CN103977591A - Scraper rectifying column and process for refining adiponitrile - Google Patents
Scraper rectifying column and process for refining adiponitrile Download PDFInfo
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- CN103977591A CN103977591A CN201410236384.7A CN201410236384A CN103977591A CN 103977591 A CN103977591 A CN 103977591A CN 201410236384 A CN201410236384 A CN 201410236384A CN 103977591 A CN103977591 A CN 103977591A
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Abstract
The invention provides a scraper rectifying column and process for refining adiponitrile. The scraper rectifying column comprises a column body and a liquid blanking pipe, as well as a scraper evaporator, a material circulating hole, a liquid phase outlet and a circulating pump, wherein the tower body internally comprises a filler layer and a plate type layer; the scraper evaporator is mounted at the outer part of the column body in a sealing manner and below the last column plate of the plate type layer; the material circulating hole is formed in the plate type layer and outside the column body; the liquid phase outlet connected with the material circulating hole through the circulating pump is formed in the bottom part of the tower body. The scraper rectifying column and process for refining adiponitrile have the beneficial effects that a special column structure is adopted, adiponitrile is separated from other dissolved foreign matters by adopting a crystal separation method, and thus the adiponitrile product can be recovered to the maximum while high-purity adiponitrile products are obtained, the problem of coking and blocking at the bottom part of a traditional rectifying column can be effectively solved, the purity of the product is improved, and the adiponitrile products can be recovered to the maximum.
Description
Technical field
The invention belongs to Chemical Manufacture process equipment technical field, relate to particularly a kind of for the refining scraper plate rectifying column of adiponitrile and adiponitrile process for refining.
Background technology
The rectifying column using in existing production adiponitrile process comprises tower body, in tower body, there are some layers of column plate, products export is arranged at tower body top, there is feed(raw material)inlet tower body middle and upper part, on the tower body of top, feed(raw material)inlet, there is reflux inlet, at the bottom of tower, there are Matter Transfer heating outlet and Matter Transfer to heat entrance, at the bottom of tower, also have heavy constituent outlet, between the ground floor column plate (being basecoat column plate) of tower body and second layer column plate, be provided with circulation heavy constituent entrance.Shortcoming is: when production, partial material at the bottom of tower is delivered to ground floor column plate to circulate, because the material composition of ground floor column plate changes, heavy constituent increases, cause the heavy constituent on each layer of column plate above also to change, finally make the heavy constituent content in overhead increase, poor product quality.
In adiponitrile production process, the separation and purification of adiponitrile adopts the mode of rectifying to carry out more, and the operation of adiponitrile treating column is very difficult, the easy coking of adiponitrile treating column materials at bottom of tower, at the bottom of crystallization goes out the auxiliary agent obstruction tower in product, heat exchanger affects normal production process.The thin film evaporation of existing heat sensitive material and the coupled system of distillation system, at the bottom of rectifying tower without circulating pump, if misoperation still can cause the coking of materials at bottom of tower and separating out 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 is processed, still can produce entrainment, separation degree is affected.As shown in Figure 1, refining to adiponitrile with traditional process, wherein the component at the bottom of rectifying column 1 tower need strictly be controlled, and not so in adiponitrile, dissolved impurity can be because at the bottom of misoperation obstruction 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, must contain non-crystallizable separating out at the bottom of the tower of No. two rectifying columns 2 of a certain amount of adiponitrile composition guarantee, has caused the waste of adiponitrile.
Summary of the invention
The present invention is for better solving the problems of the technologies described above, adopt scraper plate rectifying column, remove the solid impurity being dissolved in adiponitrile by the method for crystallization, and solid eliminating reaction being generated by rotary slagging coutrol system, can separate and obtain highly purified adiponitrile product.The concrete technical scheme adopting is as follows:
For the refining scraper plate rectifying column of adiponitrile, comprise tower body, liquid tremie pipe, in described tower body, comprise packing layer, board-like layer, 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, on described board-like last piece column plate of layer, draw 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 heat chuck, scraper plate bracing ring, scraper plate, feed opening, solid baffle, concave shape gas baffle, described evaporator tube is seal-installed on tower body outside, last piece column plate below of board-like layer, evaporator tube lower end arranges feed opening, feed opening adopts blind plate sealing, external overall is installed external heat chuck, scraper plate is fixed on scraper plate bracing ring, be installed on evaporator tube inside, and be connected with outside transmission device, 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 in board-like layer tower body outside, position, and liquid-phase outlet is in tower body bottom, and Matter Transfer mouth is connected by circulating pump with liquid-phase outlet.
At the bottom of traditional scraper plate rectifying column coupled system tower, do not set up circulation, easily the retention time of material of coking and polymerization is long, liquid-phase outlet and Matter Transfer mouth at the bottom of tower is set and sets up after circulation, has reduced 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, when feed opening blanking, opens; when system shutdown, system is carried out to nitrogen protection use, 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 is arranged in the shape of a spiral.Between described scraper plate and scraper plate, be separated by 120 °, between every group of adjacent scraper plate, rotate successively 60 °.
The full chuck of evaporator tube, evaporator tube and tower body part place increase concave shape gas baffle; The built-in solid baffle of evaporator tube; Evaporator tube rotary slagging coutrol feed opening place also needs the protection of external heat chuck, and feed opening adopts blind plate sealing.Heat medium temperature in scraper evaporator external heat chuck is elevated to 200-280 DEG C, then tower middle part Produced Liquid is entered to scraper evaporator, and helical flight is opened, and pushes solid material slag to deslagging feed opening.
Use described scraper plate rectifying column to carry out the refining technique of adiponitrile, the thick adiponitrile that upstream device is come is introduced scraper plate rectifying column, along with the carrying out of rectifying, on column plate there is variation in material concentration, have solid matter crystallization on board-like layer column plate, thick adiponitrile material liquid is introduced to easy crystallization column plate, and the material of this column plate is caused to scraper evaporator by liquid tremie pipe, by rotary slagging coutrol system, solid matter is entered to feed opening, the gas phase forming in tapping process enters upper strata and continues rectifying, and set up Matter Transfer at the bottom of using circulating pump to make tower by Matter Transfer mouth and liquid-phase outlet with between board-like layer, in operating process, at scraper plate rectifying column top extraction high-purity adiponitrile product, scraper plate rectifier bottoms is drawn 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.
When feed opening blanking, open and mend nitrogen mouth, system is carried out to nitrogen protection.
The present invention is different from traditional thin film evaporator, by traditional vertical horizontal scraper evaporator that made into, and be provided with gas and solid baffle at scraper evaporator and rectifying column tower body junction, the solid producing in production process is separated thoroughly with adiponitrile, entrainment has effectively been avoided in arranging of gas baffle, by rotary slagging coutrol system, the solid impurity composition in adiponitrile is removed, at the bottom of having avoided the stage of rectification crystallization impurity obstruction rectifying tower in adiponitrile product purification purification process, filler and reboiler at the bottom of tower are effectively protected, and increase circulating pump at the bottom of scraper plate evaporating column tower, make containing adiponitrile Matter Transfer, the reliability and stability of operation are increased, reclaim to greatest extent adiponitrile product 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 separate with other dissolved impurities adiponitrile, when obtaining highly purified adiponitrile product, reclaimed to greatest extent adiponitrile product.The problem of effectively having avoided traditional rectifier bottoms coking and blocking, has improved product purity, has reclaimed to greatest extent adiponitrile product.
Brief description of the drawings
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 heat chuck, 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
For technological means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below the specific embodiment of the present invention is described further, but does not limit 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 refining scraper plate rectifying column of adiponitrile 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 bottoms of described tower body 4, and gaseous phase outlet 7 is at the top of tower body 4, on described board-like layer 6 last piece column plate, draw 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 heat chuck 13, scraper plate bracing ring 14, scraper plate 15, feed opening 16, solid baffle 17, concave shape gas baffle 18, described evaporator tube 12 is seal-installed on tower body 4 outsides, board-like layer 6 last piece column plate below, evaporator tube 12 lower ends arrange feed opening 16, feed opening 16 adopts blind plate sealing, external overall is installed external heat chuck 13, scraper plate 15 is fixed on scraper plate bracing ring 14, be installed on evaporator tube 12 inside, and be connected with outside transmission device 11, 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 in board-like layer 6 position tower body 4 outside, and liquid-phase outlet 20 is in tower body 4 bottoms, 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, is installed on feed opening 16 places, and feed opening 16 places increase mends nitrogen mouth, when feed opening 16 blanking, opens, and when system shutdown, system is carried out to nitrogen protection use, ensures the stability of system.
Described liquid tremie pipe 9 horizontal segments are the shortest, and liquid tremie pipe 9 vertical sections and tower body 4 keep the shortest safe distance, and distance range is 400～800mm.Described scraper plate 15 is arranged in the shape of a spiral.Between described scraper plate and scraper plate, be separated by 120 °, between every group of adjacent scraper plate, rotate successively 60 °.
Heat medium temperature in scraper evaporator 10 external heat chucks 13 is elevated to 200-280 DEG C, then tower middle part Produced Liquid is entered to 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, the thick adiponitrile that upstream device is come is introduced scraper plate rectifying column 3, along with the carrying out of rectifying, on column plate there is variation in material concentration, have solid matter crystallization on board-like layer 6 column plate, thick adiponitrile material liquid is introduced to easy crystallization column plate, and the material of this column plate is caused to scraper evaporator 10 by liquid tremie pipe 9, by rotary slagging coutrol system, solid matter is entered to feed opening 16, the gas phase forming in tapping process enters upper strata and continues rectifying, and set up Matter Transfer at the bottom of using circulating pump 21 to make tower by Matter Transfer mouth 19 and liquid-phase outlet 20 and between board-like layer 6, in operating process, at scraper plate rectifying column 3 top extraction high-purity adiponitrile products, the adiponitrile product containing a small amount of heavy constituent is drawn in scraper plate rectifying column 3 bottoms, 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.
When feed opening 16 blanking, open and mend nitrogen mouth, system is carried out to nitrogen protection.
Embodiment 1:
Thick adiponitrile product A before rectifying contains adiponitrile 90%, and heavy constituent 9%, can separate out solid impurity 1%.Low owing to entering the material initial concentration of scraper plate rectifying column 3, material enters after scraper plate rectifying column 3, along with steaming of adiponitrile, the separated out solid impurity concentration being 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 places is 250～280 DEG C, system pressure is 3KPaA, and scraper evaporator 10 rotating speeds are 60～100r/min.In embodiment 1, can obtain more than 99.9% smart adiponitrile product B from scraper plate rectifying column 3 tower tops, and do not contain and can separate out solid impurity at the bottom of scraper plate rectifying column 3 towers, obtain 98.6% smart adiponitrile product B 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%, and heavy constituent 45%, can separate out solid impurity 5%.Low owing to entering the material initial concentration of scraper plate rectifying column 3, material enters after scraper plate rectifying column 3, along with steaming of adiponitrile, the separated out solid impurity concentration being 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 places is 240～260 DEG C, system pressure is 1KPaA, and scraper evaporator 10 rotating speeds are 100～150r/min.In embodiment 2, can obtain more than 99.9% smart adiponitrile product B from scraper plate rectifying column 3 tower tops, and do not contain and can separate out solid impurity at the bottom of scraper plate rectifying column 3 towers, obtain 98.0% smart adiponitrile product B 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%, and heavy constituent 9%, can separate out solid impurity 1%.Low owing to entering the material initial concentration of scraper plate rectifying column 3, material enters after scraper plate rectifying column 3, along with steaming of adiponitrile, the separated out solid impurity concentration being 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 places is 200～240 DEG C, system pressure is 1KPaA, and scraper evaporator 10 rotating speeds are 150～200r/min.In embodiment 3, can obtain more than 99.9% smart adiponitrile product B from scraper plate rectifying column 3 tower tops, and do not contain and can separate out solid impurity at the bottom of scraper plate rectifying column 3 towers, obtain 98.0% smart adiponitrile product B 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%, and heavy constituent 19%, can separate out solid impurity 1%.Low owing to entering the material initial concentration of scraper plate rectifying column 3, material enters after scraper plate rectifying column 3, along with steaming of adiponitrile, the separated out solid impurity concentration being 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 places is 280 DEG C, system pressure is 50KPaA, and scraper evaporator 10 rotating speeds are 200～240r/min.In embodiment 2, can obtain more than 99.9% smart adiponitrile product B from scraper plate rectifying column 3 tower tops, and do not contain and can separate out solid impurity at the bottom of scraper plate rectifying column 3 towers, obtain 98.0% smart adiponitrile product B 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 content appropriate change raw material of the present invention, process conditions, apparatus assembly and realize corresponding other object, its relevant change does not all depart from content of the present invention, within all similar replacements and change will become apparent to those skilled in the art that and be all deemed to be included in scope of the present invention.
Claims (10)
1. for the refining scraper plate rectifying column of adiponitrile, 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, on described board-like last piece column plate of layer, draw liquid tremie pipe vertically downward, it is characterized in that, also comprise scraper evaporator, Matter Transfer mouth, liquid-phase outlet, circulating pump, described scraper evaporator comprises transmission device, evaporator tube, external heat chuck, scraper plate bracing ring, scraper plate, feed opening, described evaporator tube is seal-installed on tower body outside, last piece column plate below of board-like layer, evaporator tube lower end arranges feed opening, feed opening adopts blind plate sealing, external overall is installed external heat chuck, scraper plate is fixed on scraper plate bracing ring, be installed on evaporator tube inside, and be connected with outside transmission device, described Matter Transfer mouth is in board-like layer tower body outside, position, and liquid-phase outlet is in tower body bottom, and Matter Transfer mouth is connected by circulating pump with liquid-phase outlet.
2. a kind ofly according to claim 1 it is characterized in that for the refining scraper plate rectifying column of adiponitrile, described scraper evaporator at least comprises an entrance, is installed on tower body outside with horizontal type structure.
3. a kind ofly according to claim 1 it is characterized in that for the refining scraper plate rectifying column of adiponitrile, described scraper plate rectifying column also comprises mends nitrogen mouth, solid baffle, concave shape gas baffle, mends nitrogen mouth and is installed on feed opening place; Solid baffle is installed on evaporator tube and tower body junction inner lower, and concave shape gas baffle is installed on evaporator tube and tower body junction upper inside.
4. a kind ofly according to claim 1 it is characterized in that for the refining scraper plate rectifying column of adiponitrile, 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 ofly according to claim 1 it is characterized in that for the refining scraper plate rectifying column of adiponitrile, described scraper plate is arranged in the shape of a spiral.
6. a kind ofly according to claim 1 it is characterized in that for the refining scraper plate rectifying column of adiponitrile, between described scraper plate and scraper plate, be separated by 120 °, between every group of adjacent scraper plate, rotate successively 60 °.
7. described in right to use requirement 1, scraper plate rectifying column carries out the refining technique of adiponitrile, it is characterized in that, the thick adiponitrile that upstream device is come is introduced scraper plate rectifying column, along with the carrying out of rectifying, on column plate there is variation in material concentration, have solid matter crystallization on board-like layer column plate, thick adiponitrile material liquid is introduced to easy crystallization column plate, and the material of this column plate is caused to scraper evaporator by liquid tremie pipe, by rotary slagging coutrol system, solid matter is entered to feed opening, the gas phase forming in tapping process enters upper strata and continues rectifying, and set up Matter Transfer at the bottom of using circulating pump to make tower by Matter Transfer mouth and liquid-phase outlet with between board-like layer, in operating process, at scraper plate rectifying column top extraction high-purity adiponitrile product, scraper plate rectifier bottoms is drawn 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, is characterized in that, the operating pressure of described scraper evaporator is 1KPaA-50KPaA.
9. adiponitrile process for refining according to claim 7, 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, when feed opening blanking, opens and mends nitrogen mouth, and system is carried out to nitrogen protection.
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| CN201410236384.7A CN103977591B (en) | 2014-05-29 | 2014-05-29 | A kind of scraper plate rectifying column refining for adiponitrile and adiponitrile process for refining |
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| CN201410236384.7A CN103977591B (en) | 2014-05-29 | 2014-05-29 | A kind of scraper plate rectifying column refining for adiponitrile and adiponitrile process for refining |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537171A (en) * | 2016-06-28 | 2018-01-05 | 江苏新河农用化工有限公司 | A kind of isophthalodinitrile evaporator |
| CN109053492A (en) * | 2018-08-24 | 2018-12-21 | 中国化学赛鼎宁波工程有限公司 | A kind of adiponitrile rectifying and purifying system and its rectification and purification method |
| CN114288699A (en) * | 2021-12-02 | 2022-04-08 | 徐州砥研医药科技有限公司 | Rectification device for preparing benzene-containing medical intermediate and working method thereof |
| CN115212599A (en) * | 2022-08-10 | 2022-10-21 | 聊城鲁西聚酰胺新材料科技有限公司 | Material circulating system of cyclohexanone oxime rectifying tower reboiler |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105797419B (en) * | 2016-05-11 | 2018-01-26 | 中国天辰工程有限公司 | A kind of coking corrosion inhibiter for adiponitrile rectifier unit |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB792572A (en) * | 1953-08-12 | 1958-04-02 | Knapsack Ag | Process for the preparation of aliphatic ª‡-unsubstituted ª‡:ª‰-unsaturated carboxylic acids and their derivatives |
| US3153084A (en) * | 1960-09-08 | 1964-10-13 | Monsanto Co | Vaporization of adipic acid and reaction thereof with ammonia to produce adiponitrile |
| GB1015725A (en) * | 1962-03-01 | 1966-01-05 | Vitamins Ltd | Improvements in or relating to molecular fractionating stills |
| CN101676261A (en) * | 2008-09-19 | 2010-03-24 | 于网林 | Adiponitrile production technology |
| CN202705270U (en) * | 2012-09-05 | 2013-01-30 | 大庆凤颐化工科技有限公司 | Preparation device for azodiisobutyronitrile |
| CN102908793A (en) * | 2012-10-25 | 2013-02-06 | 浙江大学 | Horizontal type biaxial distillation apparatus suitable for continuous separation of viscous material series |
-
2014
- 2014-05-29 CN CN201410236384.7A patent/CN103977591B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB792572A (en) * | 1953-08-12 | 1958-04-02 | Knapsack Ag | Process for the preparation of aliphatic ª‡-unsubstituted ª‡:ª‰-unsaturated carboxylic acids and their derivatives |
| US3153084A (en) * | 1960-09-08 | 1964-10-13 | Monsanto Co | Vaporization of adipic acid and reaction thereof with ammonia to produce adiponitrile |
| GB1015725A (en) * | 1962-03-01 | 1966-01-05 | Vitamins Ltd | Improvements in or relating to molecular fractionating stills |
| CN101676261A (en) * | 2008-09-19 | 2010-03-24 | 于网林 | Adiponitrile production technology |
| CN202705270U (en) * | 2012-09-05 | 2013-01-30 | 大庆凤颐化工科技有限公司 | Preparation device for azodiisobutyronitrile |
| CN102908793A (en) * | 2012-10-25 | 2013-02-06 | 浙江大学 | Horizontal type biaxial distillation apparatus suitable for continuous separation of viscous material series |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537171A (en) * | 2016-06-28 | 2018-01-05 | 江苏新河农用化工有限公司 | A kind of isophthalodinitrile evaporator |
| CN109053492A (en) * | 2018-08-24 | 2018-12-21 | 中国化学赛鼎宁波工程有限公司 | A kind of adiponitrile rectifying and purifying system and its rectification and purification method |
| CN114288699A (en) * | 2021-12-02 | 2022-04-08 | 徐州砥研医药科技有限公司 | Rectification device for preparing benzene-containing medical intermediate and working method thereof |
| CN115212599A (en) * | 2022-08-10 | 2022-10-21 | 聊城鲁西聚酰胺新材料科技有限公司 | Material circulating system of cyclohexanone oxime rectifying tower reboiler |
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|---|---|
| CN103977591B (en) | 2015-10-28 |
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