Secondary amine production device
By combining a vapor phase cooling tank, an outer flow guide sleeve, and an inner gas guide pipe, the problem of formaldehyde volatilization was solved, enabling the recovery and reuse of formaldehyde and the cascade utilization of waste heat, reducing production costs and environmental pollution, and improving energy efficiency.
Patent Information
- Application Number
- CN202520584486.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-31
- Publication Date
- 2026-02-27
- Estimated Expiration
- 2035-03-31
AI Technical Summary
In existing secondary amine production facilities, formaldehyde is easily volatilized, leading to raw material waste and environmental pollution. Insufficient energy utilization results in high production costs and fails to meet green and environmental protection requirements.
The system employs a combination of a gas phase cooling tank, an outer flow guide sleeve, an inner gas guide pipe, and a cooling jacket. The formaldehyde-containing gaseous substances generated in the reactor are collected through the inner gas guide pipe, and the formaldehyde is liquefied and recovered and the waste heat is reused by using the temperature control jacket and the cooling jacket.
It enables the recycling and reuse of formaldehyde, reduces production costs, reduces environmental pollution, and improves energy efficiency, meeting the requirements for energy conservation and emission reduction.
Smart Images
Figure CN223945643U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the technical field of secondary amine production, in particular to secondary amine production device. BACKGROUND
[0002] Secondary amine is an important class of organic compounds, which has a wide range of applications in chemical industry, medicine, materials and many other fields. The liquid phase secondary amine produced by the device is a key intermediate in fine chemical production and participates in many chemical reactions. However, there are some prominent problems in the existing secondary amine production device.
[0003] On the one hand, formaldehyde, as a key raw material in the production process of secondary amine, is extremely volatile in the reaction environment of the existing device. The volatilization of formaldehyde not only causes waste of raw materials and increases production cost, but also is toxic, which can harm the health of operators and pollute the surrounding environment, which is not in line with the concept of green and environmental protection. For example, in the traditional reaction kettle, due to the inaccurate control of reaction temperature and pressure, the unreasonable stirring mode and intensity in the reaction process, formaldehyde cannot fully participate in the reaction and a large amount of formaldehyde is volatilized and escaped.
[0004] On the other hand, the existing device has some deficiencies in energy utilization. In the whole production process, a large amount of waste heat is generated in the reaction process, and a large amount of energy is consumed in the cooling of the reaction system by the refrigeration system, but these energy is not fully recovered and reused. The high-temperature gas discharged from the reaction kettle is directly discharged into the atmosphere, taking away a large amount of heat; the low-temperature medium cooled by the refrigeration system is also directly discharged, causing waste of cold energy. This not only leads to increased energy consumption and high production cost, but also does not meet the requirements of sustainable development of energy saving and emission reduction. SUMMARY
[0005] In view of the above deficiencies in the prior art, the utility model aims to provide a secondary amine production device, which effectively solves the problem of excessive volatilization of formaldehyde by using a combination of a gas phase cooling tank, an outer flow guide sleeve, an inner gas guide pipeline and a cooling sleeve. In the reaction process, the gas phase material containing formaldehyde generated by the reaction kettle enters the gas phase cooling tank through the inner gas guide pipeline. The outer flow guide sleeve on the outside of the inner gas guide pipeline is in communication with the gas phase cooling tank, and a liquid storage tank is connected to the outer flow guide sleeve, which further optimizes the gas flow path and material collection path. The cooling sleeve on the outside of the gas phase cooling tank can reduce the temperature in the gas phase cooling tank, so that the formaldehyde contained in the gas phase is liquefied. The liquefied formaldehyde can be collected to the liquid storage tank through the pipeline, and then connected to the formaldehyde inlet pipeline through the pipeline, realizing the recycling of formaldehyde, which not only reduces the production cost, but also reduces the pollution to the environment.
[0006] The utility model is implemented by using the following technical solutions:
[0007] The secondary amine production device comprises a reaction kettle, a pre-heating kettle, a mixing tank, an extraction tower, a drying tower, a distillation tower, a filter, a stirring motor-driven stirring paddle, a dropwise metering device, and a disperser.
[0008] The pre-heating kettle is internally provided with a stirring device to stir and mix the added materials to make them evenly heated.
[0009] The pre-heating kettle is internally provided with a stirring device, and the stirring device is externally provided with a pre-heating kettle coil pipe.
[0010] The pre-heating kettle is connected with the disperser through a production pump, the dropwise metering device is connected with a formaldehyde inlet pipe, and the reaction kettle is externally provided with a temperature control sleeve.
[0011] The reaction kettle is connected with the gas-phase cooling tank through an internal gas guiding pipe, and the internal gas guiding pipe is externally provided with an external flow guiding sleeve.
[0012] The reaction kettle is internally provided with a stirring paddle driven by a stirring motor to fully mix the materials and formaldehyde, accelerate the reaction speed, and improve the reaction efficiency.
[0013] The internal gas guiding pipe extends into the gas-phase cooling tank by a length of 1 / 3 of the height of the gas-phase cooling tank.
[0014] The gas-phase cooling tank is externally provided with a cooling sleeve, and the temperature control sleeve is connected with the cooling sleeve through a connecting pipe.
[0015] The outer flow guide sleeve is connected with a liquid storage tank, and the liquid storage tank is connected with the formaldehyde inlet pipeline through a pipeline.
[0016] The working principle of the utility model is:
[0017] Material preparation stage: the raw materials (except formaldehyde) participating in the production reaction of secondary amine are added into the pre-heating kettle according to a certain proportion. The stirring device inside the pre-heating kettle starts to work to stir and mix the materials, so that the materials are uniformly heated. At the same time, the pre-heating kettle coil is opened, and the materials are pre-heated by using the residual heat transferred from the temperature control coil of the reaction kettle, so that the temperature of the materials is raised to a certain range (30-40 DEG C), so as to accelerate the subsequent reaction speed, reduce the reaction time, and improve the production efficiency.
[0018] Reaction stage: the materials in the pre-heating kettle are transported to the disperser in the reaction kettle through the production pump. The disperser uniformly disperses the materials, increases the contact area of the materials and the subsequently added formaldehyde, and promotes the reaction. The formaldehyde is slowly added into the reaction kettle through the formaldehyde inlet pipeline by the dropwise metering device, and the dropwise adding speed is accurately controlled according to the reaction progress and reaction conditions (a certain volume of formaldehyde solution is added every minute). The stirring paddle is opened, and under the driving of the stirring motor, the stirring paddle rotates at high speed, so that the materials and the formaldehyde are fully mixed, and the reaction is accelerated. At the same time, the temperature control coil and the temperature control sleeve are opened, the temperature in the reaction kettle is controlled at the appropriate reaction temperature (60-80 DEG C), and the stable reaction pressure (0.5-1.0 MPa) is maintained, so that the reaction is efficiently carried out.
[0019] Product separation and refining stage: after the reaction is completed, the reaction product enters the mixing tank through the connecting pipeline, and is fully mixed with a specific extractant in the mixing tank to realize the preliminary separation of the product and impurities. Then, the mixed liquid enters the extraction tower for extraction operation to further separate the product and impurities. The product from the extraction tower enters the drying tower, and the product is dried by the drying medium (such as silica gel, molecular sieve, etc.) in the drying tower to remove the water in the product. The dried product is filtered through the filter to remove possible solid impurities, and then enters the distillation tower for distillation operation. In the distillation tower, by controlling different temperature and pressure conditions (the temperature at the bottom of the distillation tower is 100-120 DEG C, and the pressure at the top of the tower is 0.1-0.3 MPa), the target product secondary amine is separated from other substances with different boiling points, and the high-purity liquid-phase secondary amine product is obtained.
[0020] The gas phase treatment and energy recovery stage: the gas phase material containing formaldehyde generated in the reaction process enters the gas phase cooling tank through the inner gas guide pipeline, the inner gas guide pipeline extends into the inside of the gas phase cooling tank by 1 / 3 of the height of the gas phase cooling tank, so that the gas phase material can be fully contacted with the low-temperature environment in the gas phase cooling tank, the cooling jacket outside the gas phase cooling tank is connected with the refrigerant from the temperature control jacket of the reaction kettle, the refrigerant absorbs the heat of the gas phase material in the gas phase cooling tank, so that the formaldehyde in the gas phase is liquefied, the liquefied formaldehyde flows into the outer guide sleeve and enters the liquid storage tank through the pipeline connected to the outer guide sleeve, and then can be used for the reaction again, at the same time, the gas not liquefied in the gas phase cooling tank is treated and discharged up to the standard, so as to avoid pollution to the environment.
[0021] Compared with the prior art, the utility model has the advantages that:
[0022] (1) the utility model discloses a gas phase cooling tank, outer guide sleeve, inner gas guide pipeline and cooling jacket are used in combination, effectively solve the problem of formaldehyde volatilization, in the reaction process, the gas phase material containing formaldehyde generated in the reaction kettle enters the gas phase cooling tank through the inner gas guide pipeline, the outer guide sleeve outside the inner gas guide pipeline is connected with the gas phase cooling tank, and the outer guide sleeve is connected with the liquid storage tank, and the gas flow and the material collection path are further optimized, the cooling jacket outside the gas phase cooling tank can reduce the temperature in the gas phase cooling tank, so that the formaldehyde contained in the gas phase is liquefied, the liquefied formaldehyde can be collected to the liquid storage tank through the pipeline, and then the pipeline is connected with the formaldehyde inlet pipeline, the formaldehyde is recycled and reused, the production cost is reduced, and the pollution to the environment is reduced.
[0023] (2) the device utilizes the cold energy of the refrigerant again through the temperature control jacket and the cooling jacket, the temperature control jacket is wrapped outside the reaction kettle, adjusts the temperature of the reaction kettle, and after the refrigerant in the temperature control jacket absorbs the heat of the reaction kettle and heats up, the refrigerant enters the cooling jacket outside the gas phase cooling tank through the connecting pipeline, cools the gas phase cooling tank, realizes the cascade utilization of the cold energy, and utilizes the waste heat through the temperature control coil and the preheating kettle coil, the temperature control coil outside the stirring paddle in the reaction kettle absorbs the waste heat generated in the reaction, the heat is transmitted to the preheating kettle coil through the pipeline, the material in the preheating kettle is preheated, the energy consumption in the preheating process is reduced, the energy utilization rate is improved, the production cost is reduced, and the requirements of energy saving and emission reduction are met. BRIEF DESCRIPTION OF DRAWINGS
[0024] Figure 1 It is the structure schematic view of the secondary amine production device of the utility model;
[0025] In the figure: 1, reaction kettle; 2, pre-heating kettle; 3, mixing tank; 4, extraction tower; 5, drying tower; 6, filter; 7, distillation tower; 8, disperser; 9, dropwise metering device; 10, stirring paddle; 11, temperature control coil; 12, formaldehyde inlet pipeline; 13, gas phase cooling tank; 14, outer guide sleeve; 15, inner gas guide pipeline; 16, cooling jacket; 17, liquid storage tank; 18, temperature control sleeve; 19, pre-heating kettle coil; 20, connecting pipeline. DETAILED DESCRIPTION
[0026] In order to make the utility model purposes, technical scheme more clearly, below, combining with the drawing, to the utility model make further detailed description.
[0027] Example 1
[0028] As Figure 1 shown, the secondary amine production device, including reaction kettle 1, pre-heating kettle 2, pre-heating kettle 2 is connected with reaction kettle 1 by production pump, reaction kettle 1 is connected with extraction tower 4 by mixing tank 3, extraction tower 4 is connected with distillation tower 7 by drying tower 5, and filter 6 is arranged between drying tower 5 and distillation tower 7, the inside of reaction kettle 1 is equipped with the stirring paddle 10 driven by stirring motor, the upper portion of stirring paddle 10 is equipped with dropwise metering device 9, and the lower portion of stirring paddle 10 is equipped with disperser 8.Mixing tank 3 is used to mix reaction product and extractant fully, so that product and impurities are preliminarily separated.Its structural design is beneficial to the full contact and mixing of materials, lays the foundation for the efficient extraction operation of subsequent extraction tower.Extraction tower 4 can further separate product and impurities by specific extraction process and internal structural design (filler layer, tray), and the purity of product is improved.The efficient separation of extraction tower 4 ensures the quality of subsequent product.The outer side of stirring paddle 10 is equipped with temperature control coil 11, the inside of pre-heating kettle 2 is equipped with stirring device, the outer side of stirring device is equipped with pre-heating kettle coil 19, and temperature control coil 11 is connected with pre-heating kettle coil 19 by pipeline.Pre-heating kettle 2 is connected with disperser 8 by production pump, formaldehyde inlet pipeline 12 is connected on dropwise metering device 9, and the outer side of reaction kettle 1 is equipped with temperature control sleeve 18.Reaction kettle 1 is connected with gas phase cooling tank 13 by inner gas guide pipeline 15, the outer side of inner gas guide pipeline 15 is equipped with outer guide sleeve 14, and outer guide sleeve 14 is communicated with gas phase cooling tank 13.Inner gas guide pipeline 15 extends into the inside of gas phase cooling tank 13, and the extension length is 1 / 3 of the height of gas phase cooling tank 13.The outer side of gas phase cooling tank 13 is equipped with cooling jacket 16, and temperature control sleeve 18 is connected with cooling jacket 16 by connecting pipeline 20.Liquid storage tank 17 is connected on outer guide sleeve 14, and the liquid storage tank 17 is connected with formaldehyde inlet pipeline 12 by pipeline.
[0029] The secondary amine production device, when working, includes the following steps:
[0030] (1) The raw materials participating in the production of secondary amine reaction are added to the pre-heating kettle 2 according to a certain proportion. The stirring device inside the pre-heating kettle 2 starts to work to stir and mix the materials to make them evenly heated. At the same time, the pre-heating kettle coil 19 is opened, and the residual heat transferred from the temperature control coil 11 of the reaction kettle 1 is used to pre-heat the materials.(2) The materials in the pre-heating kettle 2 are transported to the disperser 8 in the reaction kettle 1 through the production pump. The disperser 8 uniformly disperses the materials, increases the contact area of the materials with the subsequent drop of formaldehyde, and promotes the reaction. Formaldehyde is slowly dropped into the reaction kettle 1 through the formaldehyde inlet pipeline 12 by the drop meter 9, and the drop speed is accurately controlled according to the reaction progress and reaction conditions (for example, a certain volume of formaldehyde solution is dropped per minute). The stirring paddle 10 is opened, and under the drive of the stirring motor, the stirring paddle 10 rotates at high speed to make the materials and formaldehyde fully mixed and accelerate the reaction. At the same time, the temperature control coil 11 and the temperature control sleeve 18 are opened.(3) After the reaction is completed, the reaction product enters the mixing tank 3 through the connecting pipeline, and is fully mixed with a specific extractant in the mixing tank 3 to achieve the preliminary separation of the product and impurities. Then, the mixed solution enters the extraction tower 4 for extraction operation to further separate the product and impurities. The product from the extraction tower 4 enters the drying tower 5, and the product is dried by the drying medium in the drying tower 5 to remove the water in it. The dried product is filtered through the filter 6 to remove possible solid impurities, and then enters the distillation tower 7 for distillation operation. In the distillation tower 7, by controlling different temperature and pressure conditions, the target product secondary amine is separated from other substances with different boiling points to obtain high-purity liquid-phase secondary amine product.(4) The gas-phase substances containing formaldehyde generated during the reaction enter the gas-phase cooling tank 13 through the inner gas guiding pipeline 15. The inner gas guiding pipeline 15 extends into the gas-phase cooling tank 13 to a length of 1 / 3 of the height of the gas-phase cooling tank 13, so that the gas-phase substances can fully contact with the low-temperature environment in the gas-phase cooling tank 13. The cooling sleeve 16 outside the gas-phase cooling tank 13 is connected to the refrigerant from the temperature control sleeve 18 of the reaction kettle 1, which absorbs the heat of the gas-phase substances in the gas-phase cooling tank 13 to liquefy the formaldehyde in the gas phase. The liquefied formaldehyde flows into the outer guiding sleeve 14 and enters the storage tank 17 through the pipeline connected to the outer guiding sleeve 14 for storage, and then can be used for reaction again. At the same time, the gas in the gas-phase cooling tank 13 that has not been liquefied is treated and discharged up to standard to avoid pollution to the environment.
Claims
1. A secondary amine production apparatus, characterized in that, The reactor includes a reaction vessel (1) and a preheating vessel (2). The preheating vessel (2) is connected to the reaction vessel (1) via a production pump. The reaction vessel (1) is connected to the extraction tower (4) via a mixing tank (3). The extraction tower (4) is connected to the distillation tower (7) via a drying tower (5). A filter (6) is provided between the drying tower (5) and the distillation tower (7). The reactor (1) is equipped with a stirring paddle (10) driven by a stirring motor. A dropping meter (9) is provided above the stirring paddle (10), and a disperser (8) is provided below the stirring paddle (10).
2. The secondary amine production apparatus according to claim 1, characterized in that, The stirring paddle (10) is provided with a temperature control coil (11) on the outside, and the preheating kettle (2) is provided with a stirring device inside. The stirring device is provided with a preheating kettle coil (19) on the outside. The temperature control coil (11) is connected to the preheating kettle coil (19) through a pipe.
3. The secondary amine production apparatus according to claim 1, characterized in that, The preheating kettle (2) is connected to the disperser (8) via a production pump. A formaldehyde inlet pipe (12) is connected to the drip meter (9). A temperature control sleeve (18) is provided on the outside of the reaction kettle (1).
4. The secondary amine production apparatus according to claim 3, characterized in that, The reactor (1) is connected to the gas phase cooling tank (13) through an inner gas guide pipe (15). An outer guide sleeve (14) is provided on the outside of the inner gas guide pipe (15), and the outer guide sleeve (14) is connected to the gas phase cooling tank (13).
5. The secondary amine production apparatus according to claim 4, characterized in that, The internal air guide pipe (15) extends into the vapor phase cooling tank (13) and the length of the extension is 1 / 3 of the height of the vapor phase cooling tank (13).
6. The secondary amine production apparatus according to claim 5, characterized in that, The outer side of the vapor phase cooling tank (13) is provided with a cooling sleeve (16), and the temperature control sleeve (18) is connected to the cooling sleeve (16) through a connecting pipe (20).
7. The secondary amine production apparatus according to claim 4, characterized in that, The outer guide sleeve (14) is connected to a liquid storage tank (17), which is connected to the formaldehyde inlet pipe (12) through a pipe.