CN204865839U - Nitrobenzene liquid -phase hydrogenatin system aniline reaction unit - Google Patents
Nitrobenzene liquid -phase hydrogenatin system aniline reaction unit Download PDFInfo
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Abstract
The utility model provides a nitrobenzene liquid -phase hydrogenatin system aniline reaction unit, includes following part: hydrogenation dominant reaction ware fluidized bed, the reaction liquid import bottom the fluidized bed is all continuous with the outer wall of fluidized bed with the gas access, the distributor of fluidized bed bottom and gas -liquid distributing plate all link to each other with fluidized bed bottom inner wall, the gas -liquid distribution sieve that sets up on the fluidized bed inner wall all links to each other with the fluidized bed inner wall, and so on. Force outer circulation system through setting up outside the fluidized bed, both can shift the heat that produces in the fluidized bed reactor, can carry out the compulsory conversion rate that mixes reaction, improvement nitrobenzene once more through the extrinsic cycle again.
Description
Technical field
The utility model belongs to petrochemical equipment hydrogen addition technology field, provides a kind of reaction unit of nitrobenzene liquid-phase hydrogenatin aniline.
Background technology
In By Catalytic Hydrogenation of Nitrobenzene aniline reaction, nitration reaction speed is fast, course of reaction is violent, reaction heat is up to 544kJ/mol, therefore how to design in the industrial production, select suitable hydrogenation reaction device, reaction heat can be removed in time to avoid hydrogenation side reaction on benzene nucleus, and keep catalyst activity, make full use of reaction heat simultaneously, reduce the key that energy consumption becomes nitration reaction.
The production process route of domestic current aniline mainly contains By Catalytic Hydrogenation of Nitrobenzene method, phenol ammoniation process.Wherein, By Catalytic Hydrogenation of Nitrobenzene method is the main method of industrial production aniline, comprises Fixed Bed Gas Phase catalytic hydrogenation, fluidized bed gas-phase catalytic hydrogenation and nitrobenzene liquid phase catalytic hydrogenation three kinds of techniques.Wherein fixed bed, fluid bed gas phase reaction process are by rear for nitrobenzene preheating vaporization and hydrogen hydrogenation reaction; Liquid-phase hydrogenatin process be after nitrobenzene is preheating to 90 ~ 150 DEG C in liquid form with hydrogen hydrogenation reaction.
Fixed Bed Gas Phase reactor, course of reaction is also controlled by hydrogen partial pressure, and hydrogen circulation amount is larger, and hydrogen-oil ratio reaches 20:1, causes energy consumption higher thus; Inside reactor adopts complicated Machine Design, and adopts built-in heat exchange component, limits the production capacity of single covering device, is up to 100,000 tons/year; Catalyst regeneration process must be stopped replacing, causes discontinuousization that device is produced.Because catalyst is fixed in reactor, in course of reaction, easily there is hot-spot and cause side reaction and cause the inactivation of catalyst thus.
Gas fluidized bed reactor, course of reaction is controlled by hydrogen partial pressure, and hydrogen circulation amount is large, and hydrogen-oil ratio reaches 9:1, causes energy consumption higher thus; Due to the parts such as reactive internal, filter, separator, heat exchanger of inside reactor complex distribution, the production capacity that result in single covering device is up to 100,000 tons/year; Catalyst regeneration process is long for down time, and needs increase auxiliary equipment to carry out reducing/regenerating to catalyst, thus affects the continuous prodution of device.
Compared to Fixed Bed Gas Phase reactor, gas fluidized bed reactor adopts catalyst to mix also hydrogenation reaction with reactant fluidisation, solves the problem of side reaction that inside reactor hot-spot causes and catalysqt deactivation.But still there is the production capacity restriction needing to carry out catalyst regeneration and cause due to the impact of internals complexity.
For this reason, have developed reactor and the hydrogenation technique of nitrobenzene liquid-phase hydrogenatin aniline abroad.Nitrobenzene to enter reactor and catalyst together with 90 ~ 150 DEG C of hydrogen after preheating liquid phase state is fluidization mix through being preheating to, and fully reacts.
Fluid bed liquid phase hydrogenation reactor, course of reaction is by mass transport limitation, and hydrogen is excessive is 8% ~ 10% of theoretical consumption, thus reduces the energy consumption in production process; Inside reactor adopts simple sieve-board type component, and adopts external waste heat boiler transfer reaction to produce a large amount of reaction heat, improves the operating flexibility of reactor, makes the highest production capacity of single cover reaction unit reach 180,000 tons/year; Package unit catalyst can continuous supplementation and do not need shut-down operation.Inside reactor reaction temperature is low, and side reaction is few, and catalyst loading is high, and the life-span is long, and equipment capacity is large.
Weak point is that product must be separated with catalyst, and the operating maintenance cost of later separation equipment is high, it is crucial that the device of current domestic liquid-phase hydrogenatin aniline used and technique all derive from foreign patent technology, introduce and operating cost high.
Therefore, the present invention is directed to domestic existing aniline production by gas phase hydrogenation of nitrobenzene technology and external liquid-phase hydrogenatin aniline technology, design and a kind of novel nitrobenzene liquid-phase hydrogenatin reaction unit is provided.
Summary of the invention
The object of the invention is to, design and provide a kind of for nitrobenzene liquid-phase hydrogenatin aniline reaction device, to realize, nitrobenzene is quick under liquid phase state, highly effective hydrogenation reaction prepares aniline.By this reactor can make thick nitrobenzene without refining and edulcoration matter direct hydrogenation, thus reduce energy consumption in nitrobenzene hydrogenation, material consumption; Improve the operating flexibility of single cover reaction unit, reduce reaction unit running cost; Reduce the production cost of aniline, improve the competitiveness of domestic aniline on national market.
Technical solution of the present invention is as follows: nitrobenzene liquid-phase hydrogenatin Aniline Unit, is characterized in that, this device comprises as lower component:
(1) hydrogenation main reactor fluid bed (A).
(2) reactant liquors import (a) being arranged at fluid bed (A) bottom are all connected with the outer wall of fluid bed (A) with gas access (b).
(3) distributors (1) being arranged at fluid bed (A) bottom are all connected with fluid bed (A) bottom interior wall with gas-liquid distribution grid (2).
(4) one or more gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) be arranged on fluid bed (A) inwall is all connected with fluid bed (A) inwall.
(5) be one or morely distributed in the inner gas-liquid mixed reaction zone (4) (4a, 4b, 4c...) of fluid bed (A) and be uniformly distributed in two distribution of gas sieve plates (3).
(6) one or more be distributed in fluid bed (A) internal heat device (5) (5a, 5b, 5c...) be distributed in fluid bed (A) middle part, top gas-liquid mixed reaction zone (4) in and be all connected with fluid bed (A) inwall.
(7) circulation fluids being distributed in fluid bed (A) top export (c); Liquid-phase product aniline, water out (d) homogeneously fluidized bed (A) outer wall are connected.
(8) internal cyclone separators (7) being arranged at fluid bed (A) top are connected with fluid bed (A) top inner wall; A gaseous phase outlet (h) being arranged at fluid bed (A) top is connected with fluid bed (A) outer wall, and communicates with internal cyclone separators (7).
(9) oil bath heating jackets (8) being arranged at fluid bed (A) are connected with fluid bed (A) outer wall, and are provided with oil bath import (e); Oil bath outlet (e-1).
(10) catalyst being arranged at fluid bed (A) top add entrance (f) and are connected with fluid bed (A) roof; A setting is connected with fluid bed (A) upper wall with the catalyst mozzle (10) on fluid bed (A) top, and adds entrance (f) with catalyst and communicate.
(11) one are arranged at the outside forced circulation system (B) of fluid bed (A) and comprise heat-exchanger rig (6) and form an Inner eycle reaction system with forced circulation pump (9) and fluid bed (A).
Further, branch's device (1) of the fluidized-bed bottom of described device is pipe distributor.
The gas-liquid distribution grid (2) of described fluidized-bed bottom is orifice-plate type distribution grid, and distribution grid percent opening selects 3% ~ 15%, preferably 6% ~ 12%.
Gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) of described fluid bed inside is porous type sieve plate, and sieve-plate aperture ratio selects 5% ~ 20%, preferably 8% ~ 15%.
Between inner gas-liquid distribution sieve plate (3) of described fluid bed, mounting distance is 10% ~ 100% of reactor diameter.
Internal heat device (5) installation site of described fluid bed inside is between two gas-liquids distribution sieve plate (3) (3a, 3b, 3c...), and installation quantity is 10% ~ 90% of gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) quantity.
Described fluid bed top gas-solid separating device used is one-level or secondary internal cyclone separators.
Described device also comprises a set of gas and liquid feed line, and gas feed system is connected with fluidized-bed bottom gas access (b) through pipeline, and liquid feed line is connected with fluidized-bed bottom liquid inlet (a) through pipeline.
Described device also comprises a set of external circulating system B, and this system exports (c) through pipeline and fluid bed upper liquid and is connected, and circulation fluid is connected with fluidized-bed bottom liquid inlet (a) through pipeline, thus forms a set of external circulating system completed.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment of the present invention device.
In figure, (1) distributor; (2) gas-liquid distribution grid; (3) gas-liquid distribution sieve plate; (4) gas-liquid mixed reaction zone; (5) internal heat device; (6) heat-exchanger rig; (7) internal cyclone separators; (8) oil bath heating jacket; (9) forced circulation pump; (10) catalyst mozzle.
The import of (a) reactant liquor; (b) gas access; C () circulation fluid exports; (d) liquid-phase product aniline, water out; (h) gaseous phase outlet; (e) oil bath import; (e-1) oil bath outlet; F () catalyst adds entrance.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in detail.
Embodiment: the present embodiment device as shown in Figure 1, comprises as lower component:
(a) hydrogenation main reactor fluid bed (A).
B reactant liquor import (a) that () is arranged at fluid bed (A) bottom is all connected with the outer wall of fluid bed (A) with gas access (b).
C branch's device (1) that () is arranged at fluid bed (A) bottom is all connected with fluid bed (A) bottom interior wall with gas-liquid distribution grid (2).
D () one or more gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) be arranged on fluid bed (A) inwall is all connected with fluid bed (A) inwall.
E () one or more is distributed in the inner gas-liquid mixed reaction zone (4) (4a, 4b, 4c...) of fluid bed (A) and is uniformly distributed in two distribution of gas sieve plates (3).
F () one or more is distributed in fluid bed (A) internal heat device (5) (5a, 5b, 5c...) and is distributed in the gas-liquid mixed reaction zone (4) on fluid bed (A) middle part, top and is all connected with fluid bed (A) inwall.
G () is distributed in circulation fluid outlet (c) on fluid bed (A) top; Liquid-phase product aniline, water out (d) homogeneously fluidized bed (A) outer wall are connected.
H internal cyclone separators (7) that () is arranged at fluid bed (A) top is connected with fluid bed (A) top inner wall; A gaseous phase outlet (h) being arranged at fluid bed (A) top is connected with fluid bed (A) outer wall, and communicates with internal cyclone separators (7).
(i) an oil bath heating jacket (8) being arranged at fluid bed (A) is connected with fluid bed (A) outer wall, and is provided with oil bath import (e); Oil bath outlet (e-1).
J catalyst that () is arranged at fluid bed (A) top adds entrance (f) and is connected with fluid bed (A) roof; A setting is connected with fluid bed (A) upper wall with the catalyst mozzle (10) on fluid bed (A) top, and adds entrance (f) with catalyst and communicate.
K () is arranged at the outside forced circulation system (B) of fluid bed (A) and comprises heat-exchanger rig (6) and form an Inner eycle reaction system with forced circulation pump (9) and fluid bed (A).
The present embodiment device designs mainly in nitrobenzene liquid-phase hydrogenatin reaction aniline processed, and using product aniline as reaction dissolvent, nitrobenzene is as reactant.
Hydrogen gas system is had to be connected with fluid bed (A) gas access (b) in fluid bed (A) bottom; Liquid phase nitrobenzene is had to be connected with fluid bed (A) reactant liquor import (a) with aniline feed system.In order to ensure the conversion ratio of nitrobenzene in fluidized-bed reactor inside, nitrobenzene and enter fluid bed (A) reactant liquor import (a) to 70 DEG C ~ 150 DEG C as the preheater heat exchange of aniline in liquid phase feeding system of solvent, can control nitro phenenyl concentration in 5% ~ 100% charging under the prerequisite ensureing nitrobenzene conversion rate; Hydrogen through gas handling system be preheating to 70 DEG C ~ 120 DEG C laggard enter fluid bed (A) gas access (b), hydrogen feed amount controls excessive 8% ~ 10%, under ensureing that the conversion ratio of nitrobenzene reaches the prerequisite of 100%, reduces hydrogen circulating consumption, material consumption.
The present embodiment fully mixes and hydrogenation reaction in the reactor in order to realize hydrogen and nitrobenzene.Branch's device (1) of bottom is set in fluid bed (A) bottom, gas and nitrobenzene through branch's device (1) mix disperse laggard enter gas distribution grid (2) bottom fluid bed (A) again disperse to mix.In order to ensure mixed effect, gas distribution grid (2) is provided with the highdensity gas distribution holes with special construction.
The present embodiment also segmentation interpolation gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) in fluid bed (A), thus formed between gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) multistage gas-liquid mixed reaction zone (4) (4a, 4b, 4c...), nitrobenzene and hydrogen are through multistage gas-liquid mixed reaction zone (4) (4a, 4b, 4c...) fully hybrid reaction, thus nitrobenzene reaches 100% conversion.
The present embodiment also segmentation interpolation internal heat device (5) (5a, 5b, 5c...) in fluid bed (A), transfer of heat can carried out whenever necessary to fluid bed (A) inside, thus ensure fluid bed (A) internal reaction temperature even, avoid because hot-spot causes the generation of side reaction.
The present embodiment also arranges the gaseous phase outlet (h) at top on fluid bed (A) top, liquid-phase product aniline, water out (d), can change product extraction mode by these two outlets is the extraction of full gas phase aniline, full liquid phase aniline extraction or gas phase liquid phase aniline mixing extraction.Full gas phase extraction temperature controls at 230 DEG C ~ 250 DEG C, Stress control is at 1.5MPa ~ 2.0Mpa, in order to ensure that product aniline can with full gas phase extraction, on fluid bed (A) top, oil bath heating jacket (8) is set, heating oil bath adopts reflux type to enter from oil bath import (e), derives after heat exchange from oil bath outlet (e-1); Simultaneously, internal cyclone separators (7) is set on fluid bed (A) top and is separated the fine catalyst carried secretly in gaseous products, internal cyclone separators (7) adopts three grades of inward turnings to be separated, can ensure that total efficiency of separation is more than 99.95%, the gas phase aniline of entrained catalyst and water enter follow-up heat exchange from gaseous phase outlet (h) extraction after internal cyclone separators (7), cooling, water are separated, aniline is refined.
The present embodiment arranges catalyst at fluid bed (A) top and adds entrance (f), through the water conservancy diversion of catalyst mozzle (10), when system is driven in 2% ~ 5%(wt) ratio is disposable adds catalyst.
The present embodiment, in fluid bed (A) arranged outside external circulating system (B), exports (c) with the circulation fluid on fluid bed (A) top and is communicated with, and under the effect of forced circulation pump (9), forms an internal circulation system with fluid bed (A).This circulatory system can form hybrid reaction again by forced circulation in fluid bed (A), improves the conversion ratio of nitrobenzene; The reaction heat of fluid bed (A) can carry out heat exchange cooling by the heat-exchanger rig (6) be connected with external circulating system (B), to control fluid bed (A) intrasystem temperature stabilization simultaneously.
Claims (9)
1. a nitrobenzene liquid-phase hydrogenatin Aniline Unit, is characterized in that, this device comprises as lower component:
(1) hydrogenation main reactor fluid bed (A);
(2) reactant liquors import (a) being arranged at fluid bed (A) bottom are all connected with the outer wall of fluid bed (A) with gas access (b);
(3) distributors (1) being arranged at fluid bed (A) bottom are all connected with fluid bed (A) bottom interior wall with gas-liquid distribution grid (2);
(4) one or more gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) be arranged on fluid bed (A) inwall is all connected with fluid bed (A) inwall;
(5) be one or morely distributed in the inner gas-liquid mixed reaction zone (4) (4a, 4b, 4c...) of fluid bed (A) and be uniformly distributed in two distribution of gas sieve plates (3);
(6) one or more be distributed in fluid bed (A) internal heat device (5) (5a, 5b, 5c...) be distributed in fluid bed (A) middle part, top gas-liquid mixed reaction zone (4) in and be all connected with fluid bed (A) inwall;
(7) circulation fluids being distributed in fluid bed (A) top export (c); Liquid-phase product aniline, water out (d) homogeneously fluidized bed (A) outer wall are connected;
(8) internal cyclone separators (7) being arranged at fluid bed (A) top are connected with fluid bed (A) top inner wall; A gaseous phase outlet (h) being arranged at fluid bed (A) top is connected with fluid bed (A) outer wall, and communicates with internal cyclone separators (7);
(9) oil bath heating jackets (8) being arranged at fluid bed (A) are connected with fluid bed (A) outer wall, and are provided with oil bath import (e); Oil bath outlet (e-1);
(10) catalyst being arranged at fluid bed (A) top add entrance (f) and are connected with fluid bed (A) roof; A setting is connected with fluid bed (A) upper wall with the catalyst mozzle (10) on fluid bed (A) top, and adds entrance (f) with catalyst and communicate;
(11) one are arranged at the outside forced circulation system (B) of fluid bed (A) and comprise heat-exchanger rig (6) and form an Inner eycle reaction system with forced circulation pump (9) and fluid bed (A).
2. device according to claim 1, is characterized in that: branch's device (1) of described fluidized-bed bottom is pipe distributor.
3. device according to claim 1, is characterized in that: the gas-liquid distribution grid (2) of described fluidized-bed bottom is orifice-plate type distribution grid, and distribution grid percent opening selects 3% ~ 15%.
4. device according to claim 1, is characterized in that: gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) of described fluid bed inside is porous type sieve plate, and sieve-plate aperture ratio selects 5% ~ 20%.
5. device according to claim 1, is characterized in that: between inner gas-liquid distribution sieve plate (3) of described fluid bed, mounting distance is 10% ~ 100% of reactor diameter.
6. device according to claim 1, it is characterized in that: internal heat device (5) installation site of described fluid bed inside is between two gas-liquids distribution sieve plate (3) (3a, 3b, 3c...), installation quantity is 10% ~ 90% of gas-liquid distribution sieve plate (3) (3a, 3b, 3c...) quantity.
7. device according to claim 1, is characterized in that: described fluid bed top gas-solid separating device used is one-level or secondary internal cyclone separators.
8. device according to claim 1, it is characterized in that: this device also comprises a set of gas and liquid feed line, gas feed system is connected with fluidized-bed bottom gas access (b) through pipeline, and liquid feed line is connected with fluidized-bed bottom liquid inlet (a) through pipeline.
9. device according to claim 1, it is characterized in that: the forced circulation system (B) of described outside exports (c) through pipeline and fluid bed upper liquid and is connected, circulation fluid is connected with fluidized-bed bottom liquid inlet (a) through pipeline, thus forms the external circulating system of complete set.
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| CN109663546A (en) * | 2019-02-21 | 2019-04-23 | 南京科技职业学院 | A kind of antifebrin synthesis special purpose reactor |
| CN110893333A (en) * | 2019-12-19 | 2020-03-20 | 靖江神驹容器制造有限公司 | O-chlorobenzonitrile fluidized bed reactor |
| WO2020078414A1 (en) * | 2018-10-17 | 2020-04-23 | 中国石油化工股份有限公司 | Di-trapezoidal component, fluidization device, and hydrogenation method for nitro compound |
| CN111054280A (en) * | 2018-10-17 | 2020-04-24 | 中国石油化工股份有限公司 | Reaction device and reaction method for preparing aniline by hydrogenation of multi-zone nitrobenzene |
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| CN108299210A (en) * | 2018-03-21 | 2018-07-20 | 江苏安邦电化有限公司 | A kind of ortho-aminotoluene crude product piece-rate system and technological process |
| JP2022512755A (en) * | 2018-10-17 | 2022-02-07 | 中国石油化工股▲ふん▼有限公司 | Hydrogenation reaction process of double trapezoidal structural members, fluidizers and nitro compounds |
| WO2020078414A1 (en) * | 2018-10-17 | 2020-04-23 | 中国石油化工股份有限公司 | Di-trapezoidal component, fluidization device, and hydrogenation method for nitro compound |
| CN111054280A (en) * | 2018-10-17 | 2020-04-24 | 中国石油化工股份有限公司 | Reaction device and reaction method for preparing aniline by hydrogenation of multi-zone nitrobenzene |
| CN111054280B (en) * | 2018-10-17 | 2022-04-01 | 中国石油化工股份有限公司 | Reaction device and reaction method for preparing aniline by hydrogenation of multi-zone nitrobenzene |
| EP3868465A4 (en) * | 2018-10-17 | 2022-06-15 | China Petroleum & Chemical Corporation | Di-trapezoidal component, fluidization device, and hydrogenation method for nitro compound |
| JP7330269B2 (en) | 2018-10-17 | 2023-08-21 | 中国石油化工股▲ふん▼有限公司 | Double Trapezoidal Structural Member, Fluid Apparatus and Hydrogenation Process of Nitro Compounds |
| RU2802870C2 (en) * | 2018-10-17 | 2023-09-05 | Чайна Петролиум & Кемикал Корпорейшн | Element in form of two trapeziums, unit with fluidized bed, and method for carrying out reaction of nitro compound hydrogenation |
| US12098114B2 (en) | 2018-10-17 | 2024-09-24 | China Petroleum & Chemical Corporation | Double-trapezoid structural member, fluidized apparatus and nitro compound hydrogenation reaction process |
| CN109663546A (en) * | 2019-02-21 | 2019-04-23 | 南京科技职业学院 | A kind of antifebrin synthesis special purpose reactor |
| CN109663546B (en) * | 2019-02-21 | 2022-09-06 | 南京科技职业学院 | Special reactor for synthesizing acetanilide |
| CN110893333A (en) * | 2019-12-19 | 2020-03-20 | 靖江神驹容器制造有限公司 | O-chlorobenzonitrile fluidized bed reactor |
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Address after: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee after: China Petroleum & Chemical Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: China Petroleum & Chemical Corp. Patentee before: Nanhua Group Research Institute |