CN213506679U - Micro-interface reinforced cyclohexanone ammoximation reaction system - Google Patents
Micro-interface reinforced cyclohexanone ammoximation reaction system Download PDFInfo
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- CN213506679U CN213506679U CN202020532558.5U CN202020532558U CN213506679U CN 213506679 U CN213506679 U CN 213506679U CN 202020532558 U CN202020532558 U CN 202020532558U CN 213506679 U CN213506679 U CN 213506679U
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 82
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000006146 oximation reaction Methods 0.000 claims abstract description 72
- 239000007788 liquid Substances 0.000 claims abstract description 50
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000010521 absorption reaction Methods 0.000 claims abstract description 42
- 239000012528 membrane Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
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- 238000007599 discharging Methods 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 abstract description 18
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 abstract description 18
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000047 product Substances 0.000 abstract description 9
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- 238000005265 energy consumption Methods 0.000 description 9
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 5
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- 230000005501 phase interface Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
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- 229910001220 stainless steel Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
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- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
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Abstract
The utility model provides a cyclohexanone ammoximation reaction system is reinforceed to micro-interface, including oximation reactor, reaction clear solution buffer tank, tail gas absorption tower and micro-interface generator, wherein, oximation reactor includes feed inlet, discharge gate, tail gas outlet, and the outside is provided with extrinsic cycle heat transfer device, and micro-interface generator is connected with the feed inlet for the diameter is the microbubble of micron level for the dispersion broken ammonia; the discharge hole is connected with the reaction clear liquid buffer tank; the tail gas outlet is connected with the tail gas absorption tower, the bottom of the tail gas absorption tower is also provided with an absorption liquid outlet, and the absorption liquid outlet is connected with the micro-interface generator and is used for returning the absorption liquid to the oximation reactor for utilization. The utility model effectively inhibits the side reaction, fully improves the efficiency of the oximation reaction and reduces the production cost of enterprises; on the other hand, the reaction temperature and pressure are reduced, the decomposition products of cyclohexanone and cyclohexanone oxime are reduced, and the yield and quality of the final product caprolactam are improved.
Description
Technical Field
The utility model belongs to the technical field of the intensive reaction, concretely relates to cyclohexanone ammoximation reaction system is reinforceed to micro-interface.
Background
The process for preparing cyclohexanone oxime at present mainly adopts cyclohexanone, ammonia and hydrogen peroxide under the condition of low pressure, uses tert-butyl alcohol as solvent and titanium silicon molecular sieve as catalyst, and synthesizes cyclohexanone oxime in a reactor by one step, and the reaction formula is as follows: NH (NH)3+H2O2+C6H10O＝C6H11ON+2H2The method for preparing cyclohexanone oxime by the cyclohexanone ammoximation method is simple, does not produce ammonium sulfate as a byproduct, and has no difficult problem of environmental protection, so the method is favored by the caprolactam industry in recent years, but the cyclohexanone ammoximation reaction is not difficult to find in recent production and has the following problems: on one hand, the prior oximation reactor has limited gas-liquid phase mass transfer area, and in the reaction process, reaction mixed raw materials and ammonia gas can not be fully mixed, so that the cyclohexanone is incompletely converted, the oximation conversion rate is low, and the occurrence of side reaction is increased(ii) a On the other hand, the ammoximation reaction is a strong exothermic reaction (301KJ/mol), the temperature is too high, the decomposition products of cyclohexanone and cyclohexanone oxime are increased, and the products are not easy to remove in the post-process, and the yield and the quality of the final product caprolactam are influenced.
Therefore, it is urgent and necessary to fully improve the efficiency of the oximation reaction, suppress the occurrence of side reactions, and reduce the production cost under the existing technical and equipment conditions.
SUMMERY OF THE UTILITY MODEL
In view of this, the first objective of the present invention is to provide a micro-interface enhanced cyclohexanone ammoximation reaction system, which can increase the phase interface area between ammonia and liquid phase material by setting a micro-interface generator before the oximation reactor, so that ammonia and liquid phase material can be fully crushed and mixed before entering the reactor, the mass transfer space is fully satisfied, the residence time of ammonia in liquid phase is increased, thereby greatly improving oximation reaction efficiency, effectively inhibiting side reactions, and significantly reducing energy consumption in the reaction process; on the other hand, the reaction temperature and pressure are reduced, the decomposition products of cyclohexanone and cyclohexanone oxime are reduced, the yield and quality of the final product caprolactam are improved, the energy consumption is reduced, and the system safety is improved.
A second object of the present invention is to provide a method for intensifying cyclohexanone ammoximation reaction system by using the above-mentioned micro-interface to perform oximation reaction, wherein the operating conditions of the method are milder, the temperature and pressure of oximation reaction are reduced while the reaction efficiency is ensured, and the safety performance is high and the energy consumption is low, thereby achieving better reaction effect than the prior art.
In order to realize the above purpose of the utility model, the following technical scheme is adopted:
the utility model provides a micro-interface reinforced cyclohexanone ammoximation reaction system, which is characterized by comprising an oximation reactor, a reaction clear liquid buffer tank, a tail gas absorption tower and a micro-interface generator, wherein,
the oximation reactor comprises a feeding hole, a discharging hole and a tail gas outlet, an external circulation heat exchange device is arranged outside the oximation reactor, one end of the external circulation heat exchange device is connected with the bottom of the oximation reactor, and the other end of the external circulation heat exchange device is connected with the micro-interface generator; the micro-interface generator is connected with the feeding hole and is used for dispersing and crushing ammonia gas into micro-bubbles with the diameter of micron level; the discharge hole is connected with the reaction clear liquid buffer tank; the tail gas outlet is connected with the tail gas absorption tower, the bottom of the tail gas absorption tower is also provided with an absorption liquid outlet, and the absorption liquid outlet is connected with the micro-interface generator and is used for enabling absorption liquid to be reused in the oximation reactor.
In the prior art, the cyclohexanone ammoximation reaction has the following problems: on one hand, the gas-liquid phase mass transfer area of the existing oximation reactor is limited, the reaction mixed raw materials and ammonia gas cannot be fully mixed in the reaction process, so that the cyclohexanone is incompletely converted, the oximation conversion rate is low, and the occurrence of side reactions is increased; on the other hand, the ammoximation reaction is a strong exothermic reaction (301KJ/mol), the temperature is too high, the decomposition products of cyclohexanone and cyclohexanone oxime are increased, and the products are not easy to remove in the post-process, and the yield and the quality of the final product caprolactam are influenced. The utility model discloses a cyclohexanone ammoximation reaction system is reinforceed to micro-interface sets up the micro-interface generator through before oximation reactor, can increase the phase boundary area between ammonia and the liquid phase material on the one hand for ammonia and liquid phase material are fully broken before getting into the reactor and are mixed, and the mass transfer space fully satisfies, has increased the dwell time of ammonia in the liquid phase, thereby improves oximation reaction efficiency by a wide margin, effectively suppresses the side reaction, is showing the energy consumption that reduces the reaction process; on the other hand, the reaction temperature and pressure are reduced, the decomposition products of cyclohexanone and cyclohexanone oxime are reduced, the yield and quality of the final product caprolactam are improved, the energy consumption is reduced, and the system safety is improved.
Further, the micro-interface generator is one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator or a gas-liquid linkage micro-interface generator. The pneumatic micro-interface generator is driven by gas, and the input gas quantity is far larger than the liquid quantity; the hydraulic micro-interface generator is driven by liquid, and the input air quantity is generally smaller than the liquid quantity; the gas-liquid linkage type micro-interface generator is driven by gas and liquid together.
As preferred, among the utility model micro-interface generator be pneumatic micro-interface generator, the ammonia lets in pneumatic micro-interface generator's inside dispersion and breaks into micron level's microbubble, the effectual mass transfer area that has increased between ammonia and the liquid phase material reduces the mass transfer resistance, improves reaction efficiency.
Further, the micron-scale range is more than or equal to 1 μm and less than 1mm, ammonia gas enters a micro-interface generator before entering the oximation reactor, and micro-bubbles with the diameter more than or equal to 1 μm and less than 1mm are formed through crushing so as to improve the mass transfer area between the gas phase and the liquid phase and form a micro-interface.
Further, the micro-interface generator comprises a shell, a gas phase inlet, a liquid phase inlet and an emulsion outlet, wherein the shell can be in a drum shape, a spherical shape or a spherical shape; the gas phase inlet is positioned at the central position above the shell, the liquid phase inlet is positioned around the shell, gas is fully emulsified with liquid after being dispersed and crushed to form emulsion, and the emulsion outlet is positioned at the central position below the shell; the emulsion outlet is connected with the feed inlet of the oximation reactor in a welding, threaded or flange mode.
Furthermore, the setting mode, the setting position and the number of the micro-interface generator are not limited; in addition, more preferably, the number of the micro interface generators is more than one, and a plurality of micro interface generators can be arranged in series or in parallel, and all the micro interface generators can be arranged before the oximation reactor.
Further, the tail gas absorption tower comprises a tower body and a tower kettle, wherein the tower body is filled with filler, the diameter of the tower kettle is larger than that of the tower body, and the height of the tower kettle is lower than that of the tower body. In order to ensure that gas and liquid phases are contacted more fully and the heat distribution is more uniform, the tower body is filled with a filler, the material of the filler can be corrosion-resistant stainless steel or polytetrafluoroethylene, and the type of the filler can be a stepped ring, a pall ring, a column ring, a stainless steel wire mesh and the like; the diameter of the tower kettle is larger than that of the tower body, because the inner space of the tower kettle is large, gas diffusion is facilitated, the space of the tower body is small, and gas centralized adsorption is facilitated; the height of the tower kettle is lower than that of the tower body, the lower the height of the tower kettle is, the shorter the retention time of the materials in the tower kettle is, and thus, the materials can be prevented from coking.
Further, the outer circulation device comprises a circulation pipeline, and a full-automatic adjusting condenser and a circulation pump are distributed on the circulation pipeline. The ammoximation reaction is a strong exothermic reaction, no external heat is needed in the normal oximation reaction, the reaction heat energy maintains the heat needed in the continuous reaction process, the redundant heat energy causes the temperature rise of materials in the reactor, the temperature in the reaction process is controlled by arranging a circulating pipeline, the circulating pipeline can quickly and automatically cool the circulating materials by arranging a full-automatic adjusting condenser, a control module and a temperature module are arranged in the full-automatic adjusting condenser, the temperature module can monitor the temperature of the circulating materials at any time, the control module sends an instruction according to a signal fed back by the temperature module to realize full-automatic adjustment, in addition, a circulating pump is also arranged on the circulating pipeline, the circulating pump can be vertical or horizontal, the number of pump bodies is not limited, and one or more circulating power pumps can be installed in series or parallel to increase the circulating power.
Furthermore, a metal membrane filter is arranged in the oximation reactor and used for separating the catalyst, the metal membrane filter is made of 304 stainless steel, the metal membrane filter is arranged in the oximation reactor in a double-layer or single-layer membrane stack mode, 1-10 groups of membrane stacks are uniformly distributed in the same plane of the reactor on each layer, the filtering precision of the metal membrane in the metal membrane filter is 0.05-5 mu m, compared with other membrane filters, the metal membrane filter is internally arranged, the catalytic reaction and separation efficiency is improved, meanwhile, the leakage of the catalyst is avoided, and the system safety is improved; preferably, the metal membrane filter can also be designed with a back cleaning device, and the cleaning port can be cleaned by purging the filter, so that the metal membrane filter can be repeatedly used, and the service life of the filter can be prolonged.
Furthermore, the oximation reactor is internally provided with a double-coil heat exchanger, the double-coil heat exchanger comprises a cooling coil and a steam heating coil, the cooling coil is positioned on the upper part of the steam heating coil, and compared with other heat exchangers, the double-coil heat exchanger has the advantages of higher pressure, larger heat dissipation area and better cooling effect in the oximation reactor.
Further, an external filtering device is arranged on a connecting pipeline between the reaction clear liquid buffer tank and the discharge hole so as to prevent the catalyst from entering the subsequent working procedures after the built-in metal membrane filter is damaged.
Furthermore, an exhaust gas cooler is arranged on a connecting pipeline between the tail gas absorption tower and the tail gas outlet, so that non-condensable gas can be cooled, the utilization rate of on-site tail gas recovery is improved, and energy is saved.
Furthermore, the reaction clear liquid buffer tank is an air bag type buffer tank, an integral air bag is arranged in the air bag type buffer tank, and the reaction clear liquid only enters the air bag when working and does not contact with the shell in the reactor, so that the whole oximation reactor is prevented from rusting.
Furthermore, the oximation reactor is a turbine stirring tank type reactor, the turbine stirring speed is high, when the energy consumption is low, the stirring efficiency is high, strong radial flow can be generated, the reaction materials in the reactor are uniformly dispersed, and the phenomenon of gas emptying cannot occur.
In addition, the utility model also provides an oximation reaction method, including the following step:
ammonia gas is firstly sent into a micro-interface generator to be dispersed and broken into micro bubbles before being introduced into an oximation reactor;
the liquid phase material enters a micro interface generator to be fully emulsified with the dispersed and crushed micro bubbles, and then enters an oximation reactor through a feed inlet to carry out oximation reaction;
in the reaction process, unreacted ammonia, alcohol and other gases enter the tail gas absorption tower from the tail gas outlet for recycling, and reaction products enter the reaction clear liquid buffer tank through the discharge hole in a clear liquid mode for later treatment.
Furthermore, the temperature in the oximation reactor is 81-83 ℃, and the pressure is 0.15-0.2 MPa.
Compared with the prior art, the beneficial effects of the utility model reside in that:
the utility model discloses a set up behind the micro-interface generator before the oximation reactor, on the one hand can increase the phase interface area between ammonia and the liquid phase material for ammonia and liquid phase material fully break the mixture before getting into the reactor, and the mass transfer space fully satisfies, has increased the dwell time of ammonia in the liquid phase, thereby improves oximation reaction efficiency by a wide margin, effectively suppresses the side reaction, is showing the energy consumption that reduces reaction process; on the other hand, the operation condition is milder, the temperature and the pressure of the oximation reaction are reduced while the reaction efficiency is ensured, the decomposition products of cyclohexanone and cyclohexanone oxime are reduced, the yield and the quality of the final product caprolactam are improved, the energy consumption is reduced, and the system safety is improved.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic structural diagram of a micro-interface reinforced cyclohexanone ammoximation reaction system provided by an embodiment of the present invention.
Wherein:
a 10-oximation reactor; 11-a feed inlet;
12-a discharge hole; 13-tail gas outlet;
20-reaction clear liquid buffer tank; 30-a tail gas absorption tower;
31-an absorption liquid outlet; 40-a micro-interface generator;
50-an outer filtration device; 60-an exhaust gas cooler;
70-full automatic regulation condenser; 80-circulating pump.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings and detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, 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 meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In order to clarify the technical solution of the present invention, the following description is made in the form of specific embodiments.
Examples
Referring to fig. 1, in order to implement the embodiment of the present invention, a micro-interface reinforced cyclohexanone ammoximation reaction system includes an oximation reactor 10, a reaction clear liquid buffer tank 20, a tail gas absorption tower 30 and a micro-interface generator 40, wherein the oximation reactor 10 includes a feed inlet 11, a discharge port 12 and a tail gas outlet 13, an external circulation heat exchange device is disposed outside the oximation reactor 10, one end of the external circulation heat exchange device is connected to the bottom of the oximation reactor 10, the other end of the external circulation heat exchange device is connected to the micro-interface generator 40, and the micro-interface generator 40 is connected to the feed inlet 11 and is used for dispersing and breaking ammonia gas into micro bubbles with a diameter of micron level; the discharge port 12 is connected with the reaction clear liquid buffer tank 20, the tail gas outlet 13 is connected with the tail gas absorption tower 30, the bottom of the tail gas absorption tower 30 is also provided with an absorption liquid outlet 31, and the absorption liquid outlet 31 is connected with the micro-interface generator 40 so as to be used for returning the absorption liquid to the oximation reactor again for utilization.
Specifically, ammonia gas enters the micro-interface generator 40 before being introduced into the oximation reactor 10, is dispersed and crushed into micro-bubbles with the diameter of more than or equal to 1 μm and less than 1mm, meanwhile, a liquid-phase material enters the micro-interface generator 40, the dispersed and crushed micro-bubbles and the liquid-phase material are fully emulsified in the micro-interface generator 40 and then enter the oximation reactor 10 for oximation reaction, so that the mass transfer area between the ammonia gas and the liquid-phase material is effectively increased, the thickness of a liquid film is reduced, the mass transfer resistance is reduced, the energy consumption is effectively reduced, and the reaction efficiency is improved. It is understood that the number of micro-interface generators 40 is not limited, and additional micro-interface generators may be added to increase the dispersion and mass transfer effects, and multiple micro-interface generators may be arranged in series or in parallel before the oximation reactor 10, in this embodiment, the micro-interface generators 40 are pneumatic micro-interface generators.
The reaction mass in the oximation reactor 10 is filtered by a built-in metal membrane filter to realize the separation of the catalyst and the reaction product, and preferably, the oximation reactor 10 may be further provided with a catalyst discharge chute for recovering the deactivated catalyst. Reaction products enter the reaction clear liquid buffer tank 20 through the discharge hole 12 in a clear liquid mode to wait for subsequent treatment, preferably, the reaction clear liquid buffer tank 20 is an air bag type buffer tank, compared with other buffer tanks, an integral air bag is arranged in the reaction clear liquid buffer tank, and the clear liquid only enters the air bag and does not contact with a shell in the reactor during work, so that the whole oximation reactor is prevented from rusting.
In this embodiment, an external filtering device 50 is further disposed on the connecting pipeline between the reaction clear liquid buffer tank 20 and the discharge port 12 to prevent the catalyst from entering the subsequent process after the damage of the metal membrane filter disposed in the reactor. In the reaction process, unreacted gases such as ammonia and alcohol are cooled by the exhaust gas cooler 60 from the exhaust gas outlet 13 and then enter the exhaust gas absorption tower 30 for recycling, the ammonia and the alcohol in the exhaust gas absorption tower 30 are absorbed by desalted water to form absorption liquid, and the absorption liquid is pumped into the micro-interface generator 40 for recycling after coming out from the absorption liquid outlet 31. Specifically, the tail gas absorption tower 30 includes a tower body and a tower kettle, the tower body is filled with filler, the diameter of the tower kettle is larger than that of the tower body, and the height of the tower kettle is lower than that of the tower body, because the internal space of the tower kettle is large, the diffusion of gas is facilitated, the space of the tower body is small, and the concentrated adsorption of the gas is facilitated; the lower the height of the tower kettle, the shorter the retention time of the material in the kettle, thus preventing the material from coking.
In addition, the ammoximation reaction is a strong exothermic reaction, no external heat is needed in the normal oximation reaction, the reaction heat energy maintains the heat needed in the continuous reaction process, the redundant heat energy causes the temperature rise of materials in the reactor, the temperature in the reaction process is controlled by arranging an external circulation device, the external circulation device comprises a circulation pipeline, a full-automatic adjusting condenser 70 is arranged on the circulation pipeline, the full-automatic adjusting condenser 70 can quickly and automatically cool the circulation materials, a control module and a temperature module are arranged in the full-automatic adjusting condenser 70, the temperature module can monitor the temperature of the circulation materials at any time, and the control module sends an instruction according to a signal fed back by the temperature module to realize full-automatic adjustment; in addition, the circulating pipeline is provided with a circulating pump 80, in the embodiment, the circulating pump 80 can be vertical or horizontal, the number of pump bodies is not limited, and one or more circulating pumps can be installed in series or in parallel to increase circulating power.
It is understood that the oximation reactor as the main occurrence site of the oximation reaction is a shell structure, and specifically, the oximation reactor may be: kettle-type reactor, tubular reactor, tower reactor, fixed bed reactor and fluidized bed reactor as long as can guarantee that the oximation reaction can fully react as the reaction chamber of oximation reaction, in this embodiment, oximation reactor 10 is turbine stirred tank reactor, compares other reactors, and stirring speed is big, and reaction material dispersion is even. Preferably, the oximation reactor 10 is further provided therein with a double-coil heat exchanger, which comprises a cooling coil and a steam heating coil, wherein the cooling coil is located at the upper part of the steam heating coil.
The working process and principle of the micro-interface reinforced cyclohexanone ammoximation reaction system of the present invention are briefly described below.
The ammonia gas is firstly fed into the micro-interface generator 40 to be dispersed and crushed into micro-bubbles at the micron level before being fed into the oximation reactor 10, meanwhile, the liquid phase mixed raw materials (including hydrogen peroxide, cyclohexanone, circulating tert-butyl alcohol, circulating materials and the like) are fed into the micro-interface generator 40, and the dispersed and crushed micro-bubbles and the liquid phase mixed raw materials are fully emulsified, so that the mass transfer area of a gas phase and a liquid phase is effectively increased, and the mass transfer resistance is reduced.
The emulsified liquid after being fully emulsified enters an oximation reactor 10 through a feeding hole 11, and oximation reaction is carried out under the action of a catalyst, wherein the temperature in the oximation reactor is 81-83 ℃, and the pressure in the oximation reactor is 0.15-0.2 MPa. Wherein, the ammoximation reaction is a strong exothermic reaction, and the circulating material is rapidly and automatically cooled through the full-automatic adjusting condenser 70 arranged on the outer circulating pipeline, so that the temperature in the reactor is reduced.
In the reaction process, unreacted gases such as ammonia and alcohol enter the tail gas absorption tower 30 after being cooled by the exhaust gas cooler 60 from the tail gas outlet 13, the tail gas absorption tower 30 absorbs the ammonia and the alcohol in the gases by desalted water to form absorption liquid, and the absorption liquid is pumped into the micro-interface generator 40 for recycling after coming out from the absorption liquid outlet 31. The oximation reaction product enters a reaction clear liquid buffer tank 20 through a discharge hole 12 in a clear liquid mode for waiting for subsequent treatment.
The above steps are repeated circularly to make the whole treatment system run smoothly.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention.
Claims (8)
1. A micro-interface reinforced cyclohexanone ammoximation reaction system is characterized by comprising an oximation reactor, a reaction clear liquid buffer tank, a tail gas absorption tower and a micro-interface generator, wherein,
the oximation reactor comprises a feeding hole, a discharging hole and a tail gas outlet, an external circulation heat exchange device is arranged outside the oximation reactor, one end of the external circulation heat exchange device is connected with the bottom of the oximation reactor, and the other end of the external circulation heat exchange device is connected with the micro-interface generator; the micro-interface generator is connected with the feeding hole and is used for dispersing and crushing ammonia gas into micro-bubbles with the diameter of micron level; the discharge hole is connected with the reaction clear liquid buffer tank; the tail gas outlet is connected with the tail gas absorption tower, the bottom of the tail gas absorption tower is also provided with an absorption liquid outlet, and the absorption liquid outlet is connected with the micro-interface generator and is used for enabling absorption liquid to be reused in the oximation reactor.
2. The micro-interface enhanced cyclohexanone ammoximation reaction system of claim 1, wherein the micro-interface generator is a pneumatic micro-interface generator, and the number of the micro-interface generators is more than one.
3. The micro-interface reinforced cyclohexanone ammoximation reaction system of claim 1, wherein the tail gas absorption tower comprises a tower body and a tower kettle, the tower body is filled with a filler, the diameter of the tower kettle is larger than that of the tower body, and the height of the tower kettle is lower than that of the tower body.
4. The micro-interface reinforced cyclohexanone ammoximation reaction system according to claim 1, wherein the external circulation heat exchange device comprises a circulation pipeline, and a full-automatic adjusting condenser and a circulation pump are distributed on the circulation pipeline.
5. The micro-interface reinforced cyclohexanone ammoximation reaction system according to claim 1, wherein a metal membrane filter is arranged inside the oximation reactor for separating the catalyst.
6. The micro-interface reinforced cyclohexanone ammoximation reaction system according to claim 1, wherein a double-coil heat exchanger is arranged in the oximation reactor, the double-coil heat exchanger comprises a cooling coil and a steam heating coil, and the cooling coil is positioned at the upper part of the steam heating coil.
7. The micro-interface reinforced cyclohexanone ammoximation reaction system according to claim 1, wherein an external filtering device is arranged on a connecting pipeline between the reaction clear liquid buffer tank and the discharge port.
8. The micro-interface enhanced cyclohexanone ammoximation reaction system according to claim 1, wherein an exhaust gas cooler is disposed on a connecting line between the exhaust gas absorption tower and the exhaust gas outlet.
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