Device and method for continuously and mildly producing cyclohexene oxide without catalyst

Through the device and method of continuously gentle production of epoxy cyclohexane without catalysts, the pipeline design and strengthening reactors are used to solve the problems of long reaction time, high cost and serious pollution in traditional methods, and achieve high efficiency, economical and environmentally friendly Epoxy cyclohexane production improves product purity and safety.

CN119113968APending Publication Date: 2024-12-13NANJING YANCHANG REACTION TECH RES INST CO LTD
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Patent Information

Application Number
CN202411555999.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-04
Publication Date
2024-12-13

AI Technical Summary

Technical Problem

The traditional epoxy cyclohexane production methods have problems such as long reaction time, high cost, serious pollution, serious equipment corrosion, many side reactions, and difficulty in meeting environmental standards. They have failed to effectively solve the demand for economic, environmentally friendly and high-purity epoxy cyclohexane production technology. .

Method used

A device and method for continuously gentle production of epoxy cyclohexane without catalyst was designed. Through pipeline design and strengthening the application of reactor, the side reactions are reduced, the reaction efficiency and raw material conversion rate are improved, and the gas-liquid two-phase reverse hedging technology is adopted. , realize normal temperature and pressure operation, avoid high-pressure towers, and use circulation pipelines for raw material recycling and by-product utilization.

Benefits of technology

It significantly improves the reaction efficiency and raw material conversion rate, reduces costs, conforms to the concept of green chemistry, improves the purity and economic benefits of the product, and enhances the safety and environmental benefits of the reaction process.

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Abstract

The invention provides a device and a method for continuously and mildly producing cyclohexene oxide without a catalyst, the device comprises a reaction tank, the inner top of the reaction tank is provided with a liquid enhanced reactor, the liquid enhanced reactor is externally connected with a mixing pipeline, and the mixing pipeline is connected with the liquid enhanced reactor. The mixing pipeline is formed by converging a first circulating pipeline, a second circulating pipeline and a third circulating pipeline through a liquid mixer 1, and the first circulating pipeline is used for reaction; the second circulating pipeline is used for separation and recovery; the third circulating pipeline is used for refining, and the first circulating pipeline, the second circulating pipeline and the third circulating pipeline are connected in parallel. According to the device, side reactions can be reduced to a great extent through the design of the pipeline and the application of the enhanced reactor, the reaction efficiency and the conversion rate of raw materials are improved, the reaction cost can be reduced, and the concept of green chemistry is better met.
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Description

Technical Field

[0001] The invention belongs to the technical field of chemical industry, and in particular to a device and method for continuously and gently producing cyclohexene oxide without catalyst. Background Art

[0002] Epoxycyclohexane is the main raw material for the synthesis of the pesticide propargite. In recent years, the market demand for epoxycyclohexane has been on the rise. However, the traditional production method of epoxycyclohexane has problems such as long reaction time, high cost, and difficulty in meeting environmental standards. The production of epoxycyclohexane using cyclohexene as raw material is a new method that has emerged in recent years. This method is divided into organic peroxide epoxidation method, hypochlorous acid method, electrochemical method, etc. according to the different oxygen sources. However, problems such as severe pollution, severe equipment corrosion, many side reactions, and high cost have not yet been overcome. Therefore, it is of great significance to study and develop economical and environmentally friendly production technology for high-purity epoxycyclohexane.

[0003] In view of this, the present invention is proposed. Summary of the invention

[0004] The first purpose of the present invention is to provide a device for continuously and gently producing cyclohexene oxide without a catalyst. The device can greatly reduce the occurrence of side reactions through the design of pipelines and the application of enhanced reactors, improve reaction efficiency and the conversion rate of raw materials, and at the same time reduce reaction costs, which is more in line with the concept of green chemistry.

[0005] The second purpose of the present invention is to provide the above-mentioned catalyst-free continuous and mild reaction method for producing cyclohexene oxide. This method, when used in conjunction with a reaction device, can more effectively improve the reaction efficiency and the conversion rate of raw materials; and the method has simple steps and is more economical and environmentally friendly. In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted: The present invention provides a catalyst-free, continuous and mild device for producing cyclohexene oxide, comprising: A reaction tank, wherein a liquid enhanced reactor is arranged on the inner top of the reaction tank, wherein the liquid enhanced reactor is externally connected to a mixing pipeline, wherein the mixing pipeline is formed by a first circulation pipeline, a second circulation pipeline and a third circulation pipeline being brought together through a liquid mixer 1, wherein the first circulation pipeline is used for reaction; the second circulation pipeline is used for separation and recovery; the third circulation pipeline is used for refining, and the first circulation pipeline, the second circulation pipeline and the third circulation pipeline are connected in parallel.

[0006] Preferably, as a further specific embodiment, a gas intensification reactor is provided at the inner bottom of the reaction tank, and the gas intensification reactor is directly connected to a gas delivery pump provided at the bottom of the reaction tank; a pipeline is provided on the side wall of the reaction tank to connect with a flash tank, and a pipeline is provided at the bottom of the flash tank to form a first circulation pipeline through the liquid mixer 1 and the mixing pipeline.

[0007] Preferably, as a further specific implementation manner, the inlets of the first circulation pipeline and the second circulation pipeline are connected in parallel through a flash tank, a pipeline is provided on the top of the flash tank to connect with the middle part of the side wall of the product separation tower, a pipeline is provided on the top of the product separation tower to connect with the middle part of the side wall of the recovery tower, a pipeline is provided at the top outlet of the recovery tower to form a collecting pipe through a liquid mixer 2, and the collecting pipe merges into the mixing pipeline through the liquid mixer 1 to form the second circulation pipeline; the product separation tower and the recovery tower are connected in series.

[0008] Preferably, as a further specific embodiment, the inlets of the second circulation pipeline and the third circulation pipeline are connected in parallel through the separation tower, the bottom of the separation tower is provided with a pipeline connected to the middle of the side wall of the product refining tower, and the top outlet of the product refining tower is provided with a pipeline to form a collecting pipe through a liquid mixer 2, and the collecting pipe merges into the mixing pipeline through the liquid mixer 1 to form the third circulation pipeline.

[0009] Preferably, as a further specific implementation, the product separation tower, recovery tower and product refining tower are all equipped with a condenser, a reboiler and a reflux tank.

[0010] Preferably, as a further specific embodiment, the reaction device further comprises a raw material premixer, and the raw material premixer enters the mixing pipeline through the liquid mixer 1 and is connected to the reaction tank.

[0011] Preferably, as a further specific embodiment, the raw material premixer is directly connected to the raw material storage tank, and a stirring paddle is provided inside the raw material premixer, and the stirring paddle is located at 1 / 3-1 / 2 of the distance from the bottom of the raw material premixer.

[0012] Preferably, as a further specific implementation, the product separation tower, recovery tower and product refining tower are all provided with tower plates, the total number of tower plates of the product separation tower is 15-30; the total number of tower plates of the recovery tower is 15-35; the total number of tower plates of the product refining tower is 20-40.

[0013] The present invention also provides a reaction method for continuously and mildly producing cyclohexene oxide without a catalyst, comprising the following steps: Premixing the reactants and then reacting them; The obtained product is obtained through flash evaporation, cyclic separation, refinement and recovery.

[0014] Preferably, as a further specific embodiment, the reaction temperature of the reaction is 15°C-30°C, and the reaction pressure is 0.8 atm-2atm; The flash evaporation temperature is 100°C-160°C, and the flash evaporation pressure is 0.5atm-2atm; The separation temperature is 55°C-105°C, the separation pressure is 0.5 atm-1.5 atm, and the reflux ratio is 4.6-6; The refining temperature is 100°C-150°C, the refining pressure is 0.5atm-1.5atm, and the reflux ratio is 4.3-5.6; The recovery temperature is 120° C.-230° C., the recovery pressure is 4.5 atm-7 atm, and the reflux ratio is 4-8.

[0015] Compared with the prior art, the present invention has the following beneficial effects: (1) Through the gas-enhanced reactor and the liquid-enhanced reactor, the gas-liquid two-phase materials can be counter-charged, which increases the residence and retention time of the micro-droplets, improves the mass transfer effect between the reaction materials, and improves the reaction efficiency.

[0016] (2) During the reaction stage, the reaction is carried out at room temperature and pressure without using a catalyst. The operating conditions are mild, which greatly improves the safety and environmental benefits of the reaction process. During the separation and refining of the cyclohexene oxide product, the reaction is carried out at room pressure without using a high-pressure tower, thus avoiding the occurrence of other side reactions. The material recovery system can recover almost all solvents, electrolytes and unreacted materials, and at the same time obtain high-purity by-product cyclohexanone, which can improve economic benefits.

[0017] (3) Through the design of the pipeline, the reaction raw materials can be used efficiently, and the high-purity by-products generated during the reaction can be recovered and utilized in a timely manner, avoiding the by-products from entering the reaction again. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 : Example 1 is a schematic diagram of the structure of a device for continuously and gently producing cyclohexene oxide without a catalyst; Figure 2 : Schematic diagram of the first circulation pipeline in Example 1; Figure 3 : Schematic diagram of the second circulation pipeline in Example 1; Figure 4 : Schematic diagram of the third circulation pipeline in Example 1.

[0019] in: 1-reaction tank, 2-liquid enhanced reactor, 3-gas enhanced reactor, 4-flash tank, 5-product separation tower, 6-recovery tower, 7-product refining tower, 8-raw material premixer, 9-liquid mixer 3, 10-liquid mixer 1, 11-Liquid mixer 2, 12-Reboiler 1, 13-Reboiler 2, 14-Reboiler 3, 15-Reflux tank 1, 16- reflux tank 2, 17- reflux tank 3, 18- condenser 1, 19- condenser 2, 20- condenser 3, 21-delivery pump 1, 22-delivery pump 2, 23-delivery pump 3, 24-delivery pump 4, 25-delivery pump 5, 26-delivery pump 6, 27-delivery pump 7, 28-delivery pump 8, 29-delivery pump 9, 30-delivery pump 10, 31-delivery pump 11, 32-delivery pump 12, 33-stirring paddle, 34-first circulation pipeline, 35-second circulation pipeline, 36- The third circulation pipeline. DETAILED DESCRIPTION

[0020] The technical scheme of the present invention will be clearly and completely described below in conjunction with specific embodiments, but it will be appreciated by those skilled in the art that the following described embodiments are part of embodiments of the present invention, rather than all embodiments, and are only used to illustrate the present invention, and should not be considered as limiting the scope of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work, all belong to the scope of protection of the present invention. If specific conditions are not indicated in the embodiments, they are carried out according to normal conditions or conditions recommended by the manufacturer. If the manufacturer is not indicated in the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0021] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.

[0022] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0023] In order to more clearly explain the technical solution of the present invention, it is described in the form of specific embodiments below.

[0024] Example 1 See also Figure 1 As shown, the device for the continuous and mild production of cyclohexene oxide without catalyst provided in the embodiment of the present invention includes 8-raw material premixer, 8-raw material premixer and can be directly connected to the raw material storage tank, and can also be mixed with the raw material storage tank through 9-liquid mixer 3. In this embodiment, water, cyclohexene and acetonitrile (as shown in Table 1) enter the 8-raw material premixer through 9-liquid mixer 3 for stirring, and tetrabutylammonium bromide directly enters the 8-raw material premixer to stir with the raw materials mixed in advance, and at the same time, the position of 33-stirring paddle in the 8-raw material premixer is located at 1 / 3 of the bottom of the 8-raw material premixer. Since the reaction raw materials will eventually gather at the bottom of the 8-raw material premixer due to the effect of gravity, the position of the 33-stirring paddle is set at a lower position to ensure that all raw materials are fully premixed before entering the 1-reaction tank, which is more convenient for the subsequent reaction.

[0025] The premixed raw materials are transported through 21-delivery pump 1, secondary mixed through 10-liquid mixer 1, and then enter 1-reaction tank through the mixing pipeline. At this time, the reaction temperature in 1-reaction tank is 15℃-30℃, and the reaction pressure varies between 0.8atm-2atm. A 2-liquid enhanced reactor is arranged on the top of 1-reaction tank, and a nozzle is arranged at the outlet of 2-liquid enhanced reactor. The nozzle can secondary mix the premixed micro droplets and spray them out in atomization, providing power for the reaction raw materials and accelerating the reaction process; at the same time, the 2-liquid enhanced reactor is arranged on the top and connected with 8-raw material premixer, which can play a secondary mixing role, and can increase the gas-liquid two-phase contact time from top to bottom, which can make the reaction more uniform, so the position of 2-liquid enhanced reaction device is fixed. A 3-gas enhanced reactor is arranged at the inner bottom of the 1-reaction tank, and a pipeline is arranged at the outer bottom of the 1-reaction tank, which is directly connected to the 3-gas enhanced reactor through the pipeline. At the same time, a 23-delivery pump 3 is arranged on the pipeline to pass air into the 3-gas enhanced reactor. After the air enters the 3-gas enhanced reactor, it is fully crushed and fully reacts with the atomized raw materials.

[0026] The fully reacted material is transported to the 4-flash tank through the 25-transfer pump 5. The 25-transfer pump 5 can provide power for the material and also defoam the material to facilitate the next step of the reaction process. The top of the 4-flash tank is provided with a pipeline connected to the middle of the side wall of the 5-product separation tower, and the pipeline is provided with a 26-transfer pump 6. The bottom of the 4-flash tank is provided with a pipeline, one end of which is connected to the bottom of the flash tank, and the other end is connected to the mixing pipeline through the 10-liquid mixer 1, and then re-enters the 1-reaction tank. The pipeline is connected to the 1-reaction tank and is provided with a 24-transfer pump 4 in the pipeline section before entering the 10-liquid mixer 1, which is used to provide power for the material. The above two pipelines form a 34-first circulation pipeline. When the material enters the 4-flash tank, the temperature inside the 4-flash tank varies between 100°C and 160°C, and the pressure varies between 0.5atm and 2atm. The 4-flash tank can quickly vaporize and separate the material, separating the vapor phase material and the liquid phase material. The separated vapor phase material is transported from the pipeline at the top of the 4-flash tank through the 26-delivery pump 6, and enters the 5-product separation tower through the middle of the 5-product separation tower; while the separated liquid phase material is transported from the bottom of the 4-flash tank through the 24-delivery pump 4 to the 10-liquid mixer 1 for mixing, and then re-enters the 1-reaction tank through the mixing pipeline for cyclic reaction. The 34-first circulation pipeline realizes the first circulation, which can continuously reflux the liquid phase material to the 1-reaction tank, and continuously react and utilize it.

[0027] When the vapor phase material enters the 5-product separation tower, the working pressure of the 5-product separation tower is 0.5 atm-1.5 atm, the reaction temperature is 55°C-105°C, the total number of plates is 26, and the reflux ratio is 5.5. A pipeline is provided on the top of the 5-product separation tower, on which are provided 18-condenser 1, 15-reflux tank 1 and 30-delivery pump 10, 18-condenser 1 and 15-reflux tank 1 are connected in parallel and then connected in series with 30-delivery pump 10, and then connected to the middle side wall of the 6-recovery tower through 30-delivery pump 10; 19-condenser 2, 16-reflux tank 2 and 31-delivery pump 11 are also provided on the top of the 6-recovery tower, 19-condenser 2 and 16-reflux tank 2 are connected in parallel, and then connected in series with 31-delivery pump 11, and enter 11-liquid mixer 2 through 31-delivery pump and then enter the collecting pipe, the collecting pipe enters 10-liquid mixer 1 through 22-delivery pump 2 and then is connected to 1-reaction tank to form 35-second circulation pipeline. The bottom of the 5-product separation tower is provided with a pipeline directly connected to the middle of the 7-product refining tower, and a 27-delivery pump 7 is provided on the pipeline, and a 12-reboiler 1 is provided at the bottom of the 5-product separation tower; the bottom of the 6-recovery tower is provided with a 28-delivery pump 8, and a 13-reboiler 2. In the arrangement of the present invention, the material inlets in the 5-product separation tower, the 6-recovery tower and the 7-product refining tower are all arranged in the middle of the tower body. The reason for such an arrangement is that the incoming materials can be quickly changed in the middle of the tower body and separated / recovered / refined, which can effectively improve the work efficiency on the one hand; at the same time, it can make good use of gravity and the properties of the reaction raw materials themselves to promote them to enter the next process, achieve environmental benefits and improve the safety of the reaction process.

[0028] The vapor phase material generated during the reaction enters the 5-product separation tower, and the 12-reboiler 1 provides heat for the 5-product separation tower, so that the 5-product separation tower separates the vapor phase material. After separation, the light components such as water and cyclohexene that have not been fully reacted are extracted from the top of the 5-separation tower, and are condensed and refluxed through the 18-condenser 1 and the 15-reflux tank 1 to become liquid again, and are powered by the 30-transfer pump 10 to enter the 6-recovery tower through the middle of the side wall of the 6-recovery tower. At this time, the temperature in the recovery tower is 120°C-230°C, the working pressure is 4.5atm-4.7atm, the total number of plates is 25, and the reflux ratio is 5. The 13-reboiler 2 at the bottom of the 6-recovery tower provides heat for it, and at the same time makes the temperature in the 6-recovery tower higher. On the one hand, the 6-recovery tower can recover the unreacted water or cyclohexene and other reaction raw materials. On the other hand, side reactions will occur during the reaction process, and the side reactions can generate high-purity cyclohexanone. The 6-recovery tower can transfer the high-purity cyclohexanone through the 28-transfer pump 8 at the bottom of the 6-reaction tower, thereby realizing the recovery of the high-purity by-product cyclohexanone. Since the temperature in the 6-recovery tower is relatively high, the unreacted raw materials that have been recovered may be vaporized for the second time. Therefore, 19-condenser 2 and 16-reflux tank 2 are set at the outlet of the top of the 6-recovery tower for secondary condensation and reflux to convert them into liquid materials, which are mixed again through 11-liquid mixer 2 and 10-liquid mixer 1, and re-enter 1-reaction tank through the mixing pipeline to repeat the first cycle and the above reaction process.

[0029] The mixture of water and cyclohexene oxide generated in the 5-product separation tower can enter the inlet located in the middle of the side wall of the 7-product refining tower from the bottom of the 5-product separation tower through the 27-delivery pump 7. At this time, the temperature in the product refining tower is 100°C-150°C, the reaction pressure is 0.5atm-1.5atm, the total number of tower plates is 30, and the reflux ratio is 5.3. The top of the 7-product refining tower is provided with an outlet, and a pipeline is provided at the outlet to connect the 20-condenser 3 and the 17-reflux tank 3 in parallel. The two are connected in series with the 32-delivery pump 12. After passing through the 32-delivery pump 12, the pipeline is connected to the 11-liquid mixer 2 and merged into the collecting pipe. The collecting pipe enters the 10-liquid mixer 1 through the 22-delivery pump 2, and enters the 1-reaction tank again through the mixing pipeline to form the 36-third circulation pipeline. The bottom of the 7-product refining tower is provided with a pipeline connected to the 29-delivery pump 9 for directly outputting the reaction product; and a 14-reboiler 3 is also provided. After the mixture of water and cyclohexene oxide separated by the 5-product separation tower enters the 7-product refining tower, the 14-reboiler 3 works to supply energy to the 7-product refining tower; the 7-product refining tower refines and separates the mixture of water and cyclohexene oxide to obtain water and cyclohexene oxide, and the dehydrated cyclohexene oxide is output through the 29-delivery pump 9 provided at the bottom of the 7-product refining tower, and the separated water enters the 20-condenser 3 and the 17-reflux tank 3 for condensation and reflux, and then enters the 11-liquid mixer 2 through the 32-delivery pump 12, and is fully mixed with the raw materials that have not been completely reacted in the second circulation process, and finally enters the 1-reaction tank again through the 36-third circulation pipeline for circulation.

[0030] After the reaction was completed, the yield and purity of the product cyclohexene oxide and the by-product cyclohexanone were measured. The measurement results are shown in Table 2.

[0031] In the present invention, a flow control valve is provided in each pipeline. In actual use, the flow control valve can be designed and installed according to actual needs. In the flash tank, product separation tower, product refining tower and recovery tower, the temperature of the tower top and the tower bottom are different due to the structure of the tower itself, and the temperature is not uniform during the reaction process. The operating conditions are shown in Table 3.

[0032] In the present invention, the materials generated during the reaction are fully recycled through the circulation pipeline, so as to realize the maximum utilization of the raw materials without catalyst; at the same time, the recovery tower can recycle the raw materials that are not fully reacted, and realize the recycling of high-purity by-products in the recovery tower, which not only avoids the by-products from entering the reaction again, but also can effectively improve the economic benefits. At the same time, through the setting of the condenser, reboiler, reflux tank, gas enhanced reactor and liquid enhanced reactor, the reaction can be operated at normal temperature and pressure, which greatly improves the safety.

[0033] Table 1: Raw material composition

[0034] Table 2: Yield and purity of products and by-products

[0035] Table 3: Operating conditions of each unit

[0036] Example 2 The specific implementation method is consistent with Example 1, except that the raw material premixer is not used.

[0037] Example 3 The specific implementation method is consistent with Example 1, and the stirring paddle is set at 1 / 2 of the distance from the bottom of the raw material premixer.

[0038] Example 4 The specific implementation method is consistent with Example 1, and the total number of plates is changed, as shown in Table 4:

[0039] Comparative Example 1 The specific connection method is consistent with that in Example 1, and only the gas enhancement reactor and the liquid enhancement reactor in the reaction tank are removed.

[0040] Comparative Example 2 The specific implementation method is consistent with Example 1, and the connection mode is changed, and the flash tank and the product separation tower, and the recovery tower and the product refining tower are connected in series in sequence.

[0041] Comparative Example 3 The specific implementation method is consistent with Example 1, and the first circulation pipeline is connected in parallel with the second circulation pipeline, and then connected in series with the third circulation pipeline after parallel connection.

[0042] Comparative Example 4 The specific implementation method is consistent with Example 1, and the liquid enhancement reactor is arranged on the side wall of the reaction tank.

[0043] Experimental Example 1 The yield and purity of the products and by-products of the above-mentioned embodiments and comparative examples are shown in Table 5.

[0044] Table 5: Yield and purity of products and by-products of Examples and Comparative Examples

[0045] It can be seen from the experimental data of the embodiments and comparative examples that by comparing embodiment 1 with comparative examples 2-3, it can be seen that the first circulation pipeline, the second circulation pipeline and the third circulation pipeline in the present invention are connected in parallel to fully utilize the unreacted raw materials, thereby increasing the output of the product cyclohexene oxide and the output of high-purity cyclohexanone, and increasing the purity of the products and by-products. The reason is that connecting the three circulation pipelines in parallel can not only avoid the mutual influence between the products, but also ensure that each circulation pipeline reacts independently, thereby ensuring the purity of the product; on the other hand, the three circulation pipelines can fundamentally ensure that the unreacted raw materials can be re-mixed and returned to the reaction tank for re-reaction, thereby improving the utilization rate of the raw materials.

[0046] It can be seen from the comparison between Example 1 and Comparative Example 1 that the output of the product and the high-purity by-product are increased. It can be seen that the enhanced reaction unit can effectively utilize the raw materials, thereby increasing the conversion efficiency, and is also conducive to improving the purity of the product and by-product. It can be seen from the comparison between Example 1 and Comparative Example 4 that when the liquid enhanced reactor is set at the top, the contact time of the gas-liquid two phases can be increased from top to bottom, and the gravity and the force during injection can be used to fully mix the materials; and when the liquid enhanced reactor is set on the side wall, it has little effect on the output, but it will reduce the reaction purity. The reason is that when it is set on the side wall, it may cause uneven distribution of raw materials and affect the reaction. It can be seen that when the position of the liquid enhanced reactor changes, the conversion efficiency of the product will be greatly reduced.

[0047] The experimental results of Example 4 show that when the total number of plates is set in a corresponding range, it has little effect on the reaction.

[0048] The experimental results of Example 3 show that when the raw material premixer is not used, the yield of the product will be slightly reduced, but its effect on the purity is not significant. The reason is that the raw material premixer can mix the raw materials in advance, thereby ensuring that the raw materials are fully reacted when entering the reaction tank; when the raw material premixer is not added, the sufficient degree of mixing of the raw materials when entering the reaction tank will be slightly reduced, thereby slightly reducing the yield.

[0049] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A device for continuously and gently producing cyclohexene oxide without catalyst, It is characterized in that It comprises a reaction tank, the inner top of which is provided with a liquid enhanced reactor, the liquid enhanced reactor is externally connected to a mixing pipeline, the mixing pipeline is formed by a first circulation pipeline, a second circulation pipeline and a third circulation pipeline being brought together through a liquid mixer 1, the first circulation pipeline is used for reaction; the second circulation pipeline is used for separation and recovery; the third circulation pipeline is used for refining, and the first circulation pipeline, the second circulation pipeline and the third circulation pipeline are connected in parallel.

2. The device for continuously and gently producing cyclohexene oxide without catalyst according to claim 1, It is characterized in that A gas intensification reactor is arranged at the inner bottom of the reaction tank, and the gas intensification reactor is directly connected to a gas delivery pump arranged at the bottom of the reaction tank; a pipeline is arranged on the side wall of the reaction tank to be connected to a flash tank, and a pipeline is arranged at the bottom of the flash tank to form a first circulation pipeline through the liquid mixer 1 and the mixing pipeline.

3. The device for continuously and gently producing cyclohexene oxide without catalyst according to claim 2, It is characterized in that The inlets of the first circulation pipeline and the second circulation pipeline are connected in parallel through a flash tank, a pipeline is provided on the top of the flash tank to connect with the middle part of the side wall of the product separation tower, a pipeline is provided on the top of the product separation tower to connect with the middle part of the side wall of the recovery tower, a pipeline is provided at the top outlet of the recovery tower to form a collecting pipe through a liquid mixer 2, and the collecting pipe is merged into the mixing pipeline through the liquid mixer 1 to form the second circulation pipeline; the product separation tower and the recovery tower are connected in series.

4. The device for continuously and gently producing cyclohexene oxide without catalyst according to claim 3, It is characterized in that The inlets of the second circulation pipeline and the third circulation pipeline are connected in parallel through the separation tower. A pipeline is provided at the bottom of the separation tower and connected to the middle of the side wall of the product refining tower. A pipeline is provided at the top outlet of the product refining tower to form a collecting pipe through a liquid mixer 2. The collecting pipe merges into the mixing pipeline through the liquid mixer 1 to form the third circulation pipeline.

5. The device for continuously and gently producing cyclohexene oxide without catalyst according to any one of claims 3 to 4, It is characterized in that The product separation tower, recovery tower and product refining tower are all equipped with a condenser, a reboiler and a reflux tank.

6. The device for continuously and gently producing cyclohexene oxide without catalyst according to claim 1, It is characterized in that The reaction device further comprises a raw material premixer, and the raw material premixer enters the mixing pipeline through the liquid mixer 1 and is connected to the reaction tank.

7. The device for continuously and gently producing cyclohexene oxide without catalyst according to claim 6, It is characterized in that The raw material premixer is directly connected to the raw material storage tank, and a stirring paddle is arranged inside the raw material premixer, and the stirring paddle is located at 1 / 3-1 / 2 of the distance from the bottom of the raw material premixer.

8. The device for continuously and gently producing cyclohexene oxide without catalyst according to claim 5, It is characterized in that The product separation tower, recovery tower and product refining tower are all provided with tower plates. The total number of tower plates of the product separation tower is 15-30; the total number of tower plates of the recovery tower is 15-35; and the total number of tower plates of the product refining tower is 20-40.

9. A method for reacting using the device for continuously and gently producing cyclohexene oxide without catalyst as claimed in any one of claims 1 to 8, It is characterized in that The steps include: Premixing the reactants and then reacting them; The obtained product is obtained through flash evaporation, cyclic separation, refinement and recovery.

10. A method for reacting the device for continuously and gently producing cyclohexene oxide without catalyst according to claim 9, It is characterized in that The reaction temperature of the reaction is 15°C-30°C, and the reaction pressure is 0.8 atm-2atm; The flash evaporation temperature is 100°C-160°C, and the flash evaporation pressure is 0.5atm-2atm; The separation temperature is 55°C-105°C, the separation pressure is 0.5 atm-1.5 atm, and the reflux ratio is 4.6-6; The refining temperature is 100°C-150°C, the refining pressure is 0.5atm-1.5atm, and the reflux ratio is 4.3-5.6; The recovery temperature is 120° C.-230° C., the recovery pressure is 4.5 atm-7 atm, and the reflux ratio is 4-8.