CN110038498B - Continuous reactor and use method thereof - Google Patents
Continuous reactor and use method thereof Download PDFInfo
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- CN110038498B CN110038498B CN201910237302.3A CN201910237302A CN110038498B CN 110038498 B CN110038498 B CN 110038498B CN 201910237302 A CN201910237302 A CN 201910237302A CN 110038498 B CN110038498 B CN 110038498B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/02—Synthesis of the oxirane ring
- C07D301/03—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds
- C07D301/12—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with hydrogen peroxide or inorganic peroxides or peracids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/04—Compounds containing oxirane rings containing only hydrogen and carbon atoms in addition to the ring oxygen atoms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00027—Process aspects
- B01J2219/00033—Continuous processes
Abstract
The invention discloses a continuous reactor, comprising: the device comprises an upper reaction cavity, a lower reaction cavity, a first feed inlet, a second feed inlet, a water outlet and a product outlet, wherein the upper reaction cavity and the lower reaction cavity are communicated, the first feed inlet and the second feed inlet are connected with the lower reactor, the water distributor is arranged in the upper reaction cavity, the bottom of the water distributor is provided with a water phase outlet, the water phase outlet penetrates through the wall of the upper reaction cavity through a pipeline and is connected with the water outlet, and the product outlet is connected with the upper reaction cavity through an organic phase pipeline and is connected above the water distributor. The continuous reactor effectively solves the problems of separation of oil phase and water phase and circulation of an unreacted system, has the advantages of high reaction efficiency, good selectivity, strong circulation performance and the like, enables fresh materials to react more fully, and effectively inhibits side reaction.
Description
Technical Field
The invention relates to a reactor, in particular to a continuous reactor and a using method thereof, which are particularly suitable for producing styrene oxide by selectively oxidizing styrene.
Background
The mutually insoluble liquid-liquid system is a common reaction system in a chemical process, such as a nitration process of aromatic hydrocarbon, and an organic phase and an acid phase cannot be mutually dissolved and tend to be layered, so that the liquid-liquid reaction needs to fully mix the two liquid phases to ensure mass transfer and reaction between the two phases.
The hydrogen peroxide styrene oxide reaction also belongs to liquid-liquid reaction, and the traditional liquid-liquid reactor (such as a stirred tank reactor) has the defects of limited contact area, longer reaction time and high energy consumption, and meanwhile, the reactor can not effectively treat water generated in the reaction.
The traditional bubbling reactor has low hydrogen peroxide utilization rate, the selectivity of the epoxyethylbenzene is reduced along with the reaction, and the activity of the catalyst can be obviously reduced by water generated by the reaction in a system. In the traditional continuous reaction process, in order to accelerate the reaction speed, turbulent flow is generally required to be formed in the reactor through violent stirring, so that the contact time of gas-liquid or liquid-liquid is short, a large amount of kinetic energy of fluid is not fully utilized, the energy consumption of the reaction process is high, back mixing can be generated in the feeding process, part of fresh materials are taken out after the partial fresh materials are not fully reacted, and the reaction efficiency is reduced. In addition, the longer the fluid phase separation time after the reaction, also affects the overall efficiency of the reaction. Therefore, it is necessary to develop a continuous reactor for producing styrene oxide by selectively oxidizing styrene with high efficiency and high selectivity.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, an object of the present invention is to provide a continuous reactor having a high reaction rate, a high reaction efficiency, and an excellent cycle capacity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a continuous reactor, comprising: an upper reaction cavity, a lower reaction cavity, a first feed inlet, a second feed inlet, a water outlet and a product outlet which are communicated,
the lower reaction cavity is connected with the first feeding hole and the second feeding hole;
a water separator is arranged in the upper reaction cavity, a water phase outlet is arranged at the bottom of the water separator, and the water phase outlet penetrates through the wall of the upper reaction cavity through a pipeline to be connected with the water outlet; and the product outlet is connected with the upper reaction cavity through an organic phase pipeline and is connected above the water separator. After phase separation of the water-oil two-phase mixture after reaction, the water phase below the water separator is discharged through a water outlet through a pipeline, and the oil phase further rises and is discharged through an organic phase pipeline.
Preferably, the water separator further comprises a cooler.
Preferably, the second feed inlet is positioned above the first feed inlet; the lower reaction chamber also comprises a material mixing tank arranged at the upper part in the lower reaction chamber, a circulating feed inlet and a circulating discharge outlet arranged at the lower part of the lower reaction chamber, the circulating discharge outlet is connected with the circulating feed inlet through a circulating pipeline, the circulating pipeline is provided with a circulating pump, and the second feed inlet is connected with an inlet of the material mixing tank; the outlet of the mixing tank is communicated with the interior of the lower reaction cavity, and the circulating feed inlet is connected with the inlet of the mixing tank through a pipeline.
Preferably, the circulating pipeline is further provided with a first heat exchanger.
Preferably, the organic phase conduit is connected to the circulation conduit by a branch conduit.
Preferably, the circulating pipeline is provided with a batching tank, and an outlet of the batching tank is connected with the circulating feed inlet.
Preferably, the branch pipe is connected with the batching tank.
Preferably, a two-phase mixer is further arranged in the lower reaction chamber, an inlet of the two-phase mixer is communicated with an outlet of the material mixing tank, and an outlet of the two-phase mixer is communicated with the bottom of the lower reaction chamber. The reaction materials mixed by the mixing tank further enter a two-phase mixer to be further mixed by internal circulation, fully react and flow upwards.
Preferably, the mixing tank is a jet mixing tank.
Preferably, the dispensing tank is a venturi mixer.
Preferably, a second heat exchanger is further disposed on the organic phase pipeline, and the second heat exchanger is disposed between the wall of the upper reaction chamber and the branch pipe.
Preferably, the volume of the lower reaction chamber is 100L.
Preferably, the inner diameter of the lower reaction chamber is 400 mm.
Preferably, the continuous reactor of the present invention is a continuous reactor for the production of styrene oxide by the selective oxidation of styrene.
A second object of the present invention is to provide a process using the above continuous reactor, said process comprising:
reaction materials are respectively fed into the lower reaction cavity through the first feed inlet and the second feed inlet, the materials are mixed and reacted in the lower reaction cavity, then the materials rise together to enter the upper reaction cavity, and then fall into the water separator for separation; the water phase separated by the water separator is discharged through a water outlet, and the oil phase is discharged through a product outlet.
Preferably, the materials mixed and reacted in the lower reaction cavity sequentially enter the mixing tank through the circulating discharge hole and the circulating pump, and are mixed with the materials entering through the first feed inlet in the mixing tank and then enter the lower reaction cavity to form a circulating flow.
Preferably, at the beginning of the reaction, the products which are out of control are returned to the lower reaction chamber through the branch pipe and the dosing tank for full reaction.
Preferably, the method is a method for producing styrene oxide by selectively oxidizing styrene, and comprises the following steps: feeding a mixed solution of styrene, a solvent and a catalyst into a lower reaction chamber from a first feeding hole, feeding hydrogen peroxide into the lower reaction chamber from a second feeding hole, mixing and reacting the materials in the lower reaction chamber, then lifting the materials together into an upper reaction chamber, and then falling into a water separator for separation; the water phase separated by the water separator is discharged through a water outlet, and the oil phase is discharged through a product outlet.
Preferably, the materials mixed and reacted in the lower reaction cavity sequentially enter the mixing tank through the circulating discharge hole and the circulating pump, and are mixed with the hydrogen peroxide entering from the first feed inlet in the mixing tank and then enter the lower reaction cavity to form a circulating flow.
Preferably, the flow rate of the circulating flow is 4m3/h。
Preferably, the oil phase which is not qualified in the initial reaction flows into the proportioning tank through a branch pipe, and is mixed with the circulating flow for further reaction.
Preferably, the temperature in the lower reaction chamber is controlled to be 90 ℃.
The invention has the beneficial effects that:
the continuous reactor has the comprehensive characteristics of complete mixed flow reaction and oil-water separation integration, has the advantages of high reaction efficiency, good selectivity, superior cycle performance and the like, enables fresh materials to react more fully, and effectively inhibits side reaction.
The continuous reactor has simple structure, good material liquid mixing capability, enhanced mass transfer and heat transfer, and consideration of reaction rate and reaction circulation capability.
The continuous reactor of the invention utilizes the circulation of feed liquid and the separation of oil phase and water phase, greatly improves the heat transfer efficiency and the mass transfer efficiency, has high reaction rate, can greatly reduce the volume of the reactor, and shortens the reaction time. Because the lower reaction chamber and the upper reaction chamber respectively realize the complete mixed flow reaction and the oil-water two-phase separation, the high reaction efficiency is guaranteed, and other side reactions are effectively reduced.
The water-oil two-phase mixture after reaction enters the water separator from the upper edge of the water separator, the fluid speed is very low, the required phase separation time is greatly reduced, and the phase separation effect is obvious.
Drawings
FIG. 1 is a schematic view of a combination of continuous reactors according to the present invention.
Wherein, 1 is a two-phase mixer, 2 is an upper reaction chamber, 3 is a water separator, 4 is a batching tank, 5 is a mixing tank, 6 is a lower reaction chamber, 101 is a first feed inlet, 102 is a second feed inlet, 103 is a circulating discharge outlet, 104 is a circulating feed inlet, 201 is a product outlet, 202 is a water discharge outlet, E1 is a first heat exchanger, E2 is a second heat exchanger, and P1 is a circulating pump.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted", "connected", and "communicating" are to be construed broadly, e.g., as being fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
As shown in fig. 1, a continuous reactor comprises: an upper reaction chamber 2 and a lower reaction chamber 6 which are communicated, a first feed inlet 101, a second feed inlet 102, a drain outlet 202 and a product outlet 201,
the lower reaction chamber 6 is connected with the first feeding hole 101 and the second feeding hole 102;
a water separator 3 is arranged in the upper reaction chamber 2, a water phase outlet is arranged at the bottom of the water separator 3, and the water phase outlet penetrates through the wall of the upper reaction chamber 2 through a pipeline and is connected with the water outlet 202; the product outlet 201 is connected with the upper reaction chamber 2 and above the water separator 3 through an organic phase pipeline. After the phase separation of the water-oil two-phase mixture after the reaction, the water phase below the water separator 3 is discharged through the water outlet 202 by a pipeline, and the oil phase further rises and is discharged through the organic phase pipeline.
The water separator 3 also comprises a cooler.
The second feed inlet 102 is positioned above the first feed inlet 101; the lower reaction chamber 6 further comprises a material mixing tank 5 arranged at the upper part in the lower reaction chamber 6, a circulating feed inlet 104 and a circulating discharge outlet 103 arranged at the lower part of the lower reaction chamber 6, wherein the circulating discharge outlet 103 is connected with the circulating feed inlet 104 through a circulating pipeline, the circulating pipeline is provided with a circulating pump P1, and the second feed inlet 102 is connected with an inlet of the material mixing tank 5; the outlet of the mixing tank 5 is communicated with the interior of the lower reaction cavity 6, and the circulating feed inlet 104 is connected with the inlet of the mixing tank 5 through a pipeline.
The circulating pipeline is also provided with a first heat exchanger E1.
The organic phase pipeline is connected with the circulating pipeline through a branch pipe.
Be provided with batching jar 4 on the circulating line, branch union coupling batching jar 4, the exit linkage of batching jar 4 circulation feed inlet 104.
The lower reaction cavity 6 is also internally provided with a two-phase mixer 1, an inlet of the two-phase mixer 1 is communicated with an outlet of the material mixing tank 5, and an outlet of the two-phase mixer 1 is communicated with the bottom of the lower reaction cavity 6. The reaction mass mixed via the mixing bowl 5 further enters the two-phase mixer 1 where the annular flow is further mixed, fully reacted and flows upwards.
The mixing tank 5 is a jet mixing tank.
The dosing tank 4 is a venturi mixer.
The organic phase pipeline is also provided with a second heat exchanger E2, and the second heat exchanger E2 is arranged between the wall of the upper reaction chamber 2 and the branch pipe.
The volume of the lower reaction chamber 6 is 100L.
The inner diameter of the lower reaction chamber 6 is 400 mm.
The continuous reactor can be used for the continuous reaction of styrene selective oxidation to produce styrene oxide. The method for producing styrene oxide by selectively oxidizing styrene comprises the following steps:
feeding 20kg/h of fresh materials of 40 percent of styrene, 1 percent of solvent (DMF, dioxane or acetonitrile) and catalyst (cobalt acetate, manganese acetate or cobalt naphthenate) into a lower reaction cavity from a first feed inlet, feeding hydrogen peroxide into the lower reaction cavity from a second feed inlet, mixing and reacting the materials in the lower reaction cavity at the reaction temperature of 90 ℃, then raising the materials together to enter an upper reaction cavity, and then falling into a water separator for separation; the water phase separated by the water separator is discharged through a water outlet, and the oil phase is discharged through a product outlet.
The materials mixed and reacted in the lower reaction cavity sequentially enter the mixing tank through the circulating discharge hole and the circulating pump, and are mixed with hydrogen peroxide entering through the first feed inlet in the mixing tank and then enter the lower reaction cavity to form a circulating flow.
The flow rate of the circulating flow is 4m3/h。
When the reaction is started, the unqualified oil phase flows into the proportioning tank through the branch pipe, is mixed with the circulating flow, and is further reacted.
The water separator in the upper reaction cavity cools the oil and water, and after layering, the water phase is discharged from the water outlet 202, the conversion rate of styrene is 98.9% and the selectivity of styrene oxide is 99% in the whole reaction process.
Claims (9)
1. A continuous reactor, comprising: an upper reaction cavity, a lower reaction cavity, a first feed inlet, a second feed inlet, a water outlet and a product outlet which are communicated,
the lower reaction cavity is connected with the first feeding hole and the second feeding hole;
a water separator is arranged in the upper reaction cavity, a water phase outlet is arranged at the bottom of the water separator, and the water phase outlet penetrates through the wall of the upper reaction cavity through a pipeline to be connected with the water outlet; the product outlet is connected with the upper reaction cavity through an organic phase pipeline and is connected above the water separator; the second feed inlet is positioned above the first feed inlet; the lower reaction chamber also comprises a material mixing tank arranged at the upper part in the lower reaction chamber, a circulating feed inlet and a circulating discharge outlet arranged at the lower part of the lower reaction chamber, the circulating discharge outlet is connected with the circulating feed inlet through a circulating pipeline, the circulating pipeline is provided with a circulating pump, and the second feed inlet is connected with an inlet of the material mixing tank; the outlet of the mixing tank is communicated with the interior of the lower reaction cavity, and the circulating feed inlet is connected with the inlet of the mixing tank through a pipeline.
2. The continuous reactor according to claim 1, wherein the circulation conduit is further provided with a first heat exchanger.
3. The continuous reactor of claim 1, wherein the circulation pipeline is provided with a dosing tank, and an outlet of the dosing tank is connected with the circulation feed inlet.
4. Continuous reactor according to claim 1, characterized in that the organic phase conduit is connected to the circulation conduit by a branch conduit.
5. Continuous reactor according to claim 4, characterized in that the organic phase conduit is further provided with a second heat exchanger arranged between the wall of the upper reaction chamber and the branch pipe.
6. The continuous reactor according to claim 1, wherein a two-phase mixer is further arranged in the lower reaction chamber, an inlet of the two-phase mixer is communicated with an outlet of the mixing tank, and an outlet of the two-phase mixer is communicated with the bottom of the lower reaction chamber.
7. Continuous reactor according to claim 1, characterised in that the mixing bowl is a jet mixing bowl.
8. The continuous reactor according to any one of claims 1 to 7, wherein the continuous reactor is a continuous reactor for the selective oxidation of styrene to produce styrene oxide.
9. A method of using the continuous reactor of any of claims 1-8, the method comprising:
reaction materials are respectively fed into the lower reaction cavity through the first feed inlet and the second feed inlet, the materials are mixed and reacted in the lower reaction cavity, then the materials rise together to enter the upper reaction cavity, and then fall into the water separator for separation; the water phase separated by the water separator is discharged through a water outlet, and the oil phase is discharged through a product outlet.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810380819 | 2018-04-25 | ||
| CN2018103808193 | 2018-04-25 |
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| CN110038498A CN110038498A (en) | 2019-07-23 |
| CN110038498B true CN110038498B (en) | 2021-09-28 |
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| CN104080760A (en) * | 2012-09-28 | 2014-10-01 | Lg化学株式会社 | Apparatus and method for preparing alcohol from olefin |
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| CN205995420U (en) * | 2016-08-04 | 2017-03-08 | 中石化南京工程有限公司 | A kind of bubble-liquid two-phase jet reactor and bubble-liquid two-phase jet reaction system |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013072147A1 (en) * | 2011-11-14 | 2013-05-23 | Evonik Degussa Gmbh | Method and device for the separation of acidic gases from a gas mixture |
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- 2019-03-27 CN CN201910237302.3A patent/CN110038498B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104080760A (en) * | 2012-09-28 | 2014-10-01 | Lg化学株式会社 | Apparatus and method for preparing alcohol from olefin |
| CN104415711B (en) * | 2013-08-26 | 2016-12-28 | 黄志忠 | The device of methanol carbonyl oxidative synthesis dimethyl carbonate |
| CN104098474A (en) * | 2014-07-28 | 2014-10-15 | 淮安嘉诚高新化工股份有限公司 | Device and method for producing methyl aniline through performing continuous liquid-phase catalytic hydrogenation reduction on nitrotoluene |
| CN205412975U (en) * | 2016-04-01 | 2016-08-03 | 浙江衢州正邦有机硅有限公司 | Converter suitable for gather methyl triethoxysilane serialization production technology |
| CN205761194U (en) * | 2016-04-26 | 2016-12-07 | 江苏安邦电化有限公司 | A kind of venturi type recirculation loop reactor for continuous prodution ethephon |
| CN106039916A (en) * | 2016-07-26 | 2016-10-26 | 北京华福工程有限公司 | System of lowering content of waste gas in solution polymerization rubber process |
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| CN110038498A (en) | 2019-07-23 |
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