CN103537243A - Device and method for removing reaction heat in acrolein oxidation - Google Patents
Device and method for removing reaction heat in acrolein oxidation Download PDFInfo
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- CN103537243A CN103537243A CN201310524228.6A CN201310524228A CN103537243A CN 103537243 A CN103537243 A CN 103537243A CN 201310524228 A CN201310524228 A CN 201310524228A CN 103537243 A CN103537243 A CN 103537243A
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Abstract
The invention discloses a device and method for removing reaction heat in a process of generating acrolein by oxidization reaction of propylene. The device comprises a reactor and two sets of fused salt regulators, wherein one set of the fused salt regulators is connected with a reaction section of the reactor, and another set of the fused slat regulators is connected with a quenching section of the reactor; a steam drum is arranged between the two sets of regulators. The method comprises the following steps: starting an axial flow pump in the reaction section; feeding the fused salt through an inlet A2 of an F1 bottom ring cavity in the reaction section of the reactor; enabling the fused salt to flow through a baffle plate and then flow out of an outlet A1 of an upper ring cavity; controlling the quantity of fused salt entering a boiler in the reaction section through a slide valve in the reaction section, in order to form an independent cycle; starting another axial flow pump in the quenching section; feeding the fused salt through an inlet A8 of an F2 bottom ring cavity in the quenching section of the reactor; enabling the fused salt to flow through the baffle plate and then flow out of an outlet A7 of the upper ring cavity and finally flow into the upper part of the axial flow pump; and controlling the quantity of the fused salt entering another boiler in the quenching section through a slide valve in the quenching section, in order to form another independent cycle. The method is characterized in that the two sets of fused salt regulators are adopted for respectively controlling the temperature of the reaction section and the quenching section; the temperature difference between the two sections is 50 to 80 DEG C; the regulation is flexible and convenient; no interference appears between the two sections.
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, is the cacodorous liquid of water white transparency under normal conditions, and 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 synthetic 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: abroad as oil-field flooding bactericide, to suppress the growth of bacterium in water, prevent that bacterium from causing corrosion and stopping up 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 and shifts out heat with inorganic high-temp heat carrier fused salt, strict control system temperature.On the one hand, require to select in the running suitable reaction temperature strict its fluctuation range of controlling, on the other hand, pay special attention to beds, especially the temperature of focus and being controlled in safe range with the difference of reaction temperature, to avoid " temperature runaway " and catalyst is caused damage, adopt an effective measure the reacting gas temperature of reacting section catalyst bed outlet is down to rapidly below 260 ℃, to suppress the automatic depth oxidation of methacrylaldehyde.
At present, the acrolein reaction device of domestic 5000 tons/year of scales adopts as shown in Figure 1, in reactor, between conversion zone F1 and quench zone F2, is provided with tube sheet 11; Adopt a set of fused salt control system, conversion zone F1 and quench zone F2 regulate facility with a set of fused salt, 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, with steam by after 150 ℃ of thawings of fused salt, fused salt is squeezed into the upper ring cavity of reactor F1 by the fused salt submerged pump on fused salt tank, by axial-flow pump 2, fused salt is circulated respectively in reactor reaction section F1 and boiler 3, reactor quench zone F2, controlling reaction temperature is exactly by adjusting, to flow into the flow rate of molten salt of boiler 3, open the hot water valve V1 of boiler 3, from boiler, 3 hot water inlet A12 enter, steam flows out through valve V2 from boiler 3 steam (vapor) outlet A11, and reaction heat is removed heat by producing steam.Electric heater uses before driving, and makes temperature of molten salt be heated to 200 ℃ of left and right, drops into after material, and electric heater is turned off.Two sections of conversion zone F1 and quench zone F2 only have and raise simultaneously or reduce temperature, by control valve, control the fused salt amount in inflow boiler, and the temperature of quench zone F2 is uncontrollable, is that the passive variation with conversion zone F1 temperature changes.The temperature difference of two sections and gradient of temperature degree 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 shifting out effectively in time heat, solve and overcome the security hidden trouble of above-mentioned existence, improve methacrylaldehyde productive rate, is the key issue existing 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 existing in production process, improves the economic benefit of methacrylaldehyde process units.
Technical scheme of the present invention is as follows:
Reaction heat shifts out a system, comprises reactor and two cover fused salt adjusters, the conversion zone F1 of a set of coupled reaction device, the drum 10 of the quench zone F2 of a set of coupled reaction device and 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, through deflection plate, from upper ring cavity outlet A1, flow out, through conversion zone guiding valve 4, control the fused salt amount that enters conversion zone boiler 3, form an independently circulation; 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, through deflection plate, from upper ring cavity outlet A7, flow out, enter axial-flow pump 5 tops, with quench zone guiding valve 7, control the fused salt amount that enters quench zone boiler 6, form an independently circulation.
When reaction starts, solid fused salt is put into fused salt tank, with steam, by after 150 ℃ of thawings of fused salt, with the submerged pump 8 on fused salt tank, squeeze in conversion zone axial-flow pump 2 and quench zone axial-flow pump 5, make conversion zone F1 and quench zone F2 be full of fused salt.
The concrete device of native system is: 1 reactor, 2 axial-flow pumps, 2 guiding valves, 2 electric heaters, 2 boilers, 1 fused salt tank, 1 submerged pump and 1 drum, consist of.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 the upper ring cavity of reactor reaction section F1 respectively, lower ring cavity entrance A2 mouth connects, the outlet A5 of conversion zone guiding valve 4, import A6 mouth respectively with reactor on ring cavity outlet A1, lower ring cavity entrance A2 mouth connects, the entrance A9 of axial-flow pump 5, outlet A10 mouth is gone up ring cavity entrance A7 with reactor quench zone F2 respectively, 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, on drum, being provided with the water outlet A 16 being connected with conversion zone boiler 3 is connected with import A23, drum steam inlet A15 with outlet A24 be connected, on drum, be provided with the water outlet A 18 being connected with quench zone boiler 6 and be connected with import A21, drum steam inlet A17 and outlet A22.
By two cover fused salt adjusters, control respectively the temperature of conversion zone and quench zone.Two sections of temperature differ 50～80 ℃, flexible adjustment, convenience, do not interfere with each other.
At conversion zone axial-flow pump 2, with on quench zone axial-flow pump 5, the pipeline that is connected fused salt tank is set respectively, when reaction starts, solid fused salt is put into fused salt tank, after 150 ℃ of fused salts being melted with steam, fused salt is squeezed into the upper ring cavity of reactor reaction section F1 and reactor quench zone F2 base ring chamber 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, and fused salt is entered at reactor reaction section F1 base ring chamber A2 mouth, through deflection plate, from upper ring cavity A1 mouth, goes out, with guiding valve 4, automatically control the fused salt amount that enters 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; With guiding valve 7, automatically control the fused salt amount that enters 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.
Employing said method reaches conversion zone and quench zone is controlled respectively effect, and the heat that has solved conversion zone shifts out the problem on the impact of the safety in production of device in time.Main is to have got rid of potential safety hazard, guarantees 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.
The specific embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail:
According to content as described in Figure 3, after forming and 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 the upper ring cavity of reactor reaction section F1 respectively, lower ring cavity entrance A2 mouth connects, the outlet A5 of conversion zone guiding valve 4, import A6 mouth respectively with reactor on ring cavity outlet A1, lower ring cavity entrance A2 mouth connects, the entrance A9 of axial-flow pump 5, outlet A10 mouth is gone up ring cavity entrance A7 with reactor quench zone F2 respectively, 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, on drum, being provided with the water outlet A 16 being connected with conversion zone boiler 3 is connected with import A23, drum steam inlet A15 with outlet A24 be connected, on drum, be provided with the water outlet A 18 being connected with quench zone boiler 6 and 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, through deflection plate, from upper ring cavity outlet A1, flow out, through conversion zone guiding valve 4, control the fused salt amount that enters conversion zone boiler 3, form an independently circulation; 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, through deflection plate, from upper ring cavity outlet A7, flow out, enter axial-flow pump 5 tops, with quench zone guiding valve 7, control the fused salt amount that enters quench zone boiler 6, form an independently circulation.
By fused salt pipeline, go up salt pipeline, unload fused salt pipeline between salt pipeline and each equipment and connect, A15 mouth by submerged pump 8 goes out fused salt, enter respectively the A3 mouth of axial-flow pump 2 and the A11 mouth of axial-flow pump 5, 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 are carried out provision for thermal insulation.
Before driving, first solid fused salt is put into fused salt tank, after with steam, 150 ℃ of fused salts being melted, fused salt is squeezed into the upper ring cavity of 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 200 ℃ of left and right, drop into after material, electric heater is turned off.
All fused salts all melt in fused salt tank, with submerged pump, fused salt is squeezed on conversion zone in ring cavity and quench zone axial-flow pump, before driving, first with electric heater separately, fused salt in reactor is heated to 200 ℃ of left and right, 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, by venthole A20, through V2 valve, export steam, fused salt heat is shifted out, reaction is carried out continuously.During system shutdown, fused salt is cooled to 200 ℃, and whole fused salts are 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 ℃, by submerged pump, is squeezed into after reactor F1, F2, first with electric heater, heats fused salt, and heating temperature of molten salt to 200 ℃, 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 ℃, and normally producing reactor fused salt radial temperature difference is 1～2 ℃, and reactor fused salt axial temperature difference is 2～3 ℃; Reactor quench zone F2 fused salt operating pressure is 0.07MPa, and fused salt operating temperature is 250～260 ℃, and normally producing quench zone fused salt axial temperature difference is 10 ℃.Reaction stops or during overhaul of the equipments, fused salt is cooled to 200 ℃ of left and right, puts into fused salt tank, when driving next time, uses.
Claims (3)
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; Between two cover adjusters, be provided with drum.
2. the method for claim 1, the circulatory system of the fused salt adjuster of the conversion zone of its feature 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, through deflection plate, from upper ring cavity outlet A1, flow out, through conversion zone guiding valve 4, control the fused salt amount that enters conversion zone boiler 3, form an independently circulation; 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, through deflection plate, from upper ring cavity outlet A7, flow out, enter axial-flow pump 5 tops, with quench zone guiding valve 7, control the fused salt amount that enters quench zone boiler 6, form an independently circulation.
3. realize the acrolein oxidation reaction heat moving-out device of the method for claim 1, 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, formed, 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 axial-flow pump, outlet A4 mouth exports A1 with the upper ring cavity of reactor reaction section F1 respectively, lower ring cavity entrance A2 mouth connects, the outlet A5 of conversion zone guiding valve, import A6 mouth respectively with reactor on ring cavity outlet A1, lower ring cavity entrance A2 mouth connects, the entrance A9 of axial-flow pump, outlet A10 mouth is gone up ring cavity entrance A7 with reactor quench zone F2 respectively, lower ring cavity outlet A8 connects, the outlet A13 of quench zone guiding valve, entrance A14 mouth respectively with axial-flow pump entrance A11, outlet A12 mouth connects, on drum, being provided with the water outlet A 16 being connected with conversion zone boiler is connected with import A23, drum steam inlet A15 with outlet A24 be connected, on drum, be provided with the water outlet A 18 being connected with quench zone boiler and be connected with import A21, drum steam inlet A17 and outlet 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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| CN103537243A true CN103537243A (en) | 2014-01-29 |
| CN103537243B 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104437270A (en) * | 2014-11-14 | 2015-03-25 | 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 |
| CN112650327A (en) * | 2020-12-17 | 2021-04-13 | 浙江中控技术股份有限公司 | Temperature runaway prevention control system and method for electric heating tubular reactor |
| CN114797691A (en) * | 2022-05-09 | 2022-07-29 | 漳州市龙文翰苑化工有限公司 | Oxidation reactor and process for formaldehyde production |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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2013
- 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104437270A (en) * | 2014-11-14 | 2015-03-25 | 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 |
| CN112650327A (en) * | 2020-12-17 | 2021-04-13 | 浙江中控技术股份有限公司 | Temperature runaway prevention control system and method for electric heating tubular reactor |
| CN114797691A (en) * | 2022-05-09 | 2022-07-29 | 漳州市龙文翰苑化工有限公司 | Oxidation reactor and process for formaldehyde production |
| 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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| Publication number | Publication date |
|---|---|
| CN103537243B (en) | 2015-11-11 |
| CN203540518U (en) | 2014-04-16 |
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