Equipment and method for liquid-liquid mixing enhanced catalysis in cyclohexanone device

By adopting liquid-liquid micro-mix and enhanced separation technology in the cyclohexanone device, the problems of high lye consumption and low production efficiency caused by traditional static mixers are solved, and the consumption of lye and production efficiency are reduced.

CN119897056APending Publication Date: 2025-04-29CHINA PETROLEUM & CHEMICAL CORP +2
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Patent Information

Application Number
CN202311408815.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-10-27
Publication Date
2025-04-29

AI Technical Summary

Technical Problem

In the existing cyclohexanone production process, the mixing capacity of the traditional static mixer is insufficient, resulting in the inability to form a uniform and stable alkaline environment during the reaction stage, thereby reducing production efficiency and increasing alkaline consumption.

Method used

A liquid-liquid mixing and strengthening catalytic equipment and methods in a cyclohexanone device are adopted, including a venturi mixer, a micromixer, a reaction tower and a strengthening separator. Through liquid-liquid micromixing technology and strengthening separation technology, a uniform and stable alkaline environment is formed to reduce alkaline liquid consumption.

Benefits of technology

The lye consumption in the cyclohexanone production process is reduced by more than 10%, the production efficiency is improved, and the separation treatment time is shortened by about 50% through the strengthening separator.

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Abstract

The invention relates to equipment and a method for liquid-liquid mixing enhanced catalysis in a cyclohexanone device. The equipment mainly comprises a micro mixer, a three-section reaction tower, an enhanced separator and a Venturi mixer. Oxidation liquid and alkali liquor are added into a micro-mixer to be fully mixed, discharged materials of the mixer enter a reaction tower, discharged materials of the reaction tower enter an enhanced separator, a product and waste alkali liquor are discharged from an outlet of the separator, and the waste alkali liquor enters a Venturi mixer to be mixed with new alkali liquor and then enters the micro-mixer. According to the invention, the median particle size lt of the dispersed phase liquid drops under the actual process condition can be realized; and the particle size of the dispersed phase is adjustable and controllable, so that the bias flow phenomenon of the alkali liquor in the oxidation liquid decomposition tower is effectively reduced, the recycling of the alkali liquor is realized, and the consumption of the alkali liquor is reduced by more than 10% (the alkali consumption is reduced by 50kg / t ketone). While efficient mixing is ensured, the separator is enhanced to realize separation between the product and the waste alkali liquid, and the yield is increased. Under the same treatment capacity, compared with the current common process equipment, the device disclosed by the invention is small in occupied area and high in treatment precision, and can be widely applied to the process needing mixing in the production of the petrochemical industry, so that the mixing efficiency is improved, and the particle size of a dispersed phase is adjustable and controllable.
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Description

Technical Field

[0001] The invention belongs to the fields of petrochemical industry and environmental protection, and specifically relates to a device and a method for liquid-liquid mixing enhanced catalysis in a cyclohexanone device. Background Art

[0002] Cyclohexanone is an important monomer for producing caprolactam, adipic acid and caprolactone, and is a solvent for various paint products. As an important organic chemical product, it is used more and more widely and the demand is also expanding. From the perspective of domestic cyclohexanone production process, the cyclohexane oxidation method is still the most widely used process route for producing cyclohexanone due to its relatively mature technology and stable source of raw materials, especially the cyclohexane non-catalytic oxidation method. At present, the process of producing cyclohexanone by the cyclohexane non-catalytic oxidation method mainly adopts static mixing in the process of mixing alkali solution and oxidation solution, but due to the poor mixing ability of the traditional static mixer, it is impossible to form a uniform and stable alkaline environment in the device during the reaction stage, which leads to the problems of reduced cyclohexanone production efficiency and increased alkali solution consumption. Therefore, it is urgent to develop a new method and equipment for liquid-liquid mixing and enhanced catalysis in the cyclohexanone device to reduce the alkali solution consumption.

[0003] CN107400038A provides a method for improving the preparation of cyclohexanone from cyclohexyl hydrogen peroxide and reducing alkali consumption, mainly under the two-step catalytic action of isooctyl chromate and cobalt acetate, cyclohexane is first decomposed into cyclohexanone and cyclohexanol, and then the organic phase and the inorganic phase are separated. Under this condition, the consumption of alkali solution is significantly reduced. CN113173839A provides a device for micro-extraction of cyclohexane oxidation liquid with effluent waste alkali solution, which uses effluent alkali solution and cyclohexane oxidation liquid for mixed extraction and fine separation, improves the decomposition absorption rate of cyclohexane oxidation liquid, realizes the recycling of effluent waste alkali from saponification separation, and reduces the alkali consumption and energy consumption in the decomposition reaction. At present, there is no patent related to liquid-liquid micro-mixing to enhance the mixing degree of alkali solution and oxidation solution, so it is of great significance to develop and utilize enhanced liquid-liquid mixing to reduce alkali consumption. Summary of the invention

[0004] The present invention aims at the deficiencies in the prior art and provides a device and method for liquid-liquid mixing intensified catalysis in a cyclohexanone device.

[0005] The present invention provides a device for liquid-liquid mixing enhanced catalysis in a cyclohexanone device, which mainly comprises a venturi mixer, a micro mixer, a reaction tower and an enhanced separator connected in sequence; the venturi mixer is provided with a new alkali solution inlet, a waste alkali solution inlet and an alkali solution outlet, and the alkali solution outlet is connected to the micro mixer; the micro mixer is provided with an alkali solution inlet, an oxidizing solution inlet and a mixed solution outlet, and the mixed solution outlet is connected to the reaction tower; the reaction tower is provided with a mixed solution inlet, and the outlet is connected to the enhanced separator; the enhanced separator is provided with an inlet, a product outlet and a waste alkali solution outlet, and the waste alkali solution outlet is connected to the venturi mixer.

[0006] The present invention is further configured such that a plurality of Venturi tubes are evenly distributed in the Venturi mixer, a plurality of nozzles are distributed at the small end of each Venturi tube, and the new alkali solution enters the Venturi tube from the nozzle to mix with the recovered alkali solution; the diameter of the large end of the Venturi tube is 1 / 5-1 / 4 of the diameter of the mixing chamber, and the diameter of the middle part is 1 / 8-1 / 6 of the diameter of the mixing chamber. Preferably, there are 10-20 Venturi tubes, 4-6 nozzles are distributed at the small end of each Venturi tube, and the length of the Venturi tube is 2 / 3 of the length of the mixer.

[0007] The present invention is further configured that the micro mixer adopts a device and method for enhancing liquid-liquid emulsification in CN112755826A, and the device includes a spraying part and an enhanced mixing part.

[0008] The present invention is further configured as follows: the micromixer injection part and the enhanced mixing part include a dispersed phase injection end, a continuous phase injection end, a mixing chamber, a primary turbulence section, and a secondary turbulence section. The diameter of the injection end is 1 / 2 of the diameter of the mixing chamber; a jet port is provided at the top of the injection end, and the diameter of the jet port is 0.5 mm. The mixing chamber is a spiral structure, and its length is 1 / 5 of the length of the mixer. The turbulence section is divided into a spiral section, a cavity section and a variable diameter section. The length of the spiral section is 1 / 6 of the length of the mixer, and the length of the variable diameter section is 1 / 4 of the length of the mixer.

[0009] The present invention is further configured such that the reaction tower is a three-stage reaction tower, and the filler in the reaction tower is a random packing.

[0010] The present invention is further configured such that the enhanced separator is a horizontal separator, comprising a liquid distributor, a rectifier, a pre-agglomeration module, an enhanced agglomeration module, a graded depth sedimentation module, an interface meter, and a water bag.

[0011] The present invention is further configured such that the liquid distributor includes a tube-type liquid distributor and a disc-type liquid distributor, preferably a T-type tube-type liquid distributor, and small holes are evenly distributed on the T-type tubes.

[0012] The present invention is further configured such that the rectifier is a perforated flat plate with a hole diameter of 2 mm, a hole center distance of 6 mm, and a perforation rate of 20%-40%.

[0013] The present invention is further configured as follows: the pre-enhanced agglomeration module is woven by an X-type weaving method in an X-type fiber weaving method suitable for oil-water separation in CN103952853B, and the material is a hydrophilic fiber material, and the hydrophilic material includes but is not limited to stainless steel; the enhanced agglomeration module is woven by an Ω-type weaving method in an Ω-type fiber weaving method suitable for oil-water separation in CN103952852B, and the material is oleophilic and hydrophilic fiber materials, and the ratio of oleophilic to hydrophilic fibers is 1:1, wherein the oleophilic fiber materials include but are not limited to tetrafluoroethylene and polypropylene, and the hydrophilic fiber materials include but are not limited to stainless steel.

[0014] The present invention is further configured such that the interior of the graded depth sedimentation module is a corrugated plate, and the angle between the corrugated plate and the horizontal plane is 30°-60°. The graded depth sedimentation module includes a separation layer, a demulsification layer, and a coalescence layer from top to bottom. The separation layer corrugated plate is made of an oleophilic material, including but not limited to polytetrafluoroethylene; the coalescence layer corrugated plate is made of a hydrophilic material, including but not limited to polytetrafluoroethylene; the demulsification layer corrugated plate is made of an oleophilic material and a hydrophilic material stacked alternately; the crests and troughs of the corrugated plate are both provided with an equal number of small holes, and the number of holes is adjusted according to the actual situation of the separated material.

[0015] The present invention also provides a method for liquid-liquid mixing enhanced catalysis in a cyclohexanone device using the above-mentioned device, comprising the following steps: (1) The oxidizing liquid and the alkali solution enter the micro mixer and are mixed in the mixer; (2) The mixed materials in step (1) enter a reaction tower and react in the reaction tower; (3) The material obtained from the reaction tower in step (2) enters the enhanced separator to separate the product from the waste alkali liquid; (4) The waste alkali solution obtained in step (3) enters the venturi mixer, mixes with the new alkali solution, and then re-enters the micro mixer.

[0016] In the method of the present invention, the flow ratio of the alkali solution to the oxidizing solution in the micromixer is 0.4-0.8, and the flow ratio can be adjusted to achieve control of the particle size of the alkali solution dispersed phase.

[0017] The method of the present invention further comprises that after mixing in the micro mixer, the particle size distribution of the alkali solution dispersed phase is 5-50 um, wherein the median particle size of the alkali solution dispersed phase droplets is less than 40 um.

[0018] The method of the present invention further has an oil-water separation efficiency >95% after separation by the enhanced separator, a removal efficiency of no less than 95% for water droplets with a diameter greater than 15 um, and a removal rate of no less than 50% for water droplets with a diameter less than 15 um.

[0019] In the method of the present invention, the working pressure of the enhanced separator is 0.3-0.8 MPa, and the cross-sectional flow velocity is 0.001-0.02 m / s.

[0020] In the method of the present invention, the concentration of the alkali solution at the outlet of the Venturi mixer is 10%-15%.

[0021] The present invention has the following beneficial effects: (1) The present invention uses unpowered separation and mixing equipment throughout the process, thereby achieving energy consumption reduction;

[0022] (2) The alkali washing and water washing process of the present invention adopts a liquid-liquid micro-mixing method and equipment to form a uniform and stable alkaline environment, thereby improving the production efficiency of cyclohexanone and reducing the consumption of alkali solution by more than 10%;

[0023] (3) The present invention uses a venturi mixer to mix the waste alkali solution with the new alkali solution to form alkali solution, thereby reducing the consumption of alkali solution;

[0024] (4) The present invention can achieve rapid separation of the product and the waste alkali solution by adopting an enhanced separator, which shortens the processing time by 50% compared with the traditional separation method. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is an equipment process flow chart of the liquid-liquid mixing enhanced catalytic method in a cyclohexanone device according to an embodiment of the present invention.

[0026] Figure 2 Schematic diagram of the structure of the micro mixer in the embodiment.

[0027] Figure 3 It is a schematic diagram of the structure of the reaction tower in the embodiment.

[0028] Figure 4 Schematic diagram of the structure of the enhanced separator in the embodiment.

[0029] Figure 5 Schematic diagram of the structure of the venturi mixer in the embodiment.

[0030] Figure 6 Schematic diagram of the structure of the venturi tube in the embodiment. Implementation

[0031] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Example

[0032] In view of the problems that the liquid-liquid mixing efficiency is low and the alkali solution consumption is large in a certain chemical plant in the treatment of cyclohexanone, the production process is optimized by using a method and equipment for liquid-liquid mixing enhanced catalysis in a cyclohexanone device involved in the present invention, so that the particle size of the dispersed phase after treatment by this process is adjustable and controllable; for the cyclohexanone device, the alkali solution deviation phenomenon in the oxidation liquid decomposition tower is effectively reduced, the alkali solution is reused, and the alkali solution consumption is reduced by more than 10% (alkali consumption is reduced by 50kg / t ketone). Example 1

[0033] A device for liquid-liquid mixing intensified catalysis in a cyclohexanone device Figure 1-6 , mainly including a venturi mixer, a micro mixer, a reaction tower and an enhanced separator connected in sequence; the venturi mixer is provided with a new alkali solution inlet, a waste alkali solution inlet and an alkali solution outlet, and the alkali solution outlet is connected to the micro mixer; the micro mixer is provided with an alkali solution inlet, an oxidizing solution inlet and a mixed solution outlet, and the mixed solution outlet is connected to the reaction tower; the reaction tower is provided with a mixed solution inlet, and the outlet is connected to the enhanced separator; the enhanced separator is provided with an inlet, a product outlet and a waste alkali solution outlet, and the waste alkali solution outlet is connected to the venturi mixer.

[0034] In the embodiment, 15 Venturi tubes are evenly distributed in the Venturi mixer, and 4-65 nozzles are distributed at the small end of each Venturi tube. The new alkali solution enters the Venturi tube from the nozzle and mixes with the recovered alkali solution; the diameter of the large end of the Venturi tube is 1 / 4 of the diameter of the mixing chamber, the diameter of the middle part is 1 / 6 of the diameter of the mixing chamber, and the length of the Venturi tube is 2 / 3 of the length of the mixer.

[0035] In the embodiment, the micromixer adopts a device in a device and method for enhancing liquid-liquid emulsification in CN112755826A, including an injection part and an enhanced mixing part, specifically including a dispersed phase injection end, a continuous phase injection end, a mixing chamber, a primary turbulent section, and a secondary turbulent section. The diameter of the injection end is 1 / 2 of the diameter of the mixing chamber; a jet port is provided at the top of the injection end, the diameter of the jet port is 0.5 mm, the mixing chamber is a spiral structure, and the length is 1 / 5 of the length of the mixer. The turbulent section is divided into a spiral section, a cavity section and a variable diameter section. The length of the spiral section is 1 / 6 of the length of the mixer, and the length of the variable diameter section is 1 / 4 of the length of the mixer.

[0036] In the embodiment, the reaction tower is a three-stage reaction tower, and the filler in the reaction tower is a random packing.

[0037] In the embodiment, the enhanced separator is a horizontal separator, including a liquid distributor, a rectifier, a pre-agglomeration module, an enhanced agglomeration module, a graded depth sedimentation module, an interface meter, and a water bag. Example 2

[0038] The method for liquid-liquid mixing intensified catalysis in a cyclohexanone device using the equipment of Example 1 is specifically implemented using the following process (see Figure 1 ): (1) The oxidizing liquid and the alkali liquid first enter a micro mixer (the alkali liquid micro mixer in this example adopts a device and method for enhancing liquid-liquid emulsification in CN112755826A, and the flow ratio of the alkali liquid to the oxidizing liquid is 0.6). The mixed liquid enters a reaction tower for reaction.

[0039] (2) After being mixed in the micro mixer, it enters the reaction tower. After a certain period of reaction in the reaction tower, the cyclohexane in the oxidizing liquid is fully oxidized into cyclohexanone and other products. The mixed solution with the alkali solution enters the enhanced separator, where the particle size distribution of the alkali solution dispersed phase is 5-50, and the median particle size of the alkali solution dispersed phase droplets is 30um.

[0040] (3) The mixture coming out of the reaction tower enters the enhanced separator. Specifically, it enters the liquid distributor through the inlet pipe (in this example, a T-shaped tube-type liquid distributor is selected, and there are 20 evenly distributed small holes on the T-shaped tube). The incoming flow impacts the T-shaped tube to offset most of the kinetic energy, and then the flow is discharged from the holes; further, the mixture is guided to the rectifier (in this example, a perforated plate is used, with a hole diameter of 2 mm, a hole center distance of 6 mm, and a perforation rate of 25%); the rectified mixture passes through the pre-agglomeration module (in this example, the volume specific surface area of ​​the pre-agglomeration module is 5000m 2 / m 3 , porosity 0.75, module depth 400mm, all made of hydrophilic fibers woven according to the X-type weaving method in CN103952853B suitable for oil-water separation, the hydrophilic fiber material is stainless steel); the water droplets in the mixture quickly coalesce and grow under the interception of the hydrophilic fibers. The mixture after the pre-coagulation module enters the enhanced coalescence module (in this example, the volume specific surface area of ​​the enhanced coalescence module is 5000 m 2 / m 3, the porosity is 0.75, the module depth is 400mm, the weaving method is woven by an Ω-type fiber weaving method suitable for oil-water separation in CN103952852B, the ratio of hydrophilic to lipophilic fibers is 1:1, the lipophilic fiber material is tetrafluoroethylene, and the hydrophilic fiber material is stainless steel), Under the action of polar forces at different fiber nodes, the emulsified water droplets adhere to the hydrophilic fibers and aggregate, and the emulsified water droplets are converted into a free state; the mixture enters the graded depth enhanced agglomeration module (in this example, the graded enhanced sedimentation module depth is 400mm). The alkali solution is transported to the Venturi mixer through the water bag for reuse of the waste alkali solution, and the product is sent to the product storage tank. After separation by the enhanced separator, the separation efficiency of oil and water is 97%, the removal efficiency of water droplets with a diameter greater than 15um is 97%, and the removal rate of water droplets with a diameter less than 15um is 60%. The working pressure of the enhanced separator is 0.6MPa, and the cross-sectional flow rate is 0.01m / s.

[0041] (4) After the waste alkali liquid is separated from the product in the enhanced separator, it enters the Venturi mixer to mix with the newly added alkali liquid, and then enters the micro-mixer to mix with the oxidizing liquid. The alkali liquid concentration out of the Venturi mixer is 10%, and the alkali consumption is reduced by 12% compared with the original device, thereby achieving the purpose of saving alkali liquid. Example 3

[0042] A chemical plant currently produces cyclohexanone by cyclohexane non-catalytic oxidation. When treating cyclohexanone, a static mixer is used to mix the cyclohexanone before entering the tower for reaction to increase the contact area between the sodium hydroxide solution and the oxidizing liquid. However, due to the poor mixing effect of the static mixer, the alkali solution flows sideways in the reaction tower, resulting in a decrease in the conversion efficiency of the oxidizing liquid.

[0043] In order to solve the problem of alkali solution deviation, a device for liquid-liquid mixing and catalytic enhancement in a cyclohexanone device described in Example 1 is introduced into the process, and the micro-mixer is adopted, which can ultimately reduce the alkali consumption by more than 10% compared with the original device. Example 4

[0044] The method steps are the same as those in Example 2, except that in step (1), the flow ratio of alkali solution to oxidizing liquid is 0.7; in step (2), the particle size distribution of the alkali solution dispersed phase after mixing is 5-45um, wherein the median particle size of the alkali solution dispersed phase droplets is 28um; in step (3), the separation efficiency of oil and water after separation by the enhanced separator is 9896%, the removal efficiency for water droplets with a diameter greater than 15um is 98%, and the removal rate for water droplets with a diameter less than 15um is 58%; the working pressure of the enhanced separator is 0.65MPa, and the cross-sectional flow rate is 0.01m / s; in step (4), the alkali solution concentration at the outlet of the Venturi mixer is 11%, and the alkali consumption is reduced by 11% compared with the original device. Example 5

[0045] In the embodiment, 10 Venturi tubes are evenly distributed in the Venturi mixer, and 4 nozzles are distributed on the small end of each Venturi tube. New alkali solution enters the Venturi tube from the nozzle and mixes with the recovered alkali solution. The diameter of the large end of the Venturi tube is 1 / 5 of the diameter of the mixing chamber, the diameter of the middle part is 1 / 8 of the diameter of the mixing chamber, and the length of the Venturi tube is 2 / 3 of the length of the mixer.

[0046] The device parameters of the micro mixer of the device of Example 1 are adopted, and the flow ratio of alkali solution to oxidizing liquid is 0.6; in step (2), the particle size distribution of the alkali solution dispersed phase after mixing is 3-40um, wherein the median particle size of the alkali solution dispersed phase droplets is 25um; in step (3), the separation efficiency of oil and water after separation by the enhanced separator is 98%, the removal efficiency of water droplets with a diameter greater than 15um is 98%, and the removal rate of water droplets with a diameter less than 15um is 70%; the working pressure of the enhanced separator is 0.7MPa, and the cross-sectional flow rate is 0.008m / s; in step (4), the alkali solution concentration at the outlet of the Venturi mixer is 11%, and the alkali consumption is reduced by 11% compared with the original device. Example 6

[0047] The method steps are the same as those in Example 5, except that in step (1), the flow ratio of the alkali solution to the oxidizing liquid is 0.6; in step (2), the particle size distribution of the alkali solution dispersed phase after mixing is 3-40um, wherein the median particle size of the alkali solution dispersed phase droplets is 27um; in step (3), the separation efficiency of oil and water after separation by the enhanced separator is 98%, the removal efficiency of water droplets with a diameter greater than 15um is 98%, and the removal rate of water droplets with a diameter less than 15um is 72%; the working pressure of the enhanced separator is 0.75MPa, and the cross-sectional flow rate is 0.008m / s; in step (4), the alkali solution concentration at the outlet of the Venturi mixer is 11%, and the alkali consumption is reduced by 12% compared with the original device. Example 7

[0048] In the embodiment, 15 Venturi tubes are evenly distributed in the Venturi mixer, and 5 nozzles are distributed on the small end of each Venturi tube. New alkali solution enters the Venturi tube from the nozzle and mixes with the recovered alkali solution; the diameter of the large end of the Venturi tube is 1 / 4 of the diameter of the mixing chamber, the diameter of the middle part is 1 / 6 of the diameter of the mixing chamber, and the length of the Venturi tube is 2 / 3 of the length of the mixer.

[0049] In the embodiment, the volume specific surface area of ​​the pre-coagulation module of the enhanced separator is 6000m 2 / m 3 , porosity 0.55, module depth 400mm, all of which are woven with hydrophilic fibers according to an X-type fiber weaving method suitable for oil-water separation in CN103952853B, and the hydrophilic fiber material is stainless steel.

[0050] The device parameters of the micro mixer of the device of Example 1 are adopted, and the flow ratio of alkali solution to oxidizing liquid is 0.6; in step (2), the particle size distribution of the alkali solution dispersed phase after mixing is 10-55um, wherein the median particle size of the alkali solution dispersed phase droplets is 35um; in step (3), the separation efficiency of oil and water after separation by the enhanced separator is 98%, the removal efficiency of water droplets with a diameter greater than 15um is 98%, and the removal rate of water droplets with a diameter less than 15um is 70%; the working pressure of the enhanced separator is 0.6MPa, and the cross-sectional flow rate is 0.008m / s; in step (4), the alkali solution concentration at the outlet of the Venturi mixer is 12%, and the alkali consumption is reduced by 10% compared with the original device.

[0051] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A device for liquid-liquid mixing intensified catalysis in a cyclohexanone device, characterized in that It comprises a venturi mixer, a micro mixer, a reaction tower and an enhanced separator which are connected in sequence; the venturi mixer is provided with a new alkali solution inlet, a waste alkali solution inlet and an alkali solution outlet, and the alkali solution outlet is connected to the micro mixer; the micro mixer is provided with an alkali solution inlet, an oxidizing solution inlet and a mixed solution outlet, and the mixed solution outlet is connected to the reaction tower; the reaction tower is provided with a mixed solution inlet, and the outlet is connected to the enhanced separator; the enhanced separator is provided with an inlet, a product outlet and a waste alkali solution outlet, and the waste alkali solution outlet is connected to the venturi mixer.

2. The device according to claim 1, characterized in that A plurality of Venturi tubes are evenly distributed in the Venturi mixer, and a plurality of nozzles are distributed at the small end of each Venturi tube; the diameter of the large end of the Venturi tube is 1 / 5-1 / 4 of the diameter of the mixing chamber, and the diameter of the middle part is 1 / 8-1 / 6 of the diameter of the mixing chamber.

3. The device according to claim 2, characterized in that There are 10 to 20 venturi tubes, each of which has 4 to 6 nozzles at its small end, and the length of the venturi tube is 2 / 3 of the length of the mixer.

4. The device according to claim 1, characterized in that The micro mixer comprises an injection part and an enhanced mixing part, and is provided with a dispersed phase injection end, a continuous phase injection end, a mixing chamber, a primary turbulent section, and a secondary turbulent section.

5. The device according to claim 4, characterized in that The diameter of the injection end is 1 / 2 of the diameter of the mixing chamber; a jet port is provided at the top of the injection end, and the diameter of the jet port is 0.5 mm; the mixing chamber is a spiral structure, and its length is 1 / 5 of the length of the mixer; the turbulent section is divided into a spiral section, a cavity section and a variable diameter section, the length of the spiral section is 1 / 6 of the length of the mixer, and the length of the variable diameter section is 1 / 4 of the length of the mixer.

6. The device according to claim 1, characterized in that The reaction tower is a three-stage reaction tower; the enhanced separator is a horizontal separator.

7. The device according to claim 1, characterized in that The filler in the three-stage reaction tower is a random filler; the enhanced separator includes a liquid distributor, a rectifier, a pre-agglomeration module, an enhanced agglomeration module, a graded depth sedimentation module, an interface meter, and an acid bag.

8. The device according to claim 7, characterized in that The liquid distributor includes a tube-type liquid distributor and a disc-type liquid distributor, preferably a T-type tube-type liquid distributor, with small holes evenly distributed on the T-type tubes.

9. The device according to claim 7, characterized in that The rectifier is a perforated flat plate with a hole diameter of 2 mm, a hole center distance of 6 mm, and a perforation rate of 20%-40%.

10. The device according to claim 7, characterized in that The pre-reinforced coalescence module is woven from hydrophilic fibers by an X-type fiber weaving method; the reinforced coalescence module is woven from oleophilic and hydrophilic fibers by an Ω-type fiber weaving method, and the ratio of the oleophilic and hydrophilic fibers is 1:

1.

11. The device according to claim 7, characterized in that The interior of the graded depth sedimentation module is a corrugated plate, and the angle between the corrugated plate and the horizontal plane is 30°-60°; the graded depth sedimentation module includes a separation layer, a demulsification layer, and a coalescence layer from top to bottom; the separation layer corrugated plate is made of oleophilic material; the coalescence layer corrugated plate is made of hydrophilic material; the demulsification layer corrugated plate is made of oleophilic material and hydrophilic material stacked alternately; the crests and troughs of the corrugated plate are opened with an equal number of small holes, and the number of openings is adjusted according to the actual situation of the separated material.

12. A method for enhancing catalysis by liquid-liquid mixing in a cyclohexanone device using the device of any one of claims 1 to 11, characterized in that The following steps are involved: (1) The oxidizing liquid and the alkali solution enter the micro mixer and are mixed in the mixer; (2) The mixed materials in step (1) enter a reaction tower and react in the reaction tower; (3) The material obtained from the reaction tower in step (2) enters the enhanced separator to separate the product from the waste alkali liquid; (4) The waste alkali solution obtained in step (3) enters the venturi mixer, mixes with the new alkali solution, and then re-enters the micro mixer.

13. The method according to claim 12, characterized in that In step (1), the oxidizing solution and the alkali solution are fully mixed in a micro mixer, and the particle size distribution of the alkali solution dispersed phase is 5-50um, wherein the median particle size of the alkali solution dispersed phase droplets is <40um, and the flow ratio of the alkali solution to the oxidizing solution is 0.4-0.

8. The particle size of the alkali solution dispersed phase is controlled by adjusting the flow ratio.

14. The method according to claim 12, characterized in that In step (3), the separation efficiency of the product after separation by the enhanced separator is greater than 95%, the removal efficiency of water droplets with a diameter greater than 15 μm is not less than 95%, and the removal rate of water droplets with a diameter less than 15 μm is not less than 50%; the working pressure of the enhanced separator is 0.3-0.8 MPa, and the cross-sectional flow rate is 0.001-0.02 m / s.

15. The method according to claim 12, characterized in that In step (4), the concentration of the alkali solution reaches 10%-15% after passing through the Venturi mixer.

Citation Information

Patent Citations

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