CN103566837B - A kind of outer circulation reaction unit being applicable to hydrogenation exothermic reaction - Google Patents
A kind of outer circulation reaction unit being applicable to hydrogenation exothermic reaction Download PDFInfo
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Abstract
Be applicable to an outer circulation reaction unit for hydrogenation exothermic reaction, form primarily of one-level hydrogenation reactor, secondary hydrogenation reactor, hydrogen closed circuit and liquid circulation loop.Liquid circulation loop in this reaction unit will react rear portion solution and mix with fresh feed liquid, reduce the concentration of reactor Raw, alleviate the bed temperature rise that hydrogenation exothermic effect causes, and effectively control temperature in one-level hydrogenation reactor.The type of flow that one-level hydrogenation reactor adopts material liquid and hydrogen also to flow to, take liquid phase as continuous phase, catalyst is soaked in reactant liquor, while realizing catalyst bed reaction temperature constant, avoid the local temperature of catalyst surface reaction site too high, and then effectively suppressing the generation of catalyst surface organic polymer reaction, catalyst surface carbon deposition quantity is few, significant prolongation catalyst service life.Outer circulation reaction unit of the present invention is applicable to cis-butenedioic anhydride catalytic hydrogenation continuous seepage succinic anhydride and butynediols Hydrogenation BDO.
Description
Technical field
The present invention relates to a kind of 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 obtained 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 material 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, alleviating conventional plastic pollution on the environment.Significantly, PBS plastic processing performance is very good, can carry out all kinds of processing and forming on existing plastic processing common apparatus, 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.Estimate that the annual requirement of following China PBS will reach more than 3,000,000 tons, succinic acid 2,040,000 tons/year (amounting to succinic anhydride 1,740,000 tons/year) need be consumed, BDO 1,530,000 tons/year.
Succinic anhydride and the BDO production method with competitive advantage are respectively with the fixed bed hydrogenation technique that cis-butenedioic anhydride and Isosorbide-5-Nitrae-butynediols are raw material.Be that the hydrogenation technique of reactor has the following advantages with fixed bed: (1) reactant effectively can contact with catalyst, feed stock conversion and target product selectivity high; (2) catalytic mechanical loss is little; (3) structure is simple; (4) production serialization, is applicable to large-scale production.Patent US5952514 and US5770744 discloses a kind of with single tube fixed bed reactors, maleic anhydride hydrogenation produces the method for succinic anhydride: be 60-180 DEG C in reaction temperature, pressure 380bar(38MPa) under, conversion rate of maleic anhydride is 99%, and succinic anhydride is selective is 98%.Application publication CN 101890323 A has invented maleic anhydride hydrogenation produce succinic acid acid anhydride trickle bed reactor, and conversion rate of maleic anhydride is 100%, and succinic anhydride is selective is 98%.US-A 5068468 discloses under dead load type nickel/copper catalyst catalysis 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 adopting 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.But, do not relate to shifting out of reaction heat in the method for hydrotreating of above-mentioned listed succinic anhydride or BDO.
Patent US2245404 (A) discloses a kind of inner-heating tube that adopts to remove maleic anhydride hydrogenation reaction heat, thus 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 the distribution affecting reactant liquor in reactor, thus reduces catalyst reaction performance.ZL201110235411.5 controls hydrogenation reaction temperature by installing cooler in the middle of the beds of trickle bed reactor, and then highly selective synthesizing succinic acid acid anhydride, the method can control reaction bed temperature effectively, but when cis-butenedioic anhydride concentration in material solution increases to improve separate unit reactor production capacity, then the easy hydrogenation site at catalyst surface forms excessive temperature and causes 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 adopts gas and liquid and flows to the pattern by fixed bde catalyst, Isosorbide-5-Nitrae-butynediols hydrogenation is made to generate BDO, in the method, catalyst is soaked in liquid, alleviate 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
Succinic anhydride and 1 is produced for maleic anhydride hydrogenation, 4-butynediols hydrogenation produces 1,4-butanediol is strong exothermal reaction, when taking fixed bed as reactor continuous prodution, hydrogenation reaction temperature is wayward and there is focus, the easy coking of reactant is covered in catalyst surface, cause catalysqt deactivation problem, the object of the present invention is to provide one effectively can control reaction temperature, focus and coking in eliminative reaction device simultaneously, realize a kind of outer circulation reaction unit being 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 upwards type of flow, is continuous phase, is immersed in reactant liquor by catalyst with liquid.While achieving the control of whole reactor reaction temperature equalization, effectively reduce the local temperature rise of catalyst surface reaction site.Whole reactor, when average reaction temperature is constant, does not have outstanding focus, effectively avoids the generation of polymerization ofathe reactants carbon distribution, promote the reaction effect of whole reactor.And simple and reasonable for structure, be both applicable to use for laboratory, and can be used for suitability for industrialized production again, go back the gas-liquid hydrogenation reaction that easily extensible is applied to a large class.
Specifically, this reaction unit forms primarily of one-level hydrogenation reactor, secondary hydrogenation reactor, hydrogen closed circuit and liquid circulation loop.Bottom one-level hydrogenation reactor, also flow to flowing carries out hydrogenation reaction to material liquid with hydrogen, reactant liquor after hydrogenation is shunted with certain split ratio, the reactant liquor distributed enters secondary hydrogenation reactor and hydrogen through heat-exchanger rig and flows to current downflow and carries out adding H-H reaction, and residual reaction liquid is removed to mix with fresh feed liquid after heat through heat-exchanger rig and reentered one-level hydrogenation reactor; 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 being applicable to hydrogenation exothermic reaction provided by the invention, is made up 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, first gripper shoe is set above the first gas-liquid distribution apparatus, first gripper shoe sets 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; First housing bottom of one-level hydrogenation reactor has liquid-inlet, seal closure side has the first gas liquid outlet, first case side Middle face of one-level hydrogenation reactor has the first temperature-measuring port, and side bottom has gas access, and side bottom first packing layer place has first and unloads outlet;
Described secondary hydrogenation reactor, its underpart arranges the second gripper shoe, the second gripper shoe sets gradually the 3rd packing layer, the second beds and the 4th packing layer, is provided with the second gas-liquid distribution apparatus above the 4th packing layer; The top of secondary hydrogenation reactor and bottom are respectively with the second flange and three-flange sealing; 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;
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 gas access with voltage stabilization and current stabilization device respectively by pipeline, second charging delivery side of pump is connected by the outlet of the second heat-exchange device with voltage stabilization and current stabilization 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 controls the average operating temperature of whole reactor, make whole main reactor interior reaction temperature balanced, be conducive to the serialization large-scale production realizing succinic anhydride and BDO.
2. one-level hydrogenation reactor adopts material liquid and hydrogen also to flow to the type of flow, while achieving the control of whole reactor reaction temperature equalization, effectively controls and reduces hot localised points temperature.Whole reactor, when average reaction temperature is constant, does not have outstanding focus, effectively avoids the generation of polymerization ofathe reactants carbon distribution or coking, promote 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-first feed pump, 2-one-level hydrogenation reactor, 3-gas-liquid separator, 4-first heat-exchange device, 5-second feed pump, 6-second heat-exchange device, 7-voltage stabilization and current stabilization device, 8-secondary hydrogenation reactor, 21-first housing, 22-liquid-inlet, 23-gas access, 24-first gas-liquid distribution apparatus, 25-first gripper shoe, 26-first packing layer, 27-first unloads outlet, 28-first beds, 29-second packing layer, 210-pressing plate, 211-first flange, 212-seal closure, 213-first gas liquid outlet, 214-first temperature-measuring port, 81-second gripper shoe, 82-the 3rd packing layer, 83-second beds, 84-the 4th packing layer, 85-second gas-liquid distribution apparatus, the import of 86-gas-liquid, 87-second gas liquid outlet, 88-second temperature-measuring port, 89-second unloads outlet, 810-second housing, 811-second flange, 812-three-flange
Detailed description of the invention
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 made up of the first feed pump 1, one-level hydrogenation reactor 2, gas-liquid separator 3, first heat-exchange device 4, second feed pump 5, 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, first gripper shoe 25 is set above first gas-liquid distribution apparatus 24, first gripper shoe 25 sets gradually the first packing layer 26, first beds 28, second packing layer 29 and pressing plate 210, the top of one-level hydrogenation reactor 2 arranges seal closure 212; Seal closure 212 first flange 211 seals; Liquid-inlet 22 is had bottom first housing 21 of one-level hydrogenation reactor 2, seal closure 212 side has the first gas liquid outlet 213, the first temperature-measuring port 214 is had in the middle part of first housing 21 side of one-level hydrogenation reactor 2, side bottom has gas access 23, and side bottom first packing layer 26 place has first and unloads outlet 27;
Described secondary hydrogenation reactor 8, its underpart arranges the second gripper shoe 81, second gripper shoe 81 sets gradually above the 3rd packing layer 82, second beds 83 and the 4th packing layer the 84, four packing layer 84 and is provided with the second gas-liquid distribution apparatus 85; The top of secondary hydrogenation reactor 8 and bottom seal with the second flange 811 and three-flange 812 respectively; Second flange 811 has gas-liquid import 86, and three-flange 812 has the second gas liquid outlet 87, and 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 place has second and unloads outlet 89;
The outlet of the first feed pump 1 is connected with the entrance of liquid-inlet 22, second feed pump 5 of one-level hydrogenation reactor 2, the outlet of the first heat-exchange device 4 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 gas access 23 with voltage stabilization and current stabilization device 7 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.
Bottom one-level hydrogenation reactor, also flow to flowing carries out hydrogenation reaction to reaction solution with hydrogen, reactant liquor after hydrogenation is shunted with certain proportion, the reactant liquor distributed enters secondary hydrogenation reactor and hydrogen through heat-exchanger rig and flows to current downflow and carries out adding H-H reaction, and residual reaction liquid is removed to mix with fresh feed liquid after heat through heat-exchanger rig and reentered one-level hydrogenation reactor; 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 controls the average operating temperature of whole reactor, make whole main reactor interior reaction temperature balanced.Meanwhile, one-level hydrogenation reactor adopts material liquid and hydrogen also to flow to the type of flow, while achieving the control of whole reactor reaction temperature equalization, effectively controls and reduces hot localised points temperature.Whole reactor, when 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. one kind is applicable to maleic anhydride hydrogenation production succinic anhydride or 1,4-butynediols hydrogenation produces 1, the outer circulation reaction unit of 4-butanediol hydrogenation exothermic reaction, it is characterized in that, this reaction unit is made up 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), first gas-liquid distribution apparatus (24) top arranges the first gripper shoe (25), first gripper shoe (25) sets 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) the first flange (211) seals; 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 first temperature-measuring port (214) is had in the middle part of first housing (21) side of one-level hydrogenation reactor (2), side bottom has gas access (23), and side bottom first packing layer (26) place has first and unloads outlet (27);
Described secondary hydrogenation reactor (8), its underpart arranges the second gripper shoe (81), second gripper shoe (81) sets 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 top of secondary hydrogenation reactor (8) and bottom use the second flange (811) and three-flange (812) sealing respectively; Second flange (811) has gas-liquid import (86), three-flange (812) has the second gas liquid outlet (87), second housing (810) side of secondary hydrogenation reactor (8) has the second temperature-measuring port (88), and side bottom the 3rd packing layer (82) place has second and unloads 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 gas access (23) entrance with voltage stabilization and current stabilization device (7) respectively by pipeline, the outlet of the second feed pump (5) is connected by the outlet of the second heat-exchange device (6) with voltage stabilization and current stabilization device (7), 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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| CN110872209B (en) * | 2018-08-30 | 2022-07-22 | 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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| CN116020355A (en) * | 2021-10-26 | 2023-04-28 | 中国石油化工股份有限公司 | Tubular reactor for preparing succinic anhydride and method for preparing succinic anhydride |
| 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 |
| CN116020354A (en) * | 2021-10-27 | 2023-04-28 | 中国石油化工股份有限公司 | Liquid phase hydrogenation reaction system and application thereof, and maleic anhydride hydrogenation method |
| 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 |
| CN116041291B (en) * | 2021-10-28 | 2024-09-03 | 中国石油化工股份有限公司 | Production process for preparing succinic anhydride by maleic anhydride hydrogenation |
| CN116037000B (en) * | 2021-10-28 | 2024-09-17 | 中国石油化工股份有限公司 | Method for producing succinic anhydride by maleic anhydride hydrogenation and system for producing succinic anhydride by maleic anhydride hydrogenation |
| 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 |
| 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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| BE754868A (en) * | 1969-08-16 | 1971-02-15 | Basf Ag | PROCESS FOR CARRYING OUT EXOTHERMAL REACTIONS BETWEEN A GAS AND A LIQUID |
| GB8728156D0 (en) * | 1987-12-02 | 1988-01-06 | Davy Mckee Ltd | Process |
| US5958218A (en) * | 1996-01-22 | 1999-09-28 | The M. W. Kellogg Company | Two-stage hydroprocessing reaction scheme with series recycle gas flow |
| CN201529518U (en) * | 2009-05-13 | 2010-07-21 | 中国石油化工股份有限公司 | Gas-liquid-solid three-phase fixed bubbling column reactor |
| CN101735182B (en) * | 2009-12-07 | 2011-08-17 | 山西大学 | Process for continuously producing succinic anhydride through hydrogenation of maleic anhydride |
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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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