Micro-interface vaporizer, cyclohexanone-oxime vaporization system and vaporization method thereof

By using a micro-interface vaporizer to perform rotary crushing atomization and secondary crushing atomization of high-temperature airflow during the vaporization of cyclohexanone oxime, the problem of uneven heat during the vaporization of cyclohexanone oxime is solved, and an efficient improvement of the vaporization equilibrium rate is achieved.

CN119869352APending Publication Date: 2025-04-25JIANGSU YANGNONG CHEMICAL GROUP CO LTD +1
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Patent Information

Application Number
CN202510125718.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-26
Publication Date
2025-04-25

AI Technical Summary

Technical Problem

In the prior art, the heat is uneven during the vaporization of cyclohexanone oxime, resulting in the problems of coking, decomposition of cyclohexanone oxime and low gasification equilibrium rate.

Method used

Using a micro-interface vaporizer, the rotating liquid distribution plate and cyclone disk are crushed and atomized, and the secondary crushing atomization and vaporization are carried out in combination with the high-temperature airflow of the carrier gas to ensure that the cyclohexanone oxime is uniformly heated.

Benefits of technology

It significantly reduces the decomposition of cyclohexanone oxime, improves its vaporization equilibrium rate to more than 99.60%, and improves the competitiveness of the process of preparing caprolactam in the gas-phase rearrangement method.

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Abstract

The invention provides a micro-interface vaporizer, a cyclohexanone-oxime vaporization system and a cyclohexanone-oxime vaporization method, the micro-interface vaporizer comprises a cavity and an atomization piece extending into the cavity, the atomization piece comprises an atomization chamber, a liquid distribution disc is arranged in the atomization chamber, and a rotational flow disc is arranged at the bottom of the atomization chamber; a gas distribution disc is further arranged in the cavity body and is higher than the rotational flow disc, and the bottom of the cavity body is arranged to be in an inverted circular truncated cone shape. Raw material liquid containing cyclohexanone-oxime sequentially passes through the rotating liquid distribution disc and the rotational flow disc and is subjected to primary crushing and atomization to form a micro-liquid film; then, the micro-liquid film and carrier gas are subjected to secondary crushing and atomization at the inverted-circular-truncated-cone-shaped bottom of the cavity to form micron-level micro-liquid drops, and meanwhile, due to the fact that the temperature of the carrier gas is high, the micro-liquid drops are rapidly vaporized to form cyclohexanone-oxime steam. According to the micro-interface vaporizer provided by the invention, the raw material liquid containing cyclohexanone-oxime can be uniformly heated, the decomposition of cyclohexanone-oxime is reduced, and the vaporization equilibrium rate of cyclohexanone-oxime is improved.
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Description

Technical Field

[0001] The invention relates to a method for vaporizing a heat-sensitive liquid, and in particular to a micro-interface vaporizer, a vaporization system for cyclohexanone oxime and a vaporization method thereof. Background Art

[0002] ε-Caprolactam (hereinafter referred to as caprolactam) is one of the important organic chemical raw materials, mainly used for the production of nylon fiber and polyamide chips for engineering plastics. The cyclohexanone oxime Beckmann rearrangement process for producing caprolactam includes two methods: liquid phase method and gas phase method. The gas phase Beckmann rearrangement process uses molecular sieve as a catalyst, which replaces fuming sulfuric acid as a catalyst, does not produce ammonium sulfate as a by-product, and solves the problems of equipment corrosion and environmental pollution in the liquid phase rearrangement method. It is more in line with the production requirements of green environmental protection, and has therefore received widespread attention. In the gas phase Beckmann rearrangement process for producing caprolactam, cyclohexanone oxime must first be vaporized by a vaporizer and then reacted in the gas phase at 360-380°C. However, cyclohexanone oxime is a highly heat-sensitive substance, and its properties are unstable above 140°C. If it is not vaporized in time due to uneven heating during the vaporization process, it is very easy to cause side reactions such as polycondensation and decomposition, resulting in coking, resulting in raw material loss, blocking the catalyst pores, and causing catalyst deactivation.

[0003] The vaporization methods of cyclohexanone oxime recorded in the prior art mainly include the following: US Pat. No. 4,268,440A discloses a cyclohexanone oxime vaporization method, wherein cyclohexanone oxime is vaporized by contacting with inert particles such as silica sand in a fluidized bed under an inert gas environment. This method still has the problems of coking and blocking of the bed channel by the product, and because the bed pressure drop continues to increase, it is necessary to continuously increase the inlet pressure of the inert gas to balance the increase in the bed pressure drop of the fluidized bed, so the operation and control are relatively difficult.

[0004] Patent CN1379021A discloses a cyclohexanone oxime vaporization method, which selects low-carbon alcohols such as methanol or ethanol as solvent, i.e., a methanol solution of cyclohexanone oxime, and controls the vaporization temperature below 170°C under a pressure of about 141 kPa, and evaporates the solution into gaseous cyclohexanone oxime through a falling film evaporator containing a circulation system. In this method, it is not easy to achieve uniform distribution of the liquid on the falling film evaporation tube, and there are local wetting blind spots, and a small amount of cyclohexanone oxime is still decomposed by heat to form tar.

[0005] Patent CN103055526B discloses a method for evaporating cyclohexanone oxime, in which the cyclohexanone oxime feed liquid is heated and evaporated in a rising film evaporator, forming a density difference along the axial direction of the evaporation tube, prompting it to flow upward along the evaporation tube, and at the same time, the steam evaporated by the feed liquid rises at a high speed, driving the feed liquid to flow upward along the tube wall in a film-like manner, and the feed liquid and steam flow upward to the flash chamber for gas-liquid separation, and cyclohexanone oxime gas is obtained at the top of the flash chamber, and the unevaporated feed liquid returns from the bottom of the flash chamber through the circulation pipe to the bottom of the rising film evaporator to continue evaporation. Higher overflow intensity requires an increase in the circulation amount of unvaporized cyclohexanone oxime, which increases energy consumption.

[0006] Patent CN102755860B discloses a method for vaporizing cyclohexanone oxime, which proposes using a spray gun to atomize cyclohexanone oxime into small droplets using a carrier gas as an atomizer, and then heating and vaporizing it with another carrier gas to obtain gas-phase cyclohexanone oxime. However, for a single reaction, this method requires a large amount of carrier gas to be heated and vaporized, which consumes a lot of energy. It is difficult to effectively atomize and evenly disperse liquid cyclohexanone oxime without significantly increasing energy consumption.

[0007] The currently disclosed cyclohexanone oxime gasification method is mainly carried out in the following two ways: one is to reduce the residence time of cyclohexanone oxime by increasing the surface area of ​​the cyclohexanone oxime liquid through thin film evaporation or pressure atomization technology. Since the thickness of the micro-liquid layer or the droplets after atomization is very small, the thermal resistance of the heat transfer process is very low, which significantly increases the heat transfer coefficient, enables more molecules to leave the liquid, makes the vaporization process easier to occur, and reduces the time required for vaporization; however, it is difficult to achieve thin film and subsequent uniform vaporization by thin film evaporation; and the pressure atomization nozzle is prone to clogging.

[0008] The second is to reduce the vaporization temperature of cyclohexanone oxime. By introducing inert gas, the equilibrium concentration of cyclohexanone oxime in the gas phase is reduced, and then the gas phase partial pressure of cyclohexanone oxime is reduced, so that its equilibrium partial pressure is less than its saturated vapor pressure, thereby achieving vaporization of cyclohexanone oxime below the boiling point. The introduced inert gas is called carrier gas. The introduction of carrier gas also enhances the circulation speed and gas content of the liquid, increases the turbulence in the tube, and thus enhances heat transfer; the disadvantage of this method is that the amount of carrier gas used is large.

[0009] These methods still fail to avoid the problem of local overheating of cyclohexanone oxime to form tar, resulting in decomposition of cyclohexanone oxime and a decrease in the gasification equilibrium rate of cyclohexanone oxime.

[0010] In view of this, this application is hereby filed. Summary of the invention

[0011] The main purpose of the present invention is to provide a micro-interface vaporizer, a cyclohexanone oxime vaporization system and a vaporization method thereof, so as to solve the problems in the prior art of uneven heating during the vaporization process of cyclohexanone oxime, resulting in coking, cyclohexanone oxime decomposition and low cyclohexanone oxime gasification equilibrium rate.

[0012] In order to achieve the above object, according to one aspect of the present invention, a micro-interface vaporizer is provided, the micro-interface vaporizer comprising: a cavity body and an atomizing element extending into the cavity body,

[0013] The atomizing element comprises an atomizing chamber, a liquid distribution plate is arranged inside the atomizing chamber, a swirl plate is arranged at the bottom of the atomizing chamber, the liquid distribution plate is connected with a liquid inlet pipe, and the liquid inlet pipe is used to transport the raw material liquid containing cyclohexanone oxime to the liquid distribution plate;

[0014] A gas distribution plate is also provided inside the cavity body. The gas distribution plate is an annular structure. The gas distribution plate is sleeved outside the atomization chamber and is higher than the swirl plate. The gas distribution plate is connected with an air inlet pipe, which is used to transport the carrier gas to the gas distribution plate.

[0015] The bottom of the cavity is arranged in an inverted truncated cone shape, and a micro-interface vaporization outlet is also arranged at the bottom of the cavity.

[0016] Furthermore, a rotating shaft is inserted in the atomization chamber, and the liquid distribution plate and the swirl plate are both annular structures and are respectively sleeved on the rotating shaft. The liquid distribution plate and the swirl plate rotate respectively driven by the rotating shaft; wherein the liquid distribution plate is provided with a plurality of liquid fan-shaped grooves, and the groove width of the liquid fan-shaped grooves gradually increases along the direction of the liquid distribution plate away from its annular center; the swirl plate is provided with a plurality of swirl grooves, and the plurality of swirl grooves are arranged along the circumferential array of the swirl plate, and the length direction of the swirl grooves is arranged along the radial direction of the swirl plate.

[0017] Further, the gas distribution plate is arranged on the inner wall of the cavity body, and the gas distribution plate is provided with a plurality of gas sector grooves, and the groove width of the gas sector grooves gradually increases along the direction away from the annular center of the gas distribution plate.

[0018] Furthermore, the top diameter of the atomizing chamber is 60-100 mm, and the bottom diameter of the atomizing chamber is 120-200 mm.

[0019] Furthermore, the height of the atomization chamber is 200-400 mm.

[0020] Furthermore, the swirl disc comprises an upper dial and a lower dial, the upper dial and the lower dial are arranged opposite to each other, and the distance between the upper dial and the lower dial is 20-40 mm.

[0021] Furthermore, the cavity body includes a first cavity body and a second cavity body, wherein the first cavity body is cylindrical and the second cavity body is an inverted truncated cone; and the inner diameter of the first cavity body is 800-1200 mm, and the height of the first cavity body is 1000-2000 mm.

[0022] Furthermore, the ratio of the inner diameter of the first cavity body to the inner diameter of the bottom end of the second cavity body is (2-6):1.

[0023] Furthermore, the height of the second cavity is 1000-2000 mm.

[0024] According to another aspect of the present invention, a vaporization system for cyclohexanone oxime is provided, which includes a vaporization unit, the vaporization unit includes a micro-interface vaporizer and a reactor connected in sequence, the micro-interface vaporizer is the micro-interface vaporizer provided in the first aspect above; the inlet of the reactor is connected to the micro-interface vaporization outlet.

[0025] Furthermore, the vaporization system also includes a raw material supply unit, which includes a raw material liquid storage tank and a gas storage tank; the outlet of the raw material liquid storage tank is connected to the liquid inlet pipeline, and the raw material liquid storage tank is used to supply the raw material liquid containing cyclohexanone oxime; the outlet of the gas storage tank is connected to the air inlet pipeline, and the gas storage tank is used to supply the carrier gas.

[0026] Furthermore, the raw material supply unit also includes a gas preheater, which is arranged on the pipeline between the gas storage tank and the air intake pipeline.

[0027] Furthermore, the interior of the reactor is filled with fillers; the fillers include at least one of glass fillers, ceramic fillers, stainless steel fillers and titanium fillers.

[0028] Furthermore, the vaporization system also includes a gas-liquid separation unit, and the gas-liquid separation unit also includes a gas-liquid separator and a methanol tail gas absorption device; the inlet of the gas-liquid separator is connected to the outlet of the reactor, the bottom of the gas-liquid separator is provided with a first liquid phase outlet, and the top of the gas-liquid separator is provided with a first gas phase outlet, and the first liquid phase outlet is used to discharge the first liquid phase; the inlet of the methanol tail gas absorption device is connected to the first gas phase outlet, the top of the methanol tail gas absorption device is provided with a second gas phase outlet, and the bottom of the methanol tail gas absorption device is provided with a methanol absorption liquid outlet, the second gas phase outlet is used to discharge the carrier gas, and the methanol absorption liquid outlet is used to discharge the methanol absorption liquid.

[0029] Furthermore, the gas-liquid separation unit also includes a condenser, which is arranged on the pipeline between the reactor and the gas-liquid separator.

[0030] Furthermore, the second gas phase outlet is connected to a gas storage tank (not shown in the figure) for returning the cyclohexanone oxime to the vaporization system for recycling.

[0031] According to a third aspect of the present invention, a method for vaporizing cyclohexanone oxime is provided. The method is carried out in the vaporization system for cyclohexanone oxime provided in the second aspect, and comprises the following steps:

[0032] The raw material liquid containing cyclohexanone oxime is introduced into the atomizing element for primary crushing and atomization to form a micro liquid film, and the carrier gas is introduced into the micro interface vaporizer. The micro liquid film and the carrier gas are secondary crushed and atomized and primary vaporized in the inverted truncated cone-shaped cavity of the micro interface vaporizer, and then secondary heated in the reactor to obtain cyclohexanone oxime vapor.

[0033] Furthermore, the flow rate of the raw material liquid containing cyclohexanone oxime is 25-50 mL / min.

[0034] Furthermore, the flow rate of the carrier gas is 40-60 L / min.

[0035] Furthermore, the rotation speed of the atomizing element is 10000-20000 r / min.

[0036] Further, the temperature of the microinterface vaporizer is 140-250°C, and further 150-240°C.

[0037] Further, the secondary heating temperature is 350-390°C, and further 360-380°C.

[0038] Furthermore, the raw material liquid containing cyclohexanone oxime is preheated and then introduced into the atomizing element.

[0039] Furthermore, the preheating temperature of the raw material liquid containing cyclohexanone oxime is 20-60°C, and further 25-50°C.

[0040] Furthermore, the carrier gas is preheated before being introduced into the microinterface vaporizer.

[0041] Furthermore, the preheating temperature of the carrier gas is 200-260°C, and further 210-250°C.

[0042] Furthermore, the raw material liquid containing cyclohexanone oxime is a mixed solution of cyclohexanone oxime and alcohol, wherein the mass concentration of cyclohexanone oxime is 20-60wt%, and further 25-50wt%.

[0043] Furthermore, the alcohol in the mixed solution of cyclohexanone oxime and alcohol includes methanol and / or ethanol.

[0044] Furthermore, the carrier gas is nitrogen.

[0045] The technical scheme of the present invention is applied. The present application passes the raw material liquid containing cyclohexanone oxime through a rotating liquid distribution plate, so that it rotates along the wall of the atomizing chamber under the action of centrifugal force, and then obtains a tangential velocity through the swirl groove of the swirl plate, and the raw material liquid containing cyclohexanone oxime is once broken and atomized to form a micro liquid film, and rotates in a conical shape (rotating fog cone) to leave the swirl groove. The carrier gas passes through the gas distribution plate and rotates into the interior of the cavity. The outer side of the rotating fog cone is the carrier gas. Since there is a certain amount of relative speed between the two, the rotating fog cone and the rotating carrier gas swirl, and as the cross-section of the inverted truncated cone bottom of the cavity body is continuously reduced, the flow rate of the carrier gas increases, and the two squeeze and cut each other, the micro liquid film is broken and atomized into micro droplets of micrometer level by secondary crushing, and at the same time, due to the high temperature of the carrier gas, the micro droplets are rapidly vaporized to form cyclohexanone oxime vapor.

[0046] The micro-interface vaporizer provided in the present application can heat the raw material liquid containing cyclohexanone oxime uniformly, reduce the decomposition of cyclohexanone oxime, and the vaporization equilibrium rate of cyclohexanone oxime is ≥99.60%, which improves the competitiveness of the process for preparing caprolactam by gas phase rearrangement. In addition, the surface shear force of the raw material liquid containing cyclohexanone oxime is increased by a centrifugal rotary atomizer, and the wall surface of the cavity is effectively washed to prevent scaling of the wall surface. The centrifugal rotary atomizer has good atomization ability for high-viscosity liquids and suspensions, and is not easy to block holes during the atomization process. The device can operate continuously and stably for ≥2000h. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] The drawings constituting a part of the present application are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0048] Figure 1 A schematic diagram of the structure of a micro-interface vaporizer provided in some embodiments of the present invention is shown;

[0049] Figure 2 A schematic diagram of the structure of an atomizer provided in some embodiments of the present invention is shown;

[0050] Figure 3 A schematic diagram of the structure of a liquid distribution plate provided in some embodiments of the present invention is shown;

[0051] Figure 4 It shows a schematic structural diagram of a swirl disk provided in some embodiments of the present invention;

[0052] Figure 5 A schematic diagram of the structure of a gas distribution plate provided in some embodiments of the present invention is shown;

[0053] Figure 6 A schematic structural diagram of a cyclohexanone oxime vaporization system provided in some embodiments of the present invention is shown;

[0054] The above drawings include the following reference numerals:

[0055] 110. Raw liquid storage tank; 120. First pump; 210. Gas preheater; 220. First compressor; 300. Micro-interface vaporizer; 311. Atomizing chamber; 312. Liquid distribution plate; 3120. Liquid fan-shaped groove; 313. Swirl plate; 3130. Swirl groove; 314. Rotating shaft; 315. Centrifugal drive; 316. Liquid inlet pipeline; 321. First cavity; 322. Second cavity; 323. Gas distribution plate; 3230. Gas fan-shaped groove; 324. Micro-interface vaporization outlet; 325. Air inlet pipeline; 400. Reactor; 410. Filler; 510. Gas-liquid separator; 520. Methanol tail gas absorption device; 530. Condenser. DETAILED DESCRIPTION

[0056] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0057] As analyzed in the background of the present application, the prior art has the problem that the vaporization process of cyclohexanone oxime is unevenly heated, resulting in coking, decomposition of cyclohexanone oxime, and a low cyclohexanone oxime gasification equilibrium rate. In order to solve this problem, the present application provides a micro-interface vaporizer, a cyclohexanone oxime vaporization system and a vaporization method thereof.

[0058] In a typical embodiment of the present application, a micro-interface vaporizer 300 is provided, such as Figure 1 As shown, the micro-interface vaporizer 300 includes: a cavity body and an atomizing element extending into the cavity body.

[0059] Among them, the structural diagram of the atomizer is as follows Figure 2 As shown, it includes an atomizing chamber 311, a liquid distribution plate 312 is arranged inside the atomizing chamber 311, a swirl plate 313 is arranged at the bottom of the atomizing chamber 311, and the liquid distribution plate 312 is connected to a liquid inlet pipe 316, and the liquid inlet pipe 316 is used to transport the raw material liquid containing cyclohexanone oxime to the liquid distribution plate 312;

[0060] A gas distribution plate 323 is also provided inside the cavity. The gas distribution plate 323 is an annular structure. The gas distribution plate 323 is sleeved outside the atomization chamber 311 and is higher than the swirl plate 313. The gas distribution plate 323 is connected to an air inlet pipe 325, and the air inlet pipe 325 is used to transport the carrier gas to the gas distribution plate 323.

[0061] The bottom of the cavity is configured to be an inverted truncated cone, and a micro-interface vaporization outlet 324 is also provided at the bottom of the cavity.

[0062] The present application will be the raw material liquid containing cyclohexanone oxime through the rotating liquid distribution plate 312, so that it is rotated along the wall of the atomizing chamber 311 under the action of centrifugal force, and then the swirl groove 3130 of the swirl plate 313 is obtained by tangential velocity, and the raw material liquid containing cyclohexanone oxime is once broken and atomized to form a micro liquid film, and rotates (rotating fog cone) to leave the swirl groove in a conical shape. Carrier gas passes through the gas distribution plate 323 and rotates into the inside of the cavity. The outside of the rotating fog cone is carrier gas, and due to the relative speed of a certain amount between the two, the rotating fog cone and the rotating carrier gas swirl, and as the cross section of the bottom of the inverted cone of the cavity body is continuously reduced, the flow rate of the carrier gas increases, and the two squeeze and cut each other, and the micro liquid film is secondary broken and atomized into micro droplets of micron level, and at the same time, due to the high temperature of the carrier gas, the micro droplets are rapidly vaporized to form cyclohexanone oxime steam.

[0063] The micro-interface vaporizer 300 provided in the present application can heat the raw material liquid containing cyclohexanone oxime uniformly, reduce the decomposition of cyclohexanone oxime, and the vaporization equilibrium rate of cyclohexanone oxime is ≥99.60%, which improves the competitiveness of the process for preparing caprolactam by gas phase rearrangement method. In addition, the surface shear force of the raw material liquid containing cyclohexanone oxime is increased by the centrifugal rotary atomizer, and the wall surface of the cavity body is effectively washed to prevent scaling of the wall surface. The centrifugal rotary atomizer has good atomization ability for high-viscosity liquids and suspensions, and is not easy to block holes during the atomization process. The device can operate continuously and stably for ≥2000h.

[0064] The gas distribution plate 323 is above the swirl plate 313, which can further enhance the cutting effect of the carrier gas and the micro-liquid film, further promote the secondary breakup and atomization of the micro-liquid film into micro-droplets with smaller particle sizes, thereby further making the cyclohexanone oxime heated evenly during vaporization and improving the vaporization equilibrium rate of the cyclohexanone oxime.

[0065] In some embodiments, the distance between the liquid inlet pipe 316 and the liquid distribution plate 312 is 10-20 mm to ensure that the liquid inlet pipe 316 does not rotate, but at the same time, the raw material liquid containing cyclohexanone oxime can fully enter the liquid distribution plate 312. In order to further evenly distribute the raw material liquid containing cyclohexanone oxime in the liquid distribution plate 312, it is preferred that the first liquid inlet pipe and the second liquid inlet pipe are symmetrically arranged on both sides of the liquid distribution plate 312.

[0066] In some embodiments, the distance between the air inlet duct 325 and the gas distribution plate 323 is 10-20 mm to ensure that the carrier gas can fully enter the gas distribution plate 323. In order to further evenly distribute the carrier gas in the gas distribution plate 323, the first air inlet duct and the second air inlet duct are preferably symmetrically arranged on both sides of the gas distribution plate 323.

[0067] In some embodiments, a rotating shaft 314 is further inserted into the atomizing chamber 311 , and the liquid distribution plate 312 and the swirl plate 313 are both annular structures and are respectively sleeved on the rotating shaft 314 . The liquid distribution plate 312 and the swirl plate 313 rotate respectively driven by the rotating shaft 314 .

[0068] In some embodiments, the rotating shaft 314 is connected to a centrifugal driver 315 , and the centrifugal driver 315 provides power for the rotation of the rotating shaft 314 . Preferably, the centrifugal driver 315 is disposed outside the hollow cavity.

[0069] In some embodiments, the structure diagram of the liquid distribution plate 312 is as follows: Figure 3 As shown, it is provided with a plurality of liquid fan-shaped grooves 3120, and the groove width of the liquid fan-shaped grooves 3120 gradually increases along the direction away from the annular center of the liquid distribution plate 312, so as to promote the raw material liquid containing cyclohexanone oxime to be evenly broken and atomized. The position, shape and number of the liquid fan-shaped grooves 3120 can be adjusted according to actual needs to ensure that the raw material liquid containing cyclohexanone oxime is evenly broken and atomized and enters the atomization chamber 311.

[0070] In some embodiments, the structural diagram of the swirl disk 313 is as follows: Figure 4 As shown, the swirl disk 313 is provided with a plurality of swirl grooves 3130, and the plurality of swirl grooves 3130 are arranged along the circumferential array of the swirl disk 313, and the length direction of the swirl grooves 3130 is arranged along the radial direction of the swirl disk 313; it is further preferred that the number of the swirl grooves 3130 is 96, so as to further promote the filamentation and breaking of the raw material liquid containing cyclohexanone oxime into extremely fine droplets in the swirl grooves 3130.

[0071] In some embodiments, the gas distribution plate 323 is disposed on the inner wall of the cavity. The structural diagram of the gas distribution plate 323 is as shown in FIG. Figure 5 As shown, the gas distribution plate 323 is provided with a plurality of gas fan-shaped grooves 3230, and the width of the gas fan-shaped grooves 3230 gradually increases along the direction away from the annular center of the gas distribution plate 323. The gas distribution plate 323 plays a guiding role, and the carrier gas passes through the gas distribution plate 323, rotates into the interior of the cavity and is evenly dispersed.

[0072] In some embodiments, the top diameter of the atomizing chamber 311 is 60-100 mm, the bottom diameter of the atomizing chamber 311 is 120-200 mm, and the height of the atomizing chamber 311 is 200-400 mm. It is further preferred that the ratio of the top diameter to the bottom diameter of the atomizing chamber 311 is 1:2. In the present application, the top diameter of the atomizing chamber 311 is the outer diameter of the liquid distribution plate 312, the bottom diameter of the atomizing chamber 311 is the outer diameter of the upper dial of the swirl plate 313, and the height of the atomizing chamber 311 is the distance between the top of the liquid distribution plate 312 and the upper dial of the swirl plate 313.

[0073] In some embodiments, the swirl disk 313 includes an upper dial and a lower dial, the upper dial and the lower dial are arranged opposite to each other, and the distance between the upper dial and the lower dial is 20-40 mm. The height of the swirl disk 313 in the present application refers to the distance between the upper dial and the lower dial. It is further preferred that the ratio of the height of the swirl disk 313 to the height of the atomization chamber 311 is 1:10, so as to further promote the micro-liquid film to be broken and atomized into micro-droplets at the micron level.

[0074] In order to further promote the high-speed rotation and atomization of the raw material liquid containing cyclohexanone oxime in the atomizer, the atomizer is driven by the rotating shaft 314 to rotate. Preferably, when the device is running, the rotating speed of the rotating shaft 314 is 10000-20000 r / min.

[0075] In some embodiments, the cavity body includes a first cavity body 321 and a second cavity body 322, wherein the first cavity body 321 is cylindrical, and the second cavity body 322 is an inverted truncated cone type; and the inner diameter of the first cavity body 321 is 800-1200mm, and the height of the first cavity body 321 is 1000-2000mm. The top inner diameter of the second cavity body 322 is the same as the inner diameter of the first cavity body 321, and the top inner diameter of the second cavity body 322 is 800-1200mm. The cavity body is arranged as a structure in which a cylindrical cavity body and an inverted truncated cone type cavity body are connected, which can further promote the carrier gas to fully contact with the micro-liquid film (the raw material liquid containing cyclohexanone oxime is broken and atomized), and as the cross-section of the inverted truncated cone type cavity body is reduced, the carrier gas flow rate increases, and the micro-liquid film is further promoted to be broken and atomized by secondary crushing, forming a droplet of smaller size, thereby further improving the vaporization equilibrium rate of cyclohexanone oxime.

[0076] In some embodiments, the ratio of the inner diameter of the first cavity 321 to the inner diameter of the bottom end of the second cavity 322 is (2-6):1, and preferably 4:1, so as to further improve the vaporization equilibrium rate of cyclohexanone oxime.

[0077] In some embodiments, the height of the second cavity 322 is 1000-2000 mm, and it is further preferred that the first cavity 321 and the second cavity 322 have the same height to further improve the vaporization equilibrium rate of cyclohexanone oxime.

[0078] In a second typical embodiment of the present application, a cyclohexanone oxime vaporization system is provided, such as Figure 6 As shown, the vaporization system includes a vaporization unit, which includes a micro-interface vaporizer 300 and a reactor 400 connected in sequence, wherein the micro-interface vaporizer 300 is the micro-interface vaporizer 300 provided in the first typical embodiment. The inlet of the reactor 400 is connected to the micro-interface vaporization outlet 324.

[0079] The cyclohexanone oxime vaporization system provided by the present application comprises a raw material liquid containing cyclohexanone oxime, which is first crushed and atomized and vaporized once by the micro-interface vaporizer 300 provided by the above-mentioned first typical embodiment to obtain steam containing cyclohexanone oxime. The micro-interface vaporizer 300 can heat the raw material liquid containing cyclohexanone oxime uniformly, reducing the decomposition of cyclohexanone oxime. The raw material liquid is then introduced into the reactor 400 for secondary heating, which further promotes vaporization, further reduces the decomposition of cyclohexanone oxime, and improves the cyclohexanone oxime vaporization equilibrium rate.

[0080] In some embodiments, the vaporization system also includes a raw material supply unit, which includes a raw material liquid storage tank 110 and a gas storage tank (not shown in the figure); the outlet of the raw material liquid storage tank 110 is connected to the liquid inlet pipe 316, and the raw material liquid storage tank 110 is used to supply a raw material liquid containing cyclohexanone oxime; the outlet of the gas storage tank is connected to the air inlet pipe 325, and the gas storage tank is used to supply a carrier gas.

[0081] In order to transport the raw material liquid containing cyclohexanone oxime in the raw material liquid storage tank 110 to the liquid distribution plate 312 , a first pump 120 is preferably provided on the pipeline connecting the raw material liquid storage tank 110 and the liquid inlet pipeline 316 .

[0082] In order to further heat the carrier gas and promote the rapid completion of the vaporization process when the carrier gas contacts the droplets containing cyclohexanone oxime, the raw material supply unit preferably also includes a gas preheater 210, and the gas preheater 210 is arranged on the pipeline between the gas storage tank and the air inlet pipeline 325.

[0083] In order to further transport the carrier gas in the gas storage tank to the gas preheater 210 , a first compressor 220 is preferably provided on the pipeline connecting the gas storage tank and the gas preheater 210 .

[0084] In order to further improve the vaporization efficiency of cyclohexanone oxime, the interior of the reactor 400 is preferably filled with a filler 410; the filler 410 includes any one or more of a glass filler, a ceramic filler, a stainless steel filler and a titanium filler.

[0085] In some embodiments, in order to detect the vaporization effect of cyclohexanone oxime, the vaporization system further includes a gas-liquid separation unit, and the gas-liquid separation unit includes a gas-liquid separator 510 and a methanol tail gas absorption device 520;

[0086] The inlet of the gas-liquid separator 510 is connected to the outlet of the reactor 400, the bottom of the gas-liquid separator 510 is provided with a first liquid phase outlet, and the top of the gas-liquid separator 510 is provided with a first gas phase outlet, and the first liquid phase outlet is used to discharge the condensate containing cyclohexanone oxime;

[0087] The inlet of the methanol tail gas absorption device 520 is connected to the first gas phase outlet, the top of the methanol tail gas absorption device 520 is provided with a second gas phase outlet, and the bottom of the methanol tail gas absorption device 520 is provided with a methanol absorption liquid outlet. Uncondensed cyclohexanone oxime vapor and carrier are introduced into the methanol tail gas absorption device 520, and the uncondensed cyclohexanone oxime vapor is absorbed by methanol to obtain methanol absorption liquid, which is discharged from the methanol absorption liquid outlet provided at the bottom, and the carrier gas is discharged from the second gas phase outlet.

[0088] In the present application, the gas-liquid separation unit condenses or absorbs the vapor containing cyclohexanone oxime and collects it, and performs quantitative analysis by gas chromatography. The condensate containing cyclohexanone oxime and the cyclohexanone oxime in the methanol absorption liquid are quantitatively analyzed by gas chromatography to calculate the cyclohexanone oxime vaporization equilibrium rate.

[0089] In order to further reduce energy consumption and production costs, the second gas phase outlet is preferably connected to a gas storage tank, and the carrier gas is compressed by a second compressor (not shown) and then returned to the vaporization system for recycling.

[0090] In order to further promote the condensation of the steam containing cyclohexanone oxime, it is preferred that the gas-liquid separation unit further includes a condenser 530 , which is disposed on the pipeline between the reactor 400 and the gas-liquid separator 510 .

[0091] In some embodiments, the temperature of the condenser 530 is preferably 0-10°C, and further preferably, the condenser 530 also includes a first refrigerant liquid inlet and a first refrigerant liquid outlet (not shown in the figure), and the first refrigerant enters from the first refrigerant liquid inlet and is discharged from the first refrigerant liquid outlet to ensure the condensation effect of the condenser 530.

[0092] In order to further promote the gas-liquid separation effect, the gas-liquid separator 510 preferably also includes a second refrigerant inlet and a second refrigerant outlet (not shown in the figure). The second refrigerant enters from the second refrigerant inlet and is discharged from the second refrigerant outlet to ensure the condensation effect of the gas-liquid separator 510. The temperature of the gas-liquid separator 510 is preferably 20-40°C to reduce energy consumption.

[0093] In some embodiments, the filler 410 in the reactor 400 can be replaced with an MFI structure catalyst, and the raw material liquid containing cyclohexanone oxime passes through the micro-interface vaporizer 300 to obtain steam containing cyclohexanone oxime, and the steam containing cyclohexanone oxime undergoes a gas-phase rearrangement reaction in the reactor 400 under the catalysis of the catalyst to generate caprolactam steam. After the reaction, the material enters the gas-liquid separation unit to collect the caprolactam. After the reaction, the material passes through the gas-liquid separator 510, and the rearrangement reaction liquid A is obtained from the first liquid phase outlet. The uncondensed caprolactam steam and carrier gas discharged from the first gas phase outlet are then passed into the methanol tail gas absorption device 520 to absorb the caprolactam steam, and the rearrangement reaction liquid B is discharged from the methanol absorption liquid outlet, and the carrier gas is discharged from the carrier gas outlet. In order to further improve the gas-liquid separation effect, it is preferred that the gas-liquid separation unit also includes a condenser 530, and the condenser 530 is arranged on the pipeline between the reactor 400 and the gas-liquid separator 510.

[0094] In a third typical embodiment of the present application, a cyclohexanone oxime vaporization method is provided, comprising the following steps: a raw material liquid containing cyclohexanone oxime is passed into an atomizing element for primary crushing and atomization to form a micro liquid film, a carrier gas is passed into a micro-interface vaporizer 300, the micro liquid film and the carrier gas are secondary crushed and atomized and primary vaporized in the inverted frustum-shaped cavity of the micro-interface vaporizer 300, and then secondary heated in a reactor 400 to obtain cyclohexanone oxime vapor.

[0095] In the present application, the raw material liquid containing cyclohexanone oxime is passed into the rotating liquid distribution disk 312 in the atomizing element. The raw material liquid containing cyclohexanone oxime rotates along the wall of the atomizing chamber 311 under the action of centrifugal force, and then obtains the tangential velocity through the swirl groove 3130 of the swirl disk 313. The raw material liquid containing cyclohexanone oxime is broken and atomized once to form a micro liquid film, and leaves the swirl groove 3130 in a conical rotation (rotating mist cone). The carrier gas enters the gas distribution plate 323 through the air inlet pipe 325, and swirls under the diversion effect of the gas distribution plate 323. The outer side of the rotating fog cone is the carrier gas. The rotating fog cone and the rotating carrier gas swirl at high speed in the cavity of the micro-interface vaporizer 300. Because there is a certain amount of relative speed between the two, and as the cross section of the inverted truncated cone bottom of the cavity body is continuously reduced, the flow rate of the carrier gas increases, and the two squeeze and cut each other, the micro-liquid film is secondary broken and atomized into micro-droplets of micron level. At the same time, because the temperature of the carrier gas is high, the micro-droplets are rapidly vaporized once to form steam, and the steam containing cyclohexanone oxime is obtained. This vaporization method is enough to make cyclohexanone oxime evenly heated, and the decomposition of cyclohexanone oxime is reduced. Subsequently, the steam containing cyclohexanone oxime is passed into the reactor 400 for secondary heating, which further promotes the vaporization of cyclohexanone oxime into cyclohexanone oxime steam, and further reduces the decomposition of cyclohexanone oxime and improves the vaporization equilibrium rate of cyclohexanone oxime.

[0096] In some embodiments, the flow rate of the raw material liquid containing cyclohexanone oxime is 25-50 mL / min, and the flow rate of the carrier gas is 40-60 L / min, so as to further promote uniform heating of the raw material liquid containing cyclohexanone oxime during vaporization and further improve the vaporization equilibrium rate of cyclohexanone oxime.

[0097] In order to further break up and atomize the raw material liquid containing cyclohexanone oxime, it is preferred that the rotation speed of the atomizer is 10000-20000 r / min, and the rotation speed of the atomizer is the rotation speed of the rotating shaft 314 .

[0098] In order to further promote the vaporization of the raw material liquid containing cyclohexanone oxime, the temperature of the micro-interface vaporizer 300 is preferably 140-250°C, more preferably 150-240°C.

[0099] In order to make the raw material liquid containing cyclohexanone oxime vaporize more fully, the secondary heating temperature is preferably 350-390°C, more preferably 360-380°C.

[0100] In order to further improve the vaporization efficiency of the raw material liquid containing cyclohexanone oxime, the raw material liquid containing cyclohexanone oxime is first preheated and then introduced into the atomizing element; and it is further preferred that the preheating temperature of the raw material liquid containing cyclohexanone oxime is 20-60°C, more preferably 25-50°C.

[0101] In order to further ensure that cyclohexanone oxime is heated evenly during vaporization and reduce decomposition of cyclohexanone oxime, it is preferred to preheat the carrier gas before passing the carrier gas into the microinterface vaporizer 300, and it is further preferred that the preheating temperature of the carrier gas is 200-260°C, more preferably 210-250°C.

[0102] In order to further improve the vaporization equilibrium rate of cyclohexanone oxime, the raw material liquid containing cyclohexanone oxime is preferably a mixed solution of cyclohexanone oxime and alcohol, wherein the mass concentration of cyclohexanone oxime is 20-60wt%, and more preferably 25-50wt%; and when the mass concentration of cyclohexanone oxime in the raw material liquid containing cyclohexanone oxime increases, the preheating temperature of the raw material liquid containing cyclohexanone oxime can be appropriately increased to further improve the vaporization equilibrium rate of cyclohexanone oxime.

[0103] In order to further promote the dissolution of cyclohexanone oxime, it is preferred that the alcohol in the mixed solution includes methanol and / or ethanol.

[0104] In order to further promote the vaporization of cyclohexanone oxime, the carrier gas is preferably nitrogen.

[0105] In some embodiments, when the filler 410 in the reactor 400 is replaced with an MFI structured molecular sieve catalyst, in order to further promote the gas-phase rearrangement reaction of cyclohexanone oxime vapor catalyzed by the catalyst, the reaction temperature is preferably 350-390°C, more preferably 360-380°C.

[0106] The beneficial effects of the present application will be further illustrated below in combination with embodiments and comparative examples.

[0107] Example 1

[0108] This embodiment provides a micro-interface vaporizer 300, such as Figure 1 As shown, 300, micro-interface vaporizer; 311, atomization chamber; 312, liquid distribution plate; 313, swirl plate; 314, rotating shaft; 315, centrifugal drive; 316, liquid inlet pipe; 321, first cavity; 322, second cavity; 323, gas distribution plate; 324, micro-interface vaporization outlet; 325, air inlet pipe.

[0109] The micro-interface vaporizer 300 includes: a hollow body and an atomizing element extending into the hollow body, the atomizing element includes an atomizing chamber 311, a liquid distribution plate 312 is arranged inside the atomizing chamber 311, a swirl plate 313 is arranged at the bottom of the atomizing chamber 311, the liquid distribution plate 312 is provided with a plurality of liquid fan-shaped grooves 3120, and the groove width of the liquid fan-shaped grooves 3120 gradually increases along the direction away from the annular center of the liquid distribution plate 312. The liquid distribution plate 312 is connected to a liquid inlet pipe 316, and the liquid inlet pipe 316 is used to transport the raw material liquid containing cyclohexanone oxime to the liquid distribution plate 312. The side of the swirl disk 313 is provided with 96 swirl grooves 3130, which are arranged in a circumferential array along the swirl disk 313, and the length direction of the swirl grooves 3130 is arranged along the radial direction of the swirl disk 313; wherein, the top diameter of the atomization chamber 311 is 60-100mm, the bottom diameter of the atomization chamber 311 is 120-200mm, and the height of the atomization chamber 311 is 200-400mm. The swirl disk 313 includes an upper dial and a lower dial, and the distance between the upper dial and the lower dial (the height of the swirl disk) is 20-40mm.

[0110] The rotating shaft 314 is inserted into the atomizing chamber 311, and the liquid distribution plate 312 and the swirl plate 313 are both annular structures and are respectively sleeved on the rotating shaft 314. The liquid distribution plate 312 and the swirl plate 313 are respectively rotated under the drive of the rotating shaft 314. The rotating shaft 314 is connected to a centrifugal driver 315, and the centrifugal driver 315 is used to rotate the rotating shaft 314 to generate centrifugal force. The centrifugal driver 315 is arranged outside the cavity.

[0111] A gas distribution plate 323 is also disposed inside the cavity body. The gas distribution plate 323 is disposed on the inner wall of the cavity body. The gas distribution plate 323 is provided with a plurality of gas fan-shaped grooves 3230, and the groove width of the gas fan-shaped grooves 3230 gradually increases along the direction away from the annular center of the gas distribution plate 323. The gas distribution plate 323 is connected to an air inlet pipe 325, and the air inlet pipe 325 is used to transport the carrier gas to the gas distribution plate 323. Among them, the gas distribution plate 323 is higher than the swirl plate 313.

[0112] The cavity body includes a first cavity body 321 and a second cavity body 322, wherein the first cavity body 321 is cylindrical and the second cavity body 322 is an inverted truncated cone; the inner diameter of the first cavity body 321 is 800-1200 mm, and the height of the first cavity body 321 is 1000-2000 mm; the inner diameter of the top of the second cavity body 322 is 800-1200 mm, the ratio of the inner diameter of the first cavity body 321 to the inner diameter of the bottom of the second cavity body 322 is (2-6):1, and the height of the second cavity body 322 is 1000-2000 mm. A micro-interface vaporization outlet 324 is also provided at the bottom of the second cavity body 322.

[0113] Example 2

[0114] This embodiment provides a vaporization system for cyclohexanone oxime, such as Figure 6 As shown, the vaporization system includes a raw material supply unit, a vaporization unit and a gas-liquid separation unit, and the micro-interface vaporizer 300 in the vaporization unit in this embodiment is the micro-interface vaporizer 300 provided in Example 1.

[0115] The raw material supply unit includes a raw material liquid storage tank 110, a gas storage tank (not shown in the figure) and a gas preheater 210. The outlet of the raw material liquid storage tank 110 is connected to the liquid inlet pipeline 316, and a first pump 120 is provided on the pipeline connecting the raw material liquid storage tank 110 and the liquid inlet pipeline 316. The outlet of the gas storage tank is connected to the inlet of the gas preheater 210, and the outlet of the gas preheater 210 is connected to the air inlet pipeline 325. A first compressor 220 is provided on the pipeline connecting the gas storage tank and the gas preheater 210, and the first compressor 220 is used to transport the carrier gas in the gas storage tank to the gas preheater 210.

[0116] The vaporization unit includes a microinterface vaporizer 300 and a reactor 400 connected in sequence, and the inlet of the reactor 400 is connected to the microinterface vaporization outlet 324. The reactor 400 is filled with a filler 410, which includes any one or more of glass fillers, ceramic fillers, stainless steel fillers and titanium fillers.

[0117] The gas-liquid separation unit includes a gas-liquid separator 510, a methanol tail gas absorption device 520 and a condenser 530. The outlet of the reactor 400 is connected to the inlet of the condenser 530, and the outlet of the condenser 530 is connected to the inlet of the gas-liquid separator 510. The bottom of the gas-liquid separator 510 is provided with a first liquid phase outlet, and the top of the gas-liquid separator 510 is provided with a first gas phase outlet, and the first liquid phase outlet is used to discharge the first liquid phase. The inlet of the methanol tail gas absorption device 520 is connected to the first gas phase outlet, the top of the methanol tail gas absorption device 520 is provided with a second gas phase outlet, and the bottom of the methanol tail gas absorption device 520 is provided with a methanol absorption liquid outlet, the second gas phase outlet is used to discharge the carrier gas, and the methanol absorption liquid outlet is used to discharge the methanol absorption liquid. Wherein, the second gas phase outlet is connected to the gas storage tank (not shown in the figure), and a second compressor (not shown in the figure) is provided on the pipeline where the second gas phase outlet is connected to the gas storage tank to return the carrier gas to the vaporization system of cyclohexanone oxime for recycling.

[0118] Example 3

[0119] This embodiment provides a method for vaporizing cyclohexanone oxime. The vaporization method is performed using the cyclohexanone oxime vaporization system provided in Example 2, and comprises the following steps:

[0120] (1) A mixed solution of cyclohexanone oxime and methanol (the mass concentration of cyclohexanone oxime in the mixed solution is 40 wt%) is preheated to 40° C. in a raw liquid storage tank 110, and then introduced into a liquid distribution plate 312 in a rotating atomizing element at a flow rate of 40 mL / min through a liquid inlet pipe 316. The mixed solution of cyclohexanone oxime and methanol rotates at a high speed along the wall of the atomizing chamber 311 under the action of centrifugal force, and then obtains a tangential velocity through a swirl groove 3130 of a swirl disc 313. The mixed solution of cyclohexanone oxime and methanol is once broken and atomized to form a micro-liquid film, and leaves the swirl groove 3130 in a conical rotation (rotating mist cone). The rotation speed of the atomizing element is 15000 r / min, the top diameter of the atomizing chamber 311 is 80 mm, the bottom diameter of the atomizing chamber 311 is 160 mm, the height of the atomizing chamber 311 is 300 mm, and the height of the swirl disc 313 is 30 mm.

[0121] The nitrogen enters the gas preheater 210 through the first compressor 220 and is preheated to 230° C. The preheated nitrogen passes through the air inlet pipe 325 and enters the gas distribution plate 323 at a flow rate of 50 L / min. Under the flow guidance of the gas distribution plate 323, the swirl flow is performed, and the rotating fog cone and the rotating nitrogen swirl in the micro-interface vaporizer 300, and the micro-interface vaporizer 300 is preheated to 220° C. As the cross-section of the second cavity 322 continues to decrease, the two squeeze and cut each other, so that the micro-liquid film is broken and atomized into micro-droplets at the micron level for the second time, and the micro-droplets are quickly vaporized to form steam, and a mixed gas of cyclohexanone oxime vapor, methanol vapor and nitrogen is obtained. The inner diameter of the first cavity body 321 is 1000 mm, and the height of the first cavity body 321 is 1500 mm; the inner diameter of the top end of the second cavity body 322 is 1000 mm, the inner diameter of the bottom end of the second cavity body 322 is 250 mm, and the height of the second cavity body 322 is 1500 mm.

[0122] The mixed gas enters the reactor 400 filled with glass filler (glass balls) for secondary heating to obtain vaporized material. The secondary heating temperature is 370°C.

[0123] (2) The vaporized material enters the condenser 530 for condensation, the temperature of the condenser 530 is 5°C, and then passes through the gas-liquid separator 510, the temperature of the gas-liquid separator 510 is 30°C, and the condensate of cyclohexanone oxime and methanol and the first gas phase are collected in the gas-liquid separator 510, the first gas phase includes nitrogen and a small amount of uncondensed cyclohexanone oxime and methanol vapor. The first gas phase is passed into the methanol tail gas absorption device 520 for absorption to obtain methanol absorption liquid and nitrogen. After being compressed by the second compressor, the nitrogen is returned to the vaporization system for recycling.

[0124] The above device was operated for 500 hours. After testing, no blockage occurred in the pipeline, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.93%.

[0125] Example 4

[0126] The difference from Example 3 is that the device in Example 4 runs for 1000 hours. After testing, no blockage occurs in the pipeline, no obvious coking occurs inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime is 99.81%.

[0127] Example 5

[0128] The difference from Example 3 is that in Example 5, the device was operated for 2000 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.60%.

[0129] Example 6

[0130] The difference from Example 3 is that the rotation speed of the atomizer in Example 6 is 10000 r / min;

[0131] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.85%.

[0132] Example 7

[0133] The difference from Example 3 is that the rotation speed of the atomizer in Example 7 is 20000 r / min;

[0134] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.88%.

[0135] Example 8

[0136] The difference from Example 3 is that in Example 8, the top diameter of the atomizing chamber 311 is 60 mm, the bottom diameter is 120 mm, the height is 200 mm, and the height of the swirl disk 313 is 20 mm;

[0137] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.81%.

[0138] Example 9

[0139] The difference from Example 3 is that in Example 9, the top diameter of the atomizing chamber 311 is 100 mm, the bottom diameter is 200 mm, the height is 400 mm, and the height of the swirl disk 313 is 40 mm;

[0140] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.86%.

[0141] Example 10

[0142] The difference from Example 3 is that in Example 10, the top diameter of the atomizing chamber 311 is 60 mm, the bottom diameter is 120 mm, the height is 400 mm, and the height of the swirl disk 313 is 40 mm;

[0143] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.85%.

[0144] Embodiment 11

[0145] The difference from Example 3 is that in Example 11, the top diameter of the atomizing chamber 311 is 100 mm, the bottom diameter is 200 mm, the height is 200 mm, and the height of the swirl disk 313 is 20 mm;

[0146] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.87%.

[0147] Example 12

[0148] The difference from Example 3 is that in Example 12, the inner diameter of the first cavity body 321 is 800 mm, the height of the first cavity body 321 is 1000 mm, the top inner diameter of the second cavity body 322 is 800 mm, the bottom inner diameter of the second cavity body 322 is 200 mm, and the height of the second cavity body 322 is 1000 mm.

[0149] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.86%.

[0150] Example 13

[0151] The difference from Example 3 is that in Example 13, the inner diameter of the first cavity body 321 is 1200 mm, the height of the first cavity body 321 is 2000 mm, the top inner diameter of the second cavity body 322 is 1200 mm, the bottom inner diameter of the second cavity body 322 is 300 mm, and the height of the second cavity body 322 is 2000 mm.

[0152] The device was operated for 500 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.93%.

[0153] Embodiment 14

[0154] The difference from Example 3 is that in Example 14, the inner diameter of the first cavity body 321 is 800 mm, the height of the first cavity body 321 is 2000 mm, the top inner diameter of the second cavity body 322 is 800 mm, the bottom inner diameter of the second cavity body 322 is 200 mm, and the height of the second cavity body 322 is 2000 mm.

[0155] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.88%.

[0156] Embodiment 15

[0157] The difference from Example 3 is that in Example 15, the inner diameter of the first cavity body 321 is 1200 mm, the height of the first cavity body 321 is 1000 mm, the top inner diameter of the second cavity body 322 is 1200 mm, the bottom inner diameter of the second cavity body 322 is 300 mm, and the height of the second cavity body 322 is 1000 mm.

[0158] The device was operated for 500 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.91%.

[0159] Example 16

[0160] The difference from Example 3 is that in Example 16, the mixed solution of cyclohexanone oxime and methanol (the mass concentration of cyclohexanone oxime in the mixed solution is 20 wt %) is preheated to 20° C. in the raw material liquid storage tank;

[0161] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.92%.

[0162] Embodiment 17

[0163] The difference from Example 3 is that in Example 17, the mixed solution of cyclohexanone oxime and methanol (the mass concentration of cyclohexanone oxime in the mixed solution is 60wt%) is preheated to 60°C in the raw liquid storage tank;

[0164] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.87%.

[0165] Embodiment 18

[0166] The difference from Example 3 is that in Example 18, the mixed solution of cyclohexanone oxime and methanol (the mass concentration of cyclohexanone oxime in the mixed solution is 20wt%) is preheated to 60°C in the raw liquid storage tank;

[0167] The device was operated for 500 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.91%.

[0168] Embodiment 19

[0169] The difference from Example 3 is that in Example 19, the mixed solution of cyclohexanone oxime and methanol (the mass concentration of cyclohexanone oxime in the mixed solution is 60wt%) is preheated to 20°C in the raw liquid storage tank;

[0170] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.81%.

[0171] Embodiment 20

[0172] The difference from Example 3 is that in Example 20, the nitrogen is preheated to 200°C;

[0173] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.86%.

[0174] Embodiment 21

[0175] The difference from Example 3 is that in Example 21, the nitrogen is preheated to 210°C;

[0176] The device was operated for 500 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.91%.

[0177] Embodiment 22

[0178] The difference from Example 3 is that in Example 22, the nitrogen is preheated to 250°C;

[0179] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.90%.

[0180] Embodiment 23

[0181] The difference from Example 3 is that in Example 23, the nitrogen is preheated to 260°C;

[0182] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.84%.

[0183] Embodiment 24

[0184] The difference from Example 3 is that in Example 24, the microinterface vaporizer 300 is preheated to 140°C;

[0185] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.81%.

[0186] Embodiment 25

[0187] The difference from Example 3 is that in Example 25, the microinterface vaporizer 300 is preheated to 150°C;

[0188] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.85%.

[0189] Embodiment 26

[0190] The difference from Example 3 is that in Example 26, the microinterface vaporizer 300 is preheated to 240°C;

[0191] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.78%.

[0192] Embodiment 27

[0193] The difference from Example 3 is that in Example 27, the microinterface vaporizer 300 is preheated to 250°C;

[0194] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.72%.

[0195] Embodiment 28

[0196] The difference from Example 3 is that the secondary heating temperature in Example 28 is 350°C;

[0197] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.75%.

[0198] Embodiment 29

[0199] The difference from Example 3 is that the secondary heating temperature in Example 29 is 360°C;

[0200] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.86%.

[0201] Embodiment 30

[0202] The difference from Example 3 is that the secondary heating temperature in Example 30 is 380°C;

[0203] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.83%.

[0204] Embodiment 31

[0205] The difference from Example 3 is that the secondary heating temperature in Example 31 is 390°C;

[0206] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.72%.

[0207] Embodiment 32

[0208] The difference from Example 3 is that in Example 32, the feed flow rate of the mixed solution of cyclohexanone oxime and methanol is 25 mL / min, and the feed flow rate of nitrogen is 40 L / min;

[0209] The device was operated for 500 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.93%.

[0210] Embodiment 33

[0211] The difference from Example 3 is that in Example 33, the feed flow rate of the mixed solution of cyclohexanone oxime and methanol is 50 mL / min, and the feed flow rate of nitrogen is 60 L / min;

[0212] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.90%.

[0213] Embodiment 34

[0214] The difference from Example 3 is that in Example 34, the feed flow rate of the mixed solution of cyclohexanone oxime and methanol is 25 mL / min, and the feed flow rate of nitrogen is 60 L / min;

[0215] The device was operated for 500 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.93%.

[0216] Embodiment 35

[0217] The difference from Example 3 is that in Example 35, the feed flow rate of the mixed solution of cyclohexanone oxime and methanol is 50 mL / min, and the feed flow rate of nitrogen is 40 L / min;

[0218] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.86%.

[0219] Embodiment 36

[0220] The difference from Example 3 is that the filler of the reactor 400 in Example 36 is a ceramic filler;

[0221] The device was operated for 750 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.87%.

[0222] Embodiment 37

[0223] The difference from Example 3 is that the packing of the reactor 400 in Example 37 is stainless steel packing;

[0224] The device was operated for 650 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.74%.

[0225] Embodiment 38

[0226] The difference from Example 3 is that the filler of the reactor 400 in Example 38 is a titanium filler;

[0227] The device was operated for 720 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.83%.

[0228] Embodiment 39

[0229] The difference from Example 3 is that in Example 39, the temperature of the condenser 530 is 0°C, and the temperature of the gas-liquid separator 510 is 20°C;

[0230] The device was operated for 500 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.93%.

[0231] Embodiment 40

[0232] The difference from Example 3 is that in Example 40, the temperature of the condenser 530 is 10°C, and the temperature of the gas-liquid separator 510 is 40°C;

[0233] The device was operated for 500 hours, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 99.91%.

[0234] Comparative Example 1

[0235] The difference from Example 3 is that the rotation speed of the atomizing element in Comparative Example 1 is 0;

[0236] The device was operated for 500 h, and the vaporization equilibrium rate of cyclohexanone oxime was 96.64%.

[0237] Comparative Example 2

[0238] The difference from Example 3 is that the mixed solution of cyclohexanone oxime and methanol and nitrogen in Comparative Example 2 do not pass through the microinterface vaporizer 300, but are mixed in a stainless steel pipe, and after the mixed solution is vaporized at 220°C, it is passed into the reactor 400 for secondary heating;

[0239] The device was operated for 500 h, and the vaporization equilibrium rate of cyclohexanone oxime was 95.28%.

[0240] Comparative Example 3

[0241] The difference from Example 3 is that the rotation speed of the atomizer in Comparative Example 3 is 3000 r / min;

[0242] The device was operated for 500 h, the pipeline was not blocked, no obvious coking occurred inside the micro-interface vaporizer 300, and the vaporization equilibrium rate of cyclohexanone oxime was 97.36%.

[0243] Test Example 1

[0244] 1. The condensate of cyclohexanone oxime and methanol and the cyclohexanone oxime in the methanol absorption liquid obtained in the above Examples 3-40 and Comparative Examples 1-3 were subjected to gas chromatography quantitative analysis to calculate the vaporization equilibrium rate of cyclohexanone oxime. The results are shown in Table 1.

[0245] Among them, gas chromatography quantitative analysis was performed in an Agilent gas chromatograph instrument;

[0246] Cyclohexanone oxime vaporization equilibrium rate = (weight of condensate of cyclohexanone oxime and methanol per unit time × quantitative content of cyclohexanone oxime in condensate + weight of methanol absorption liquid per unit time × quantitative content of cyclohexanone oxime in methanol absorption liquid) / (weight of raw material liquid feed per unit time × mass concentration of cyclohexanone oxime in raw material liquid) × 100%;

[0247] Cyclohexanone oxime quantitative content = (internal standard weight / internal standard peak area) / (sampling weight / cyclohexanone oxime peak area) × correction factor; wherein the internal standard is m-dichlorobenzene, and the correction factor is obtained based on 99.8% analytically pure cyclohexanone oxime.

[0248] Gas-liquid feed volume ratio = nitrogen flow rate / flow rate of mixed solution of cyclohexanone oxime and methanol

[0249] 2. The mixed gas of cyclohexanone oxime steam, methanol steam and nitrogen obtained in Example 3 is passed into a reactor 400 filled with an MFI structure molecular sieve (the molecular sieve has a double ten-membered ring cross-channel structure), and is heated again to 370° C. in the reactor 400. The cyclohexanone oxime steam after the second heating is catalyzed by a catalyst to undergo a gas-phase rearrangement reaction to generate caprolactam; the material after the reaction enters a condenser 530 for condensation at a condensation temperature of 5° C., and then passes through a gas-liquid separator 510. The rearrangement reaction liquid A and the gas carrying a small amount of caprolactam steam are collected in the gas-liquid separator 510 at 30° C. The gas carrying a small amount of caprolactam steam is absorbed by a methanol tail gas absorption device 520 to obtain a rearrangement reaction liquid B and nitrogen. The nitrogen is compressed by a second compressor and returned to the system for recycling. The caprolactam in the rearrangement reaction liquid A and the rearrangement reaction liquid B is quantitatively analyzed by gas chromatography to calculate the caprolactam yield.

[0250] The device was operated for 2000 h, and the microinterface vaporizer 300 and the reactor 400 were not blocked. The rearrangement reaction liquid A and the rearrangement reaction liquid B were analyzed by gas chromatography, and the caprolactam yield was 96.26%.

[0251] Among them, gas chromatography quantitative analysis was performed in an Agilent gas chromatograph;

[0252] Cyclohexanone oxime conversion rate = {1-(weight of rearrangement reaction liquid A per unit time × quantitative content of cyclohexanone oxime in rearrangement reaction liquid A + weight of rearrangement reaction liquid B per unit time × quantitative content of cyclohexanone oxime in rearrangement reaction liquid B) / (weight of raw material liquid feed per unit time × mass concentration of cyclohexanone oxime in raw material liquid)} × 100%;

[0253] Caprolactam selectivity = (weight of rearrangement reaction liquid A per unit time × quantitative content of caprolactam in rearrangement reaction liquid A + weight of rearrangement reaction liquid B per unit time × quantitative content of caprolactam in rearrangement reaction liquid B) / (weight of raw material liquid feed per unit time × mass concentration of cyclohexanone oxime in raw material liquid) × 100%;

[0254] Caprolactam yield = cyclohexanone oxime conversion × caprolactam selectivity × 100%.

[0255] Table 1

[0256]

[0257]

[0258]

[0259] Note: Taking Example 3 as an example, the "8" in the atomization device parameter "8 / 16 / 30 / 3" means that the top diameter of the atomization chamber 311 is 8 cm, "16" means that the bottom diameter of the atomization chamber 311 is 16 cm, "30" means that the height of the atomization chamber 311 is 30 cm, and "3" means that the height of the swirl disk 313 is 3 cm. The micro-interface vaporizer parameters "100 / 150 / 100 / 25 / 150" are counted from left to right. The first "100" means that the inner diameter of the first cavity 321 is 100 cm, the first "150" means that the height of the first cavity 321 is 150 cm, the second "100" means that the top inner diameter of the second cavity 322 is 150 cm, "25" means that the bottom inner diameter of the second cavity 322 is 25 cm, and the second "150" means that the height of the second cavity 322 is 150 cm. In the carrier gas / micro-interface vaporizer preheating temperature “230 / 220”, “230” means that the preheating temperature of the carrier gas is 230°C, and “220” means that the preheating temperature of the micro-interface vaporizer 300 is 220°C.

[0260] From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects:

[0261] In the present application, the raw material liquid containing cyclohexanone oxime is passed into the rotating liquid distribution disk 312 in the atomizing element. The raw material liquid containing cyclohexanone oxime rotates along the wall of the atomizing chamber 311 under the action of centrifugal force, and then obtains the tangential velocity through the swirl groove 3130 of the swirl disk 313. The raw material liquid containing cyclohexanone oxime is broken and atomized once to form a micro liquid film, and leaves the swirl groove 3130 in a conical rotation (rotating mist cone). The carrier gas enters the gas distribution plate 323 through the air inlet pipe 325, and swirls under the diversion effect of the gas distribution plate 323. The outer side of the rotating fog cone is the carrier gas. The rotating fog cone and the rotating carrier gas swirl at high speed in the cavity of the micro-interface vaporizer 300. Because there is a certain amount of relative speed between the two, and as the cross section of the inverted truncated cone bottom of the cavity body is continuously reduced, the flow rate of the carrier gas increases, and the two squeeze and cut each other, the micro-liquid film is secondary broken and atomized into micro-droplets of micron level. At the same time, because the temperature of the carrier gas is high, the micro-droplets are rapidly vaporized once to form steam, and the steam containing cyclohexanone oxime is obtained. This vaporization method is enough to make cyclohexanone oxime evenly heated, and the decomposition of cyclohexanone oxime is reduced. Subsequently, the steam containing cyclohexanone oxime is passed into the reactor 400 for secondary heating, which further promotes the vaporization of cyclohexanone oxime into cyclohexanone oxime steam, and further reduces the decomposition of cyclohexanone oxime and improves the vaporization equilibrium rate of cyclohexanone oxime.

[0262] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A micro-interface vaporizer, characterized in that: The micro-interface vaporizer (300) comprises: a cavity body and an atomizing element extending into the cavity body, The atomizing element comprises an atomizing chamber (311), a liquid distribution plate (312) is arranged inside the atomizing chamber (311), a swirl plate (313) is arranged at the bottom of the atomizing chamber (311), the liquid distribution plate (312) is connected to a liquid inlet pipe (316), and the liquid inlet pipe (316) is used to transport the raw material liquid containing cyclohexanone oxime to the liquid distribution plate (312); A gas distribution plate (323) is further provided inside the cavity body. The gas distribution plate (323) is an annular structure. The gas distribution plate (323) is sleeved outside the atomization chamber (311), and the gas distribution plate (323) is higher than the swirl plate (313). The gas distribution plate (323) is connected to an air intake pipe (325), and the air intake pipe (325) is used to transport the carrier gas to the gas distribution plate (323); The bottom of the cavity is configured to be an inverted truncated cone, and a micro-interface vaporization outlet (324) is also provided at the bottom of the cavity.

2. The micro-interface vaporizer according to claim 1, characterized in that: A rotating shaft (314) is also inserted into the atomizing chamber (311), and the liquid distribution plate (312) and the swirl plate (313) are both annular structures and are respectively sleeved on the rotating shaft (314), and the liquid distribution plate (312) and the swirl plate (313) are respectively rotated under the drive of the rotating shaft (314); wherein the liquid distribution plate (312) is provided with a plurality of liquid fan-shaped grooves (3120), and the groove width of the liquid fan-shaped grooves (3120) gradually increases along the direction away from the annular center of the liquid distribution plate (312); the swirl plate (313) is provided with a plurality of swirl grooves (3130), and the plurality of swirl grooves (3130) are arranged in a circumferential array along the swirl plate (313), and the length direction of the swirl grooves (3130) is arranged along the radial direction of the swirl plate (313); And / or, the gas distribution plate (323) is arranged on the inner wall of the cavity body, and the gas distribution plate (323) is provided with a plurality of gas fan-shaped grooves (3230), and the groove width of the gas fan-shaped grooves (3230) gradually increases along the direction away from the annular center of the gas distribution plate (323).

3. The micro-interface vaporizer according to claim 1, characterized in that: The top diameter of the atomizing chamber (311) is 60-100 mm, and the bottom diameter of the atomizing chamber (311) is 120-200 mm; And / or, the height of the atomization chamber (311) is 200-400 mm; And / or, the swirl disc (313) comprises an upper dial and a lower dial, the upper dial and the lower dial are arranged opposite to each other, and the distance between the upper dial and the lower dial is 20-40 mm.

4. The microinterface vaporizer according to claim 1, characterized in that: The cavity body comprises a first cavity body (321) and a second cavity body (322), wherein the first cavity body (321) is cylindrical and the second cavity body (322) is an inverted truncated cone; the inner diameter of the first cavity body (321) is 800-1200 mm, and the height of the first cavity body (321) is 1000-2000 mm; Preferably, the ratio of the inner diameter of the first cavity (321) to the inner diameter of the bottom end of the second cavity (322) is (2-6):1; Preferably, the height of the second cavity (322) is 1000-2000 mm.

5. A cyclohexanone oxime vaporization system, characterized in that: The vaporization system comprises a vaporization unit, wherein the vaporization unit comprises a micro-interface vaporizer (300) and a reactor (400) connected in sequence, wherein the micro-interface vaporizer (300) is the micro-interface vaporizer (300) according to any one of claims 1 to 4; The inlet of the reactor (400) is connected to the micro-interface vaporization outlet (324).

6. The cyclohexanone oxime vaporization system according to claim 5, characterized in that: The vaporization system further comprises a raw material supply unit, wherein the raw material supply unit comprises a raw material liquid storage tank (110) and a gas storage tank; The outlet of the raw liquid storage tank (110) is connected to the liquid inlet pipeline (316), and the raw liquid storage tank (110) is used to supply the raw liquid containing cyclohexanone oxime; The outlet of the gas storage tank is connected to the air inlet pipeline (325), and the gas storage tank is used to supply carrier gas; Preferably, the raw material supply unit further comprises a gas preheater (210), and the gas preheater (210) is arranged on the pipeline between the gas storage tank and the air intake pipeline (325).

7. The cyclohexanone oxime vaporization system according to claim 6, characterized in that: The vaporization system further comprises a gas-liquid separation unit, and the gas-liquid separation unit further comprises a gas-liquid separator (510) and a methanol tail gas absorption device (520); The inlet of the gas-liquid separator (510) is connected to the outlet of the reactor (400), the bottom of the gas-liquid separator (510) is provided with a first liquid phase outlet, the top of the gas-liquid separator (510) is provided with a first gas phase outlet, and the first liquid phase outlet is used to discharge the first liquid phase; The inlet of the methanol tail gas absorption device (520) is connected to the first gas phase outlet, the top of the methanol tail gas absorption device (520) is provided with a second gas phase outlet, and the bottom of the methanol tail gas absorption device (520) is provided with a methanol absorption liquid outlet, the second gas phase outlet is used to discharge the carrier gas, and the methanol absorption liquid outlet is used to discharge the methanol absorption liquid; Preferably, the gas-liquid separation unit further comprises a condenser (530), and the condenser (530) is arranged on a pipeline between the reactor (400) and the gas-liquid separator (510); Preferably, the second gas phase outlet is connected to the gas storage tank for returning to the vaporization system of the cyclohexanone oxime for recycling.

8. A method for vaporizing cyclohexanone oxime, characterized in that: The vaporization method is carried out in a vaporization system of cyclohexanone oxime according to any one of claims 5 to 7, comprising the following steps: A raw material liquid containing cyclohexanone oxime is introduced into an atomizing element for primary crushing and atomization to form a micro-liquid film, and a carrier gas is introduced into a micro-interface vaporizer (300). The micro-liquid film and the carrier gas are secondary crushed and atomized and primary vaporized in the inverted truncated cone-shaped cavity of the micro-interface vaporizer (300), and then secondary heated in a reactor (400) to obtain cyclohexanone oxime vapor.

9. The method for vaporizing cyclohexanone oxime according to claim 8, characterized in that: The flow rate of the raw material liquid containing cyclohexanone oxime is 25-50 mL / min; And / or, the flow rate of the carrier gas is 40-60 L / min; And / or, the rotation speed of the atomizing element is 10000-20000 r / min; and / or, the temperature of the microinterface vaporizer (300) is 140-250°C, preferably 150-240°C; And / or, the secondary heating temperature is 350-390°C, preferably 360-380°C.

10. The method for vaporizing cyclohexanone oxime according to claim 8 or 9, characterized in that: The raw material liquid containing cyclohexanone oxime is firstly preheated and then introduced into the atomizing element; Preferably, the preheating temperature of the raw material liquid containing cyclohexanone oxime is 20-60° C., more preferably 25-50° C.; Preferably, the carrier gas is preheated before being introduced into the micro-interface vaporizer (300); Preferably, the preheating temperature of the carrier gas is 200-260°C, more preferably 210-250°C; Preferably, the raw material liquid containing cyclohexanone oxime is a mixed solution of cyclohexanone oxime and alcohol, wherein the mass concentration of cyclohexanone oxime is 20-60wt%, preferably 25-50wt%; Preferably, the alcohol in the mixed solution of cyclohexanone oxime and alcohol includes methanol and / or ethanol; Preferably, the carrier gas is nitrogen.

Citation Information

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