CN103537243B - Acrolein oxidation reaction heat moving-out device and method - Google Patents
Acrolein oxidation reaction heat moving-out device and method Download PDFInfo
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- CN103537243B CN103537243B CN201310524228.6A CN201310524228A CN103537243B CN 103537243 B CN103537243 B CN 103537243B CN 201310524228 A CN201310524228 A CN 201310524228A CN 103537243 B CN103537243 B CN 103537243B
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Abstract
The present invention discloses the reaction of a kind of propylene oxidation and generates the hot moving-out device of acrolein reaction and method.Comprise reactor and two cover fused salt adjusters, the conversion zone of a set of coupled reaction device, the quench zone of a set of coupled reaction device; Drum is provided with between two cover adjusters.Open conversion zone axial-flow pump, fused salt enters at reactor reaction section F1 base ring chamber import A2, flows out, control the fused salt amount entering conversion zone boiler, form one and independently circulate through conversion zone guiding valve through deflection plate from upper ring cavity outlet A1; Open quench zone axial-flow pump, fused salt is entered at reactor quench zone F2 base ring chamber import A8, flow out from upper ring cavity outlet A7 through deflection plate, enter axial-flow pump top, control with quench zone guiding valve the fused salt amount entering quench zone boiler, form one and independently circulate.By two cover fused salt adjusters, control the temperature of conversion zone and quench zone respectively.Two sections of temperature difference 50 ~ 80 DEG C, flexible adjustment, convenience, do not interfere with each other.
Description
Technical field
The present invention relates to field of chemical technology, particularly propylene oxidation reaction generates the hot moving-out device of acrolein reaction and method.
Background technology
Methacrylaldehyde is a kind of conventional basic important Organic Chemicals, and its downstream product has development and application prospect quite widely.Methacrylaldehyde is the simplest unsaturated aldehyde, and chemical formula is C
3h
4o, be the cacodorous liquid of water white transparency under normal conditions, its steam has very strong excitant and tearing property, is synthetic intermediate very important in chemical industry, is widely used in production of resins and organic synthesis.
Purposes 1: as chromatography standard substance, also for organic synthesis.Methacrylaldehyde is a kind of important chemical intermediate, can be used for the synthesis of the important chemical products such as picoline, pyridine, glutaraldehyde and acrylic acid.
Purposes 2: be mainly used in methionine processed and other Propenal derivatives.Methionine can be widely used in the fields such as medicine, food, feed and cosmetics, and wherein the consumption of feed addictive is maximum.
Purposes 3: external as oil-field flooding bactericide, to suppress the growth of bacterium in water, prevents bacterium from causing corrosion and blocking on stratum.
The reaction that propylene oxidation generates methacrylaldehyde is strong exothermic reaction, and reaction equation is: CH
2=CHCH
3+ O
2→ CH
2=CHCHO+H
2o+3.4X10
5j, recycles with inorganic high-temp thermal medium-molten salt and shifts out heat, strict control system temperature.On the one hand, require that the reaction temperature selecting in the running to be suitable for is also strict and control its fluctuation range, on the other hand, pay special attention to beds, especially focus temperature and control in safe range with the difference of reaction temperature, to avoid " temperature runaway " and to cause damage to catalyst, adopt an effective measure by reacting section catalyst bed export reacting gas temperature be down to rapidly less than 260 DEG C, be oxidized to suppress the automatic depth of methacrylaldehyde.
At present, the acrolein reaction device of domestic 5000 tons/year of scales adopts as shown in Figure 1, in reactor, is provided with tube sheet 11 between conversion zone F1 and quench zone F2; Adopt a set of fused salt control system, namely a set of fused salt of conversion zone F1 and quench zone F2 regulates facility, and capital equipment comprises axial-flow pump, boiler, electric heater, guiding valve, fused salt tank, fused salt submerged pump etc.Before driving, first solid fused salt is put into fused salt tank, after fused salt 150 DEG C being melted with steam, fused salt squeezes into ring cavity on reactor F1 by the fused salt submerged pump on fused salt tank, fused salt is made respectively at reactor reaction section F1 and boiler 3, reactor quench zone F2 Inner eycle by axial-flow pump 2, controlling reaction temperature is exactly by regulating the flow rate of molten salt flowing into boiler 3, open the hot water valve V1 of boiler 3, enter from boiler 3 hot water inlet A12, steam flows out from boiler 3 steam (vapor) outlet A11 through valve V2, and heat is removed by producing steam by reaction heat.Electric heater uses before driving, and makes temperature of molten salt be heated to about 200 DEG C, and after dropping into material, electric heater is turned off.Conversion zone F1 and quench zone F2 two sections only has rising simultaneously or reduces temperature, and flow into the fused salt amount in boiler by governor valve control, the temperature of quench zone F2 is uncontrollable, is the passive change with conversion zone F1 temperature and changes.The temperature difference and the gradient of temperature degree of two sections are different, are unfavorable for controlling.
If heat shifts out not in time, catalyst is temperature runaway or inefficacy likely, and product or oxidation generate acrylic acid or acrylic acid polymer.
Therefore how effectively shifting out heat in time, solve and overcome the security hidden trouble of above-mentioned existence, improve acrolein yield, is the key issue existed at present.
Summary of the invention
In order to solve existing technical problem, the present invention discloses a kind of propylene oxidation reaction generation acrolein reaction heat and shifts out system and method, solves the potential safety hazard existed in production process, improves the economic benefit of methacrylaldehyde process units.
Technical scheme of the present invention is as follows:
A kind of acrolein oxidation reaction heat shifts out system, comprises reactor and two cover fused salt adjusters, the conversion zone F1 of a set of coupled reaction device, the quench zone F2 of a set of coupled reaction device and the drum 10 of output steam.
The circulatory system of the fused salt adjuster of the conversion zone F1 of coupled reaction device is: open conversion zone axial-flow pump 2, fused salt is entered at reactor reaction section F1 base ring chamber import A2, flow out from upper ring cavity outlet A1 through deflection plate, control through conversion zone guiding valve 4 the fused salt amount entering conversion zone boiler 3, form one and independently circulate; The circulatory system of the fused salt adjuster of the quench zone F2 of coupled reaction device is: open quench zone axial-flow pump 5, fused salt is entered at reactor quench zone F2 base ring chamber import A8, flow out from upper ring cavity outlet A7 through deflection plate, enter axial-flow pump 5 top, control with quench zone guiding valve 7 the fused salt amount entering quench zone boiler 6, form one and independently circulate.
When reaction starts, solid fused salt is put into fused salt tank, after fused salt 150 DEG C being melted with steam, squeeze in conversion zone axial-flow pump 2 and quench zone axial-flow pump 5 with the submerged pump 8 on fused salt tank, make conversion zone F1 and quench zone F2 be full of fused salt.
The concrete device of native system is: be made up of 1 reactor, 2 axial-flow pumps, 2 guiding valves, 2 electric heaters, 2 boilers, 1 fused salt tank, 1 submerged pump and 1 drum.After reactor is fixing, axial-flow pump, guiding valve, electric heater, boiler are connected with reactor, and drum 10 is arranged between 2 boilers, and higher than reactor head, fused salt tank connects the material pipeline of two axial-flow pumps through submerged pump.The entrance A3 of axial-flow pump 2, outlet A4 mouth exports A1 with ring cavity on reactor reaction section F1 respectively, lower ring cavity entrance A2 mouth connects, the outlet A5 of conversion zone guiding valve 4, import A6 mouth exports A1 with ring cavity on reactor respectively, lower ring cavity entrance A2 mouth connects, the entrance A9 of axial-flow pump 5, outlet A10 mouth respectively with ring cavity entrance A7 on reactor quench zone F2, lower ring cavity outlet A8 connects, the outlet A13 of quench zone guiding valve 7, entrance A14 mouth respectively with axial-flow pump 5 entrance A11, outlet A12 mouth connects, drum is provided with the water outlet A 16 be connected with conversion zone boiler 3 to be connected with import A23, drum steam inlet A15 with and export A24 and be connected, drum is provided with the water outlet A 18 be connected with quench zone boiler 6 to be connected with import A21, drum steam inlet A17 and outlet A22.
By two cover fused salt adjusters, control the temperature of conversion zone and quench zone respectively.Two sections of temperature difference 50 ~ 80 DEG C, flexible adjustment, convenience, do not interfere with each other.
Conversion zone axial-flow pump 2 with quench zone axial-flow pump 5 arrange the pipeline being connected fused salt tank respectively, when reaction starts, solid fused salt is put into fused salt tank, after being melted by fused salt 150 DEG C with steam, fused salt squeezes into ring cavity and reactor quench zone F2 base ring chamber on reactor reaction section F1 by pumping hole under the liquid fused salt on fused salt tank.
Be described in detail as follows:
Conversion zone F1 opens axial-flow pump 2, fused salt is entered at reactor reaction section F1 base ring chamber A2 mouth, goes out through deflection plate from upper ring cavity A1 mouth, automatically control with guiding valve 4 the fused salt amount entering boiler 3, temperature drift in conversion zone F1, guiding valve 4 leaves greatly, in conversion zone F1, temperature is on the low side, and guiding valve 4 leaves less.Equally, quench zone F2 opens axial-flow pump 5, make fused salt reactor quench zone F2 base ring chamber enter through deflection plate from ring cavity go out to enter axial-flow pump top; Automatically control with guiding valve 7 the fused salt amount entering boiler 6, temperature drift in quench zone F2, guiding valve 7 leaves greatly, and in quench zone F2, temperature is on the low side, and guiding valve 7 leaves less.
Adopt said method to reach conversion zone and quench zone control effects respectively, the heat solving conversion zone shifts out the problem of the impact of the safety in production on device in time.More importantly eliminate potential safety hazard, ensure the safe operation of acrolein reaction device.Can be used in extensive acrolein reaction system, also can be used on similar reactor fused salt heat-tranferring system.
Accompanying drawing explanation
Fig. 1: former technique acrolein oxidation reaction heat shifts out system diagram.
Fig. 2: acrolein oxidation reaction heat of the present invention shifts out system flow diagram.
Fig. 3: the acrolein oxidation reaction heat of band fused salt tank of the present invention and submerged pump shifts out system flow diagram.
Wherein: 1-propylene oxidation reactor, 2-conversion zone axial-flow pump, 3-conversion zone boiler, 4-conversion zone guiding valve, 5-quench zone axial-flow pump, 6-quench zone boiler, 7-quench zone guiding valve, 8-fused salt submerged pump, 9-fused salt tank, 10-drum, 11-tube sheet.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail:
According to content as described in Figure 3, after being formed be it is characterized in that reactor is fixing by 1 reactor, 2 axial-flow pumps, 2 guiding valves, 2 electric heaters, 2 boilers, 1 fused salt tank, 1 submerged pump and 1 drum, axial-flow pump, guiding valve, electric heater, boiler are connected with reactor, drum 10 is arranged between 2 boilers, higher than reactor head, fused salt tank connects the material pipeline of two axial-flow pumps through submerged pump.The entrance A3 of axial-flow pump 2, outlet A4 mouth exports A1 with ring cavity on reactor reaction section F1 respectively, lower ring cavity entrance A2 mouth connects, the outlet A5 of conversion zone guiding valve 4, import A6 mouth exports A1 with ring cavity on reactor respectively, lower ring cavity entrance A2 mouth connects, the entrance A9 of axial-flow pump 5, outlet A10 mouth respectively with ring cavity entrance A7 on reactor quench zone F2, lower ring cavity outlet A8 connects, the outlet A13 of quench zone guiding valve 7, entrance A14 mouth respectively with axial-flow pump 5 entrance A11, outlet A12 mouth connects, drum is provided with the water outlet A 16 be connected with conversion zone boiler 3 to be connected with import A23, drum steam inlet A15 with and export A24 and be connected, drum is provided with the water outlet A 18 be connected with quench zone boiler 6 to be connected with import A21, drum steam inlet A17 and outlet A22.
The circulatory system of the fused salt adjuster of the conversion zone of coupled reaction device is: open conversion zone axial-flow pump 2, fused salt is entered at reactor reaction section F1 base ring chamber import A2, flow out from upper ring cavity outlet A1 through deflection plate, control through conversion zone guiding valve 4 the fused salt amount entering conversion zone boiler 3, form one and independently circulate; The circulatory system of the fused salt adjuster of the quench zone F2 of coupled reaction device is: open quench zone axial-flow pump 5, fused salt is entered at reactor quench zone F2 base ring chamber import A8, flow out from upper ring cavity outlet A7 through deflection plate, enter axial-flow pump 5 top, control with quench zone guiding valve 7 the fused salt amount entering quench zone boiler 6, form one and independently circulate.
By fused salt pipeline, namely go up salt pipeline, unload fused salt pipeline between salt pipeline and each equipment and connect, fused salt is gone out by the A15 mouth of submerged pump 8, enter the A3 mouth of axial-flow pump 2 and the A11 mouth of axial-flow pump 5 respectively, the salt line of putting of all devices all enters fused salt tank A16 mouth, and all fused salt pipeline insulations or companion's heat carry out provision for thermal insulation.
Before driving, first solid fused salt is put into fused salt tank, after being melted by fused salt 150 DEG C with steam, fused salt squeezes into ring cavity on reactor reaction section F1 by pumping hole under the liquid fused salt on fused salt tank, and electric heater uses before driving, and makes temperature of molten salt be heated to about 200 DEG C, after dropping into material, electric heater is turned off.
All fused salts all melt in fused salt tank, fused salt to be squeezed on conversion zone in ring cavity and quench zone axial-flow pump with submerged pump, before driving, first with respective electric heater, fused salt in reactor is heated to about 200 DEG C, turn off electric heater, pass into reaction mixture gas body, temperature of molten salt raises, open the hot water valve V1 of drum 10, hot water enters drum A19 import, respectively through boiler 6 import A21, outlet A22 produces steam, the A23 import of boiler 3, outlet A24 produces steam, steam enters drum air intake A15, A17 mouth, steam is exported through V2 valve by venthole A20, fused salt heat is shifted out, reaction is carried out continuously.During system shutdown, fused salt is cooled to 200 DEG C, and whole fused salt is put into fused salt tank.
Acrolein reaction device fused salt concrete operations data are as follows:
Solid fused salt melts in fused salt tank, and fusion temperature is 150 DEG C, after squeezing into reactor F1, F2, first heats fused salt with electric heater by submerged pump, and heating temperature of molten salt to 200 DEG C, then turns off electrical heating.Start logical material.Reactor reaction section F1 fused salt operating pressure is 0.07MPa, and fused salt operating temperature is 305 ~ 340 DEG C, and normal production reactor fused salt radial temperature difference is 1 ~ 2 DEG C, and reactor fused salt axial temperature difference is 2 ~ 3 DEG C; Reactor quench zone F2 fused salt operating pressure is 0.07MPa, and fused salt operating temperature is 250 ~ 260 DEG C, and normal production quench zone fused salt axial temperature difference is 10 DEG C.When reaction stopping or overhaul of the equipments, fused salt is cooled to about 200 DEG C, puts into fused salt tank, use when next time drives.
Claims (2)
1. acrolein oxidation reaction heat shifts out method, comprises reactor and two cover fused salt adjusters, it is characterized in that the conversion zone of a set of coupled reaction device, the quench zone of a set of coupled reaction device; Drum is provided with between two cover adjusters; Open conversion zone axial-flow pump (2), fused salt ring cavity entrance (A2) under reactor reaction section (F1) is entered, export (A1) through deflection plate from upper ring cavity to flow out, control through conversion zone guiding valve (4) the fused salt amount entering conversion zone boiler (3), form one and independently circulate; The circulatory system of the fused salt adjuster of the quench zone (F2) of coupled reaction device is: open quench zone axial-flow pump (5), fused salt ring cavity entrance (A8) under reactor quench zone (F2) is entered, export (A7) through deflection plate from upper ring cavity to flow out, enter quench zone axial-flow pump (5) top, control with quench zone guiding valve (7) the fused salt amount entering quench zone boiler (6), form one and independently circulate; Reactor reaction section (F1) fused salt operating pressure is 0.07MPa, and fused salt operating temperature is 305 ~ 340 DEG C, and normal production reactor fused salt radial temperature difference is 1 ~ 2 DEG C, and reactor fused salt axial temperature difference is 2 ~ 3 DEG C; Reactor quench zone (F2) fused salt operating pressure is 0.07MPa, and fused salt operating temperature is 250 ~ 260 DEG C, and normal production quench zone fused salt axial temperature difference is 10 DEG C; When reaction stopping or overhaul of the equipments, fused salt is cooled to 200 DEG C, puts into fused salt tank, use when next time drives.
2. realize the acrolein oxidation reaction heat moving-out device of the method for claim 1, be made up of 1 reactor, 2 axial-flow pumps, 2 guiding valves, 2 electric heaters, 2 boilers, 1 fused salt tank, 1 submerged pump and 1 drum, after it is characterized in that reactor is fixing, axial-flow pump, guiding valve, electric heater, boiler are connected with reactor, drum is arranged between 2 boilers, higher than reactor head, fused salt tank connects the material pipeline of two axial-flow pumps through submerged pump, the entrance (A3) of conversion zone axial-flow pump, upper ring cavity exports (A1) outlet (A4) mouth with reactor reaction section (F1) respectively, lower ring cavity entrance (A2) mouth connects, the import (A5) of conversion zone guiding valve, upper ring cavity exports (A1) outlet (A6) mouth with reactor reaction section (F1) respectively, lower ring cavity entrance (A2) mouth connects, first entrance (A9) of quench zone axial-flow pump, upper ring cavity exports (A7) first outlet (A10) mouth with reactor quench zone (F2) respectively, lower ring cavity entrance (A8) connects, the outlet (A13) of quench zone guiding valve, entrance (A14) mouth is connected with quench zone axial-flow pump second entrance (A11) respectively, second outlet (A12) mouth connects, drum is provided with the first delivery port (A16) to be connected with conversion zone boiler inlet (A23), drum steam first import (A15) is connected with conversion zone boiler export (A24), drum is provided with the second delivery port (A18) to be connected with quench zone boiler inlet (A21), drum steam second import (A17) is connected with quench zone boiler export (A22).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310524228.6A CN103537243B (en) | 2013-10-30 | 2013-10-30 | Acrolein oxidation reaction heat moving-out device and method |
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|---|---|---|---|
| CN201320677039.8U CN203540518U (en) | 2013-10-30 | 2013-10-30 | Device for removing reaction heat generated in acrolein oxidation |
| CN201310524228.6A CN103537243B (en) | 2013-10-30 | 2013-10-30 | Acrolein oxidation reaction heat moving-out device and method |
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| CN103537243B true CN103537243B (en) | 2015-11-11 |
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| CN201310524228.6A Active CN103537243B (en) | 2013-10-30 | 2013-10-30 | Acrolein oxidation reaction heat moving-out device and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103933916A (en) * | 2014-04-04 | 2014-07-23 | 金发科技股份有限公司 | Heating-cooling method and heating-cooling system utilizing fused salt as carrier |
| CN104437270B (en) * | 2014-11-14 | 2017-06-09 | 中国石油集团东北炼化工程有限公司吉林设计院 | Acrylic acid reaction system |
| CN107721786A (en) * | 2017-11-23 | 2018-02-23 | 魏艳娟 | A kind of alkylated reaction equipment and alkylation |
| CN112650327B (en) * | 2020-12-17 | 2022-06-24 | 浙江中控技术股份有限公司 | Temperature runaway prevention control system and method for electric heating tubular reactor |
| CN113432111B (en) * | 2021-08-25 | 2021-11-16 | 山东蓝湾新材料有限公司 | Automatic change heat recovery unit in propylene oxidation legal system acrylic acid production line |
| CN114797691B (en) * | 2022-05-09 | 2024-02-27 | 漳州市龙文翰苑化工有限公司 | Oxidation reactor and process for formaldehyde production |
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| JP4553440B2 (en) * | 2000-03-10 | 2010-09-29 | 三菱レイヨン株式会社 | Method for producing methacrylic acid |
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- 2013-10-30 CN CN201320677039.8U patent/CN203540518U/en not_active Expired - Lifetime
- 2013-10-30 CN CN201310524228.6A patent/CN103537243B/en active Active
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| CN201301294Y (en) * | 2008-11-03 | 2009-09-02 | 山东科技大学 | Tube array type epoxy ethane reactor with quench zone |
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| CN103537243A (en) | 2014-01-29 |
| CN203540518U (en) | 2014-04-16 |
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