CN103566837A - External circular reaction device suitable for hydrogenation exothermic reaction - Google Patents
External circular reaction device suitable for hydrogenation exothermic reaction Download PDFInfo
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Abstract
The invention discloses an external circular reaction device suitable for hydrogenation exothermic reaction. The external circular reaction device mainly comprises a first-stage hydrogenation reactor, a second-stage hydrogenation reactor, a hydrogen circulation loop and a liquid circulation loop. The liquid circulation loop in the reaction device is used for mixing a part of reacted solution and a fresh raw material solution, so that the concentration of raw materials in the reactor is reduced, the bed temperature rise generated by a heat release effect caused by hydrogenation is relieved, and the temperature inside the first-stage hydrogenation reactor is effectively controlled. A way that the raw material solution and hydrogen flow up in parallel is adopted in the first-stage hydrogenation reactor, a liquid phase is used as a continuous phase, and a catalyst is soaked into a reaction liquid, so that the reaction temperature of a catalyst bed keeps constant, meanwhile, the overhigh local temperature of a reaction site on the surface of the catalyst is avoided, furthermore, the occurrence of polymerization reaction of organic matters on the surface of the catalyst is effectively inhibited, the carbon deposition quantity on the surface of the catalyst is low, and the service life of the catalyst is remarkably prolonged. The external circular reaction device disclosed by the invention is suitable for continuously producing succinic anhydride by using maleic anhydride through catalytic hydrogenation and preparing 1- 4-butanediol by using butynediol through hydrogenation.
Description
Technical field
The present invention relates to a kind ofly with liquid circulation loop and gas circulation loop, be applicable to the outer circulation reaction unit of hydrogenation exothermic reaction, specifically a kind ofly can control reaction temperature equilibrium, simultaneously without the outer circulation hydrogenation reactor of focus.
Background technology
Poly butylene succinate (PBS), is made by succinic acid and BDO esterifying polycondensation, the outstanding person in biodegradable plastic material, purposes is very extensive, and it can finally be degraded into the materials such as carbon dioxide and water, environmental sound under the effect of bacterium or enzyme.In addition, the fusing point of PBS is higher, functional, is hopeful to replace general polyethylene or polypropylene and enters general-purpose plastics field, alleviates conventional plastic pollution on the environment.Particularly importantly, PBS plastic processing performance is very good, can on existing plastic processing common apparatus, carry out all kinds of processing and forming, is that current degradative plastics processing characteristics is best.The market prospects of PBS are boundless, and this also will stimulate and drive the market demand of its upstream product succinic acid and BDO.The annual requirement of future China PBS will reach more than 3,000,000 tons, need to consume 2,040,000 tons/year of succinic acid (amounting to 1,740,000 tons/year of succinic anhydrides), 1,530,000 tons/year of BDOs.
There is the succinic anhydride of competitive advantage and BDO production method and be and take respectively the fixed bed hydrogenation technique that cis-butenedioic anhydride and Isosorbide-5-Nitrae-butynediols be raw material.The hydrogenation technique that the fixed bed of take is reactor has the following advantages: (1) reactant can effectively contact with catalyst, and feed stock conversion and target product selectivity are high; (2) catalyst mechanical loss is little; (3) simple in structure; (4) production serialization, is applicable to large-scale production.Patent US5952514 and US5770744 disclose a kind of with single tube fixed bed reactors, maleic anhydride hydrogenation is produced the method for succinic anhydride: in reaction temperature, be 60-180 ℃, pressure 380bar(38MPa) under, cis-butenedioic anhydride conversion ratio is 99%, and succinic anhydride is selectively 98%.Application publication CN 101890323 A have invented maleic anhydride hydrogenation produce succinic acid acid anhydride trickle bed reactor, and cis-butenedioic anhydride conversion ratio is 100%, and succinic anhydride is selectively 98%.US-A 5068468 disclose under the catalysis of dead load type nickel/copper catalyst 1,4-butynediols Hydrogenation 1,4-butanediol, under the pressure of 250bar, the space-time yield of butanediol is 0.3Kg/Lh, BE-B 745225 discloses the preparation method who adopts Raney's nickel fixed bde catalyst under the pressure of 259bar, and by two-step reaction, the space-time yield of butanediol is 0.286Kg/Lh.It is worth noting, maleic anhydride hydrogenation synthesizing succinic acid acid anhydride (Δ H=-128KJ/mol) and 1,4-butynediols Hydrogenation 1,4-butanediol (Δ H=-251KJ/mol) is strong exothermal reaction, this just makes the hydrogenation site local temperature of catalyst surface in course of reaction too high, cause organic matter at catalyst surface polymerization coking, reduce catalyst activity.Meanwhile, due to the accumulation of reaction heat, easily make reaction bed temperature sharply raise, temperature runaway phenomenon occurs, make reaction be forced to stop.Yet, in the method for hydrotreating of above-mentioned listed succinic anhydride or BDO, do not relate to shifting out of reaction heat.
Patent US2245404 (A) discloses a kind of employing inner-heating tube and has removed maleic anhydride hydrogenation reaction heat, thereby controls the method for beds temperature rise.The reaction heat that the method is applicable to more small-sized reaction unit shifts out, if reaction unit increases, moves heat pipe and not only reaction heat evenly can not be shifted out and affects the distribution of reactant liquor in reactor, thereby reduce catalyst reaction performance.ZL201110235411.5 controls hydrogenation reaction temperature by cooler is installed in the middle of the beds at trickle bed reactor, and then highly selective synthesizing succinic acid acid anhydride, the method can be controlled reaction bed temperature effectively, yet when cis-butenedioic anhydride concentration increases to improve separate unit reactor production capacity in material solution, easily in the hydrogenation site of catalyst surface, form excessive temperature and cause catalyst activity component sintering or organic polymer coking.Meanwhile, this reactor processed complex, technique is loaded down with trivial details.EP-B 0319207, DE-A 1941633 and DE-A 2040501 adopt gas and liquid and flow to upper by the pattern of fixed bde catalyst, make Isosorbide-5-Nitrae-butynediols hydrogenation generate BDO, in the method, catalyst is soaked in liquid, alleviated the local temperature rise in catalyst surface hydrogenation site in hydrogenation process, but when reaction solution Raw Isosorbide-5-Nitrae-butynediols concentration improves, beds longitudinal temperature skewness, reaction temperature is difficult to control.
Summary of the invention
For maleic anhydride hydrogenation, produce succinic anhydride and 1,4-butynediols hydrogenation produces 1,4-butanediol is strong exothermal reaction, take fixed bed when reactor serialization is produced, hydrogenation reaction temperature is wayward and have a focus, the easy coking of reactant is covered in catalyst surface, cause catalysqt deactivation problem, the object of the present invention is to provide and a kind ofly can effectively control reaction temperature, eliminate focus and coking in reactor simultaneously, realize a kind of outer circulation reaction unit that is applicable to hydrogenation exothermic reaction of the serialization large-scale production of succinic anhydride and BDO.
This reactor has liquid circulation loop and gas circulation loop simultaneously, and one-level hydrogenation reactor adopts the gas and liquid flowing type of flow that makes progress, and take liquid as continuous phase, and catalyst is immersed in reactant liquor.When having realized whole reactor reaction temperature equalization control, the local temperature rise that effectively reduces catalyst surface reaction site.Whole reactor, in the situation that average reaction temperature is constant, does not have outstanding focus, effectively avoids the generation of polymerization ofathe reactants carbon distribution, promotes the reaction effect of whole reactor.And simple and reasonable for structure, be both applicable to use for laboratory, can be used for again suitability for industrialized production, also can expanded application in the gas-liquid hydrogenation reaction of a large class.
Specifically, this reaction unit is mainly comprised of one-level hydrogenation reactor, secondary hydrogenation reactor, hydrogen closed circuit and liquid circulation loop.Material liquid flows and carries out hydrogenation reaction with hydrogen the flow direction from one-level hydrogenation reactor bottom, reactant liquor after hydrogenation is shunted with certain split ratio, the reactant liquor distributing enters secondary hydrogenation reactor and hydrogen and flows to current downflow through heat-exchanger rig adds H-H reaction, and residual reaction liquid mixes and reenters one-level hydrogenation reactor with fresh feed liquid after heat-exchanger rig is removed heat; The hydrogen that one-level hydrogenation reactor is discharged, a part enters secondary hydrogenation reactor through voltage stabilizing, constant-current stabilizer, and remainder mixes with fresh hydrogen and reenters one-level hydrogenation reactor.
A kind of outer circulation reaction unit that is applicable to hydrogenation exothermic reaction provided by the invention, is comprised of the first feed pump, one-level hydrogenation reactor, gas-liquid separator, the first heat-exchange device, the second feed pump, the second heat-exchange device, voltage stabilization and current stabilization device secondary hydrogenation reactor;
Described one-level hydrogenation reactor, its underpart arranges the first gas-liquid distribution apparatus, the first gas-liquid distribution apparatus top arranges the first gripper shoe, in the first gripper shoe, set gradually the first packing layer, the first beds, the second packing layer and pressing plate, the top of one-level hydrogenation reactor arranges seal closure; Seal closure the first flange seal; The first housing bottom of one-level hydrogenation reactor has liquid-inlet, seal closure side has the first gas liquid outlet, the first middle part, housing side of one-level hydrogenation reactor has the first temperature-measuring port, and side bottom has gas access, and side bottom the first packing layer place has first and unloads outlet;
Described secondary hydrogenation reactor, its underpart arranges the second gripper shoe, sets gradually the 3rd packing layer, the second beds and the 4th packing layer in the second gripper shoe, and the 4th packing layer top is provided with the second gas-liquid distribution apparatus; The top of secondary hydrogenation reactor and bottom are respectively with the second flange and three-flange sealing; The second flange has gas-liquid import, and three-flange has the second gas liquid outlet, and the second housing side of secondary hydrogenation reactor has the second temperature-measuring port, and side bottom the 3rd packing layer place has second and unloads outlet;
The first charging delivery side of pump is connected with the entrance of one-level hydrogenation reactor liquid-inlet, the second feed pump, the outlet of the first heat-exchange device respectively by pipeline; The entrance of gas-liquid separator is connected with the first gas liquid outlet of one-level hydrogenation reactor, the liquid outlet of gas-liquid separator is connected with the entrance of the first heat-exchange device, the gas vent of gas-liquid separator is connected with the entrance of voltage stabilization and current stabilization device with gas access respectively by pipeline, the second charging delivery side of pump is connected with the outlet of voltage stabilization and current stabilization device by the second heat-exchange device, and the gas-liquid import of secondary hydrogenation reactor is connected with the outlet of voltage stabilization and current stabilization device with the outlet of the second heat-exchange device respectively by pipeline.
Compared with prior art, advantage of the present invention:
1. adopt outer circulation thermal withdrawal mode, reaction heat is evenly shifted out, effectively controlled the average operation temperature of whole reactor, make whole main reactor interior reaction temperature balanced, be conducive to realize the serialization large-scale production of succinic anhydride and BDO.
2. one-level hydrogenation reactor adopts material liquid with hydrogen and flows to the upper type of flow, when having realized whole reactor reaction temperature equalization control, effectively controls and reduces hot localised points temperature.Whole reactor, in the situation that average reaction temperature is constant, does not have outstanding focus, effectively avoids the generation of polymerization ofathe reactants carbon distribution or coking, promotes the reaction effect of whole reactor.
3. reactor structure is simple, is easy to processing.
Accompanying drawing explanation
Fig. 1 reaction unit structural representation of the present invention
In figure: 1-the first feed pump, 2-one-level hydrogenation reactor, 3-gas-liquid separator, 4-the first heat-exchange device, 5-the second feed pump, 6-the second heat-exchange device, 7-voltage stabilization and current stabilization device, 8-secondary hydrogenation reactor, 21-the first housing, 22-liquid-inlet, 23-gas access, 24-the first gas-liquid distribution apparatus, 25-the first gripper shoe, 26-the first packing layer, 27-first unloads outlet, 28-the first beds, 29-the second packing layer, 210-pressing plate, 211-the first flange, 212-seal closure, 213-the first gas liquid outlet, 214-the first temperature-measuring port, 81-the second gripper shoe, 82-the 3rd packing layer, 83-the second beds, 84-the 4th packing layer, 85-the second gas-liquid distribution apparatus, the import of 86-gas-liquid, 87-the second gas liquid outlet, 88-the second temperature-measuring port, 89-second unloads outlet, 810-the second housing, 811-the second flange, 812-three-flange
The specific embodiment
Below in conjunction with drawings and Examples, invention is described in further detail, but this does not limit the scope of the invention.
Fig. 1 is reaction unit structural representation of the present invention.
This reaction unit is comprised of the first feed pump 1, one-level hydrogenation reactor 2, gas-liquid separator 3, the first heat-exchange device 4, the second feed pump 5, the second heat-exchange device 6, voltage stabilization and current stabilization device 7 and secondary hydrogenation reactor 8;
Described one-level hydrogenation reactor 2, its underpart arranges the first gas-liquid distribution apparatus 24, the first gas-liquid distribution apparatus 24 tops arrange the first gripper shoe 25, in the first gripper shoe 25, set gradually the first packing layer 26, the first beds 28, the second packing layer 29 and pressing plate 210, the top of one-level hydrogenation reactor 2 arranges seal closure 212; Seal closure 212 use the first flange 211 sealings; The first housing 21 bottoms of one-level hydrogenation reactor 2 have liquid-inlet 22, seal closure 212 sides have the first gas liquid outlet 213, the first housing 21 middle parts, side of one-level hydrogenation reactor 2 have the first temperature-measuring port 214, side bottom has gas access 23, and side bottom the first packing layer 26 places have first and unload outlet 27;
Described secondary hydrogenation reactor 8, its underpart arranges and in the second gripper shoe 81, the second gripper shoes 81, sets gradually the 3rd packing layer 82, the second beds 83 and the 4th packing layer 84, the four packing layer 84 tops and be provided with the second gas-liquid distribution apparatus 85; The top of secondary hydrogenation reactor 8 and bottom are respectively with the second flange 811 and three-flange 812 sealings; The second flange 811 has gas-liquid import 86, the three-flanges 812 and has the second gas liquid outlet 87, and the second housing 810 sides of secondary hydrogenation reactor 8 have the second temperature-measuring port 88, and side bottom the 3rd packing layer 82 places have second and unload outlet 89;
The outlet of the first feed pump 1 is connected with liquid-inlet 22, the entrance of the second feed pump 5, the outlet of the first heat-exchange device 4 of one-level hydrogenation reactor 2 respectively by pipeline; The entrance of gas-liquid separator 3 is connected with the first gas liquid outlet 213 of one-level hydrogenation reactor 2, the liquid outlet of gas-liquid separator 3 is connected with the entrance of the first heat-exchange device 4, the gas vent of gas-liquid separator 3 is connected with the entrance of voltage stabilization and current stabilization device 7 with gas access 23 respectively by pipeline, the outlet of the second feed pump 5 is connected with the outlet of voltage stabilization and current stabilization device 7 by the second heat-exchange device 6, and the gas-liquid import 86 of secondary hydrogenation reactor 8 is connected with the outlet of voltage stabilization and current stabilization device 7 with the outlet of the second heat-exchange device 6 respectively by pipeline.
Reaction solution flows and carries out hydrogenation reaction with hydrogen the flow direction from one-level hydrogenation reactor bottom, reactant liquor after hydrogenation is shunted with certain proportion, the reactant liquor distributing enters secondary hydrogenation reactor and hydrogen and flows to current downflow through heat-exchanger rig adds H-H reaction, and residual reaction liquid mixes and reenters one-level hydrogenation reactor with fresh feed liquid after heat-exchanger rig is removed heat; The hydrogen part that one-level hydrogenation reactor is discharged enters secondary hydrogenation reactor through voltage stabilizing, constant-current stabilizer, and remainder mixes with fresh hydrogen and reenters one-level hydrogenation reactor.
Because this reactor adopts outer circulation thermal withdrawal mode, reaction heat is evenly shifted out, effectively controlled the average operation temperature of whole reactor, make whole main reactor interior reaction temperature balanced.Meanwhile, one-level hydrogenation reactor adopts material liquid with hydrogen and flows to the upper type of flow, when having realized whole reactor reaction temperature equalization control, effectively controls and reduces hot localised points temperature.Whole reactor, in the situation that average reaction temperature is constant, does not have outstanding focus, effectively avoids the generation of polymerization ofathe reactants carbon distribution or coking, significantly promotes the reaction effect of whole reactor.
Claims (1)
1. an outer circulation reaction unit that is applicable to hydrogenation exothermic reaction, it is characterized in that, this reaction unit is comprised of the first feed pump (1), one-level hydrogenation reactor (2), gas-liquid separator (3), the first heat-exchange device (4), the second feed pump (5), the second heat-exchange device (6), voltage stabilization and current stabilization device (7) and secondary hydrogenation reactor (8);
Described one-level hydrogenation reactor (2), its underpart arranges the first gas-liquid distribution apparatus (24), the first gas-liquid distribution apparatus (24) top arranges the first gripper shoe (25), in the first gripper shoe (25), set gradually the first packing layer (26), the first beds (28), the second packing layer (29) and pressing plate (210), the top of one-level hydrogenation reactor (2) arranges seal closure (212); Seal closure (212) seals with the first flange (211); The first housing (21) bottom of one-level hydrogenation reactor (2) has liquid-inlet (22), seal closure (212) side has the first gas liquid outlet (213), the middle part, the first housing (21) side of one-level hydrogenation reactor (2) has the first temperature-measuring port (214), side bottom has gas access (23), and side bottom the first packing layer (26) is located to have first and unloaded outlet (27);
Described secondary hydrogenation reactor (8), its underpart arranges the second gripper shoe (81), in the second gripper shoe (81), set gradually the 3rd packing layer (82), the second beds (83) and the 4th packing layer (84), the 4th packing layer (84) top is provided with the second gas-liquid distribution apparatus (85); The second flange (811) and three-flange (812) sealing are used respectively in the top of secondary hydrogenation reactor (8) and bottom; The second flange (811) has gas-liquid import (86), three-flange (812) has the second gas liquid outlet (87), the second housing (810) side of secondary hydrogenation reactor (8) has the second temperature-measuring port (88), and side bottom the 3rd packing layer (82) is located to have second and unloaded outlet (89);
The outlet of the first feed pump (1) is connected with the entrance of one-level hydrogenation reactor (2) liquid-inlet (22), the second feed pump (5), the outlet of the first heat-exchange device (4) respectively by pipeline, the entrance of gas-liquid separator (3) is connected with first gas liquid outlet (213) of one-level hydrogenation reactor (2), the liquid outlet of gas-liquid separator (3) is connected with the entrance of the first heat-exchange device (4), the gas vent of gas-liquid separator (3) is connected with the entrance of voltage stabilization and current stabilization device (7) with gas access (23) respectively by pipeline, the outlet of the second feed pump (5) is connected with the outlet of voltage stabilization and current stabilization device (7) by the second heat-exchange device (6), the gas-liquid import (86) of secondary hydrogenation reactor (8) is connected with the outlet of voltage stabilization and current stabilization device (7) with the outlet of the second heat-exchange device (6) respectively by pipeline.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110872209A (en) * | 2018-08-30 | 2020-03-10 | 中国石化工程建设有限公司 | Device and method for preparing phenethyl alcohol by acetophenone hydrogenation |
| CN111889036A (en) * | 2019-05-05 | 2020-11-06 | 中国石油集团工程股份有限公司 | Cyclopentadiene fixed bed catalytic hydrogenation reaction device, system and method |
| CN114247386A (en) * | 2021-11-24 | 2022-03-29 | 中国五环工程有限公司 | Evaporative isothermal hydrogenation reaction method and evaporative isothermal reaction system |
| CN114288952A (en) * | 2021-12-31 | 2022-04-08 | 万华化学集团股份有限公司 | Airlift type external circulation reactor and method |
| CN114516667A (en) * | 2020-11-20 | 2022-05-20 | 中国石油天然气集团有限公司 | Reaction device for fixed bed cracking of oily wastewater for laboratory |
| CN116023351A (en) * | 2021-10-27 | 2023-04-28 | 中国石油化工股份有限公司 | Preparation method and system of succinic anhydride |
| CN116041290A (en) * | 2021-10-28 | 2023-05-02 | 中国石油化工股份有限公司 | Maleic anhydride hydrogenation method and maleic anhydride hydrogenation system |
| CN116041289A (en) * | 2021-10-28 | 2023-05-02 | 中国石油化工股份有限公司 | Production process for preparing succinic anhydride by maleic anhydride hydrogenation |
| CN116041291A (en) * | 2021-10-28 | 2023-05-02 | 中国石油化工股份有限公司 | Production process for preparing succinic anhydride by maleic anhydride hydrogenation |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110872209A (en) * | 2018-08-30 | 2020-03-10 | 中国石化工程建设有限公司 | Device and method for preparing phenethyl alcohol by acetophenone hydrogenation |
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| CN114516667A (en) * | 2020-11-20 | 2022-05-20 | 中国石油天然气集团有限公司 | Reaction device for fixed bed cracking of oily wastewater for laboratory |
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| CN116041291A (en) * | 2021-10-28 | 2023-05-02 | 中国石油化工股份有限公司 | Production process for preparing succinic anhydride by maleic anhydride hydrogenation |
| WO2023072047A1 (en) * | 2021-10-28 | 2023-05-04 | 中国石油化工股份有限公司 | Method for preparing succinic anhydride by means of hydrogenation of maleic anhydride and production system |
| CN116041290B (en) * | 2021-10-28 | 2024-05-07 | 中国石油化工股份有限公司 | Maleic anhydride hydrogenation method and maleic anhydride hydrogenation system |
| CN114247386A (en) * | 2021-11-24 | 2022-03-29 | 中国五环工程有限公司 | Evaporative isothermal hydrogenation reaction method and evaporative isothermal reaction system |
| CN114247386B (en) * | 2021-11-24 | 2023-10-13 | 中国五环工程有限公司 | Evaporation type isothermal hydrogenation reaction method and evaporation type isothermal reaction system |
| CN114288952A (en) * | 2021-12-31 | 2022-04-08 | 万华化学集团股份有限公司 | Airlift type external circulation reactor and method |
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Application publication date: 20140212 Assignee: Shanghai Diyang Chemical Technology Co.,Ltd. Assignor: Shanxi University Contract record no.: X2021980000475 Denomination of invention: An external circulation reactor for exothermic hydrogenation Granted publication date: 20150930 License type: Common License Record date: 20210119 |
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