1 a, rectifying column, 2, No. two rectifying columns, 3, scraper plate rectifying column, 4, tower body, 5, packing layer, 6, board-like layer, 7, gaseous phase outlet, 8, material inlet, 9, liquid tremie pipe, 10, scraper evaporator, 11, transmission device, 12, evaporator tube, 13, external heating jacket, 14, scraper plate bracing ring, 15, scraper plate, 16, feed opening, 17, solid baffle, 18, concave shape gas baffle, 19, Matter Transfer mouth, 20, liquid-phase outlet, 21, circulating pump, 22,120 ° of angles
A, thick adiponitrile product, B, smart adiponitrile product, C, heavy constituent
Detailed description of the invention
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below the specific embodiment of the present invention being described further, but not limiting protection scope of the present invention.
First for concrete operations flow process of the present invention, be illustrated by reference to the accompanying drawings:
The scraper plate rectifying column that adiponitrile is refining as shown in Figure 3, comprise tower body 4, liquid tremie pipe 9, comprise packing layer 5, board-like layer 6 in described tower body 4, packing layer 5 is above board-like layer 6, material inlet 8 is in packing layer 5 bottom of described tower body 4, and gaseous phase outlet 7 is at the top of tower body 4, described last block column plate of board-like layer 6 is drawn liquid tremie pipe 9 vertically downward, described scraper plate rectifying column also comprises scraper evaporator 10, Matter Transfer mouth 19, liquid-phase outlet 20, circulating pump 21, described scraper evaporator 10 comprises transmission device 11, evaporator tube 12, external heating jacket 13, scraper plate bracing ring 14, scraper plate 15, feed opening 16, solid baffle 17, concave shape gas baffle 18, it is outside that described evaporator tube 12 is seal-installed on tower body 4, below last block column plate of board-like layer 6, evaporator tube 12 lower end arranges feed opening 16, feed opening 16 adopts blind plate sealing, external overall installs external heating jacket 13, scraper plate 15 is fixed on scraper plate bracing ring 14, be installed on evaporator tube 12 inner, and be connected with the transmission device 11 of outside, solid baffle 17 is installed on evaporator tube 12 and tower body 4 junction inner lower, concave shape gas baffle 18 is installed on evaporator tube 12 and tower body 4 junction upper inside, described Matter Transfer mouth 19 is outside at board-like layer 6 position tower body 4, and liquid-phase outlet 20 is bottom tower body 4, and Matter Transfer mouth 19 is connected by circulating pump 21 with liquid-phase outlet 20.
Described scraper evaporator 10 at least comprises an entrance, also comprises and mends nitrogen mouth, be installed on feed opening 16 place, and feed opening 16 place increases mends nitrogen mouth, opens, carries out nitrogen protection use during system shutdown to system, ensure the stability of system during feed opening 16 blanking.
Described liquid tremie pipe 9 horizontal segment is the shortest, and liquid tremie pipe 9 vertical section and tower body 4 keep the shortest safe distance, and distance range is 400 ~ 800mm.Described scraper plate 15 arranges in the shape of a spiral.Be separated by 120 ° between described scraper plate and scraper plate, between adjacent often group scraper plate, rotate 60 ° successively.
Heating medium temperature in scraper evaporator 10 external heating jacket 13 is elevated to 200-280 DEG C, then Produced Liquid in the middle part of tower is entered scraper evaporator 10, and helical flight 15 is opened, and pushes solid material slag to deslagging feed opening 16.
Described scraper plate rectifying column carries out the refining technique of adiponitrile as shown in Figure 2, thick adiponitrile upstream device come introduces scraper plate rectifying column 3, along with the carrying out of rectifying, on column plate, material concentration there occurs change, have solid matter crystallization on board-like layer 6 column plate, thick adiponitrile material liquid is introduced easy crystallization column plate, and the material of this column plate is caused scraper evaporator 10 by liquid tremie pipe 9, by rotary slagging coutrol system, solid matter is entered feed opening 16, the gas phase formed in tapping process enters upper strata and continues rectifying, and use circulating pump 21 to make to set up Matter Transfer at the bottom of tower and between board-like layer 6 by Matter Transfer mouth 19 and liquid-phase outlet 20, in operation, at scraper plate rectifying column 3 top extraction high-purity adiponitrile product, the adiponitrile product containing a small amount of heavy constituent is drawn bottom scraper plate rectifying column 3, enter subordinate's rectifying column through buffering and carry out rectifying, the high-purity adiponitrile product of subordinate's rectifying column top extraction, extraction heavy constituent in bottom reclaims.
The operating pressure of described scraper evaporator 10 is 1KPaA-50KPaA, and operating temperature is 200-280 DEG C, and rotating speed is 60 ~ 240r/min.
Open during feed opening 16 blanking and mend nitrogen mouth, nitrogen protection is carried out to system.
Embodiment 1:
Thick adiponitrile product A before rectifying contains adiponitrile 90%, heavy constituent 9%, can separate out solid impurity 1%.Because the material initial concentration entering scraper plate rectifying column 3 is low, after material enters scraper plate rectifying column 3, along with steaming of adiponitrile, the separated out solid impurity concentration be dissolved in adiponitrile solution rises, control the temperature of column plate point for measuring temperature at 160 ~ 180 DEG C, corresponding, the temperature at scraper evaporator 10 place is 250 ~ 280 DEG C, system pressure is 3KPaA, and scraper evaporator 10 rotating speed is 60 ~ 100r/min.The smart adiponitrile product B of more than 99.9% can be obtained from scraper plate rectifying column 3 tower top in embodiment 1, and not containing separating out solid impurity at the bottom of scraper plate rectifying column 3 tower, obtain the smart adiponitrile product B of 98.6% from No. two rectifying column 2 tower tops, at the bottom of tower, heavy constituent C separates out without solid matter.
Embodiment 2:
Thick adiponitrile product A before rectifying contains adiponitrile 50%, heavy constituent 45%, can separate out solid impurity 5%.Because the material initial concentration entering scraper plate rectifying column 3 is low, after material enters scraper plate rectifying column 3, along with steaming of adiponitrile, the separated out solid impurity concentration be dissolved in adiponitrile solution rises, control the temperature of column plate point for measuring temperature at 160 ~ 180 DEG C, corresponding, the temperature at scraper evaporator 10 place is 240 ~ 260 DEG C, system pressure is 1KPaA, and scraper evaporator 10 rotating speed is 100 ~ 150r/min.The smart adiponitrile product B of more than 99.9% can be obtained from scraper plate rectifying column 3 tower top in embodiment 2, and not containing separating out solid impurity at the bottom of scraper plate rectifying column 3 tower, obtain the smart adiponitrile product B of 98.0% from No. two rectifying column 2 tower tops, at the bottom of tower, heavy constituent C separates out without solid matter.
Embodiment 3:
Thick adiponitrile product A before rectifying contains adiponitrile 90%, heavy constituent 9%, can separate out solid impurity 1%.Because the material initial concentration entering scraper plate rectifying column 3 is low, after material enters scraper plate rectifying column 3, along with steaming of adiponitrile, the separated out solid impurity concentration be dissolved in adiponitrile solution rises, control the temperature of column plate point for measuring temperature at 160 ~ 180 DEG C, corresponding, the temperature at scraper evaporator 10 place is 200 ~ 240 DEG C, system pressure is 1KPaA, and scraper evaporator 10 rotating speed is 150 ~ 200r/min.The smart adiponitrile product B of more than 99.9% can be obtained from scraper plate rectifying column 3 tower top in embodiment 3, and not containing separating out solid impurity at the bottom of scraper plate rectifying column 3 tower, obtain the smart adiponitrile product B of 98.0% from No. two rectifying column 2 tower tops, at the bottom of tower, heavy constituent C separates out without solid matter.
Embodiment 4:
Thick adiponitrile product A before rectifying contains adiponitrile 80%, heavy constituent 19%, can separate out solid impurity 1%.Because the material initial concentration entering scraper plate rectifying column 3 is low, after material enters scraper plate rectifying column 3, along with steaming of adiponitrile, the separated out solid impurity concentration be dissolved in adiponitrile solution rises, control the temperature of column plate point for measuring temperature at 160 ~ 180 DEG C, corresponding, the temperature at scraper evaporator 10 place is 280 DEG C, system pressure is 50KPaA, and scraper evaporator 10 rotating speed is 200 ~ 240r/min.The smart adiponitrile product B of more than 99.9% can be obtained from scraper plate rectifying column 3 tower top in embodiment 2, and not containing separating out solid impurity at the bottom of scraper plate rectifying column 3 tower, obtain the smart adiponitrile product B of 98.0% from No. two rectifying column 2 tower tops, at the bottom of tower, heavy constituent C separates out without solid matter.
Equipment and technology method of the present invention is described by specific embodiment.Those skilled in the art can use for reference the links such as the suitable feed change of content of the present invention, process conditions, apparatus assembly and realize other object corresponding, its relevant change does not all depart from content of the present invention, all similar replacements and change will become apparent to those skilled in the art that and be all deemed to be included within scope of the present invention.
Claims (10)
1., for the scraper plate rectifying column that adiponitrile is refining, it is characterized in that, comprise tower body, liquid tremie pipe, packing layer, board-like layer is comprised in described tower body, packing layer is above board-like layer, and material inlet is in the packing layer bottom of described tower body, and gaseous phase outlet is at the top of tower body, last block column plate of described board-like layer is drawn liquid tremie pipe vertically downward, described scraper plate rectifying column also comprises scraper evaporator, Matter Transfer mouth, liquid-phase outlet, circulating pump, described scraper evaporator comprises transmission device, evaporator tube, external heating jacket, scraper plate bracing ring, scraper plate, feed opening, solid baffle, concave shape gas baffle, described evaporator tube is seal-installed on tower body outside, below last block column plate of board-like layer, evaporator tube lower end arranges feed opening, feed opening adopts blind plate sealing, external overall installs external heating jacket, scraper plate is fixed on scraper plate bracing ring, be installed on evaporator tube inside, and be connected with the transmission device of outside, solid baffle is installed on evaporator tube and tower body junction inner lower, concave shape gas baffle is installed on evaporator tube and tower body junction upper inside, described Matter Transfer mouth is outside at board-like layer position tower body, and liquid-phase outlet is bottom tower body, and Matter Transfer mouth is connected by circulating pump with liquid-phase outlet.
2. a kind of scraper plate rectifying column refining for adiponitrile according to claim 1, it is characterized in that, described scraper evaporator at least comprises an entrance, is installed on tower body outside with horizontal type structure.
3. a kind of scraper plate rectifying column refining for adiponitrile according to claim 1, it is characterized in that, described scraper plate rectifying column also comprises mends nitrogen mouth, mends nitrogen mouth and is installed on feed opening place.
4. a kind of scraper plate rectifying column refining for adiponitrile according to claim 1, it is characterized in that, described liquid tremie pipe horizontal segment is the shortest, and liquid tremie pipe vertical section and tower body keep the shortest safe distance.
5. a kind of scraper plate rectifying column refining for adiponitrile according to claim 1, it is characterized in that, described scraper plate arranges in the shape of a spiral.
6. a kind of scraper plate rectifying column refining for adiponitrile according to claim 1, is characterized in that, be separated by 120 ° between described scraper plate and scraper plate, rotate 60 ° successively between adjacent often group scraper plate.
7. use scraper plate rectifying column described in claim 1 to carry out the refining technique of adiponitrile, it is characterized in that, thick adiponitrile upstream device come introduces scraper plate rectifying column, along with the carrying out of rectifying, on column plate, material concentration there occurs change, have solid matter crystallization on board-like layer column plate, thick adiponitrile material liquid is introduced easy crystallization column plate, and the material of this column plate is caused scraper evaporator by liquid tremie pipe, by the running of scraper evaporator, solid matter is entered feed opening, the gas phase formed in tapping process enters upper strata and continues rectifying, and use circulating pump to make to set up Matter Transfer at the bottom of tower and between board-like layer by Matter Transfer mouth and liquid-phase outlet, in operation, at scraper plate rectifying column top extraction high-purity adiponitrile product, scraper plate rectifier bottoms draws the adiponitrile product containing a small amount of heavy constituent, enter subordinate's rectifying column through buffering and carry out rectifying, the high-purity adiponitrile product of subordinate's rectifying column top extraction, extraction heavy constituent in bottom reclaims.
8. adiponitrile process for refining according to claim 7, it is characterized in that, the operating pressure of described scraper evaporator is 1KPaA-50KPaA.
9. adiponitrile process for refining according to claim 7, it is characterized in that, the operating temperature of described scraper evaporator is 200-280 DEG C, and rotating speed is 60 ~ 240r/min.
10. adiponitrile process for refining according to claim 7, is characterized in that, opens and mends nitrogen mouth, carry out nitrogen protection to system during feed opening blanking.
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Cited By (1)
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CN105797419A (en) * | 2016-05-11 | 2016-07-27 | 中国天辰工程有限公司 | Coking corrosion inhibitor for adiponitrile rectification device |
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