Device for directly recycling piperidine from wastewater
By performing stand-alone layered extraction in wastewater, the problem of piperidine remaining in wastewater is solved, low-cost and efficient piperidine recovery is achieved, production and treatment costs are reduced, and the operation process is simplified.
Patent Information
- Application Number
- CN202420044300.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-01-09
- Publication Date
- 2025-01-07
- Estimated Expiration
- 2034-01-09
AI Technical Summary
In the prior art, piperidine remains in the wastewater in the form of an acid salt, wastes catalysts, increases production costs and increases the difficulty of wastewater treatment, and the distillation and recycling method consumes high energy and has a large investment.
A device for recycling piperidine from wastewater was designed. Through the recycling kettle and the metering tank, the wastewater, neutralizing agent and extraction agent were input, and the static layered extraction was performed, which avoided the high energy consumption and high investment in distillation, and achieved Effective recovery of low content of piperidine.
It reduces production costs and wastewater treatment costs, improves product yields, is simple to operate, and avoids high operating costs and complex recycling processes.
Smart Images
Figure CN222312779U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the field of fine chemicals, in particular to a device for recovering piperidine from waste water for direct application. Background Art
[0002] In the process of synthesizing the pesticide intermediate ethylthiopropyltrione (also known as propionyltrione), the intermediate 6-ethylthio-3-heptene-2-one (hereinafter referred to as heptene ketone) must be synthesized first. When synthesizing heptene ketone, an aqueous solution of sodium acetoacetate reacts with thioetheraldehyde under the action of a catalyst, wherein the catalyst is a piperidine solution of acetic acid, a piperidine solution of hydrochloric acid or a piperidine solution of sulfuric acid. The acidic piperidine salts in the wastewater are all treated in the wastewater treatment station. A patent describes adding acid (sulfuric acid, hydrochloric acid) to piperidine and N,N-dimethylformamide in the wastewater to form an acid salt; centrifugation separation is performed by a centrifugal device; the obtained piperidine salt is added with a base and an extractant (methyl tert-butyl ether, cyclohexane, isopropyl ether, n-hexane, etc.), and the piperidine is extracted and then distilled and purified. Piperidine can also be recovered by distillation directly from the neutralized wastewater.
[0003] In the prior art, piperidine remains in the waste water in the form of acid salt, which wastes the catalyst piperidine, thereby increasing production costs and increasing the difficulty of sewage treatment. If the piperidine in the waste water is purified and reused by various means, the operation is difficult and the operating cost is also very high. If it is recovered by distillation, because the content in the waste water is very low (about 0.18%), the energy consumption is very large, and the investment in building a distillation tower is relatively high. Utility Model Content
[0004] Therefore, it is necessary to provide a device for recovering piperidine from wastewater for direct application, so as to solve the problem in the prior art that piperidine remains in the wastewater in the form of acid salt, which wastes the catalyst piperidine, thereby increasing production costs and increasing the difficulty of sewage treatment.
[0005] To achieve the above object, the utility model provides a device for recovering piperidine from wastewater for direct application, comprising:
[0006] A recovery kettle, the recovery kettle comprising an inner chamber and a first recovery input port, a second recovery input port, a third recovery input port and a recovery output port connected to the inner chamber;
[0007] A first metering tank, the first metering tank comprising a first metering input port and a first metering output port, the first metering input port is used to input wastewater, and the first metering output port is connected to the first recovery input port;
[0008] A second metering tank, the second metering tank comprising a second metering input port and a second metering output port, the second metering input port is used to input a neutralizing agent, and the second metering output port is connected to the second recovery input port;
[0009] The third metering tank comprises a third metering input port and a third metering output port. The third metering input port is used to input the extractant, and the third metering output port is connected with the third recovery input port.
[0010] Different from the prior art, the above technical scheme is to set a recovery kettle to be connected with the first metering tank, the second metering tank and the third metering tank respectively, and to input wastewater, a neutralizing agent and an extractant into the recovery kettle through the first metering tank, the second metering tank and the third metering tank respectively, to perform static stratification after being evenly mixed, and finally to discharge the alkaline wastewater and the piperidine extractant mixed solution respectively through the output port of the recovery kettle, so as to realize the extraction of low-content piperidine in the wastewater, avoid the high energy consumption and high investment of the distillation method for recovery, and at the same time, the piperidine solution recovered by the device can be used directly, avoiding the cumbersome operation and high operation cost of recovering piperidine by other means.
[0011] Furthermore, a stirring mechanism is included, and the stirring mechanism is arranged in the recovery kettle and is used to stir the solution in the inner chamber.
[0012] Furthermore, the recovery kettle also includes a temperature control chamber and a steam input port and a condensate output port communicated with the temperature control chamber, and the temperature control chamber is arranged between the outer wall of the recovery kettle and the inner chamber.
[0013] Furthermore, a pH meter is included, which is arranged on the recovery kettle and is used to detect the pH value of the solution in the inner chamber.
[0014] Furthermore, a thermometer is included, which is arranged on the recovery kettle and is used to detect the temperature of the solution in the inner chamber.
[0015] Furthermore, a viewing mirror is included, and the viewing mirror is arranged at the rear end of the output port.
[0016] Furthermore, a branch valve is included, and the branch valve is arranged at the rear end of the output port.
[0017] Furthermore, the first metering tank, the second metering tank and the third metering tank are all arranged above the recovery kettle.
[0018] Furthermore, the first recovery input port, the second recovery input port and the third recovery input port are all arranged at the top of the recovery kettle; and the output port is arranged at the bottom of the recovery kettle.
[0019] Furthermore, a vent valve is included, and the recovery kettle, the first metering tank, the second metering tank and the third metering tank are all provided with the vent valve.
[0020] Through the above technical solutions, the present invention can achieve the following beneficial effects:
[0021] (1) Reduced raw material consumption reduces production costs.
[0022] (2) Reduce the cost of wastewater treatment.
[0023] (3) Increased product yield (the intermediate has a certain solubility in wastewater).
[0024] (4) Simple and convenient operation. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 It is a structural schematic diagram of the device described in the specific implementation mode;
[0026] Figure 2 It is a structural schematic diagram of a device provided with a stirring mechanism according to a specific embodiment;
[0027] Figure 3 The device described in the specific implementation manner is provided with a temperature control chamber, a steam input port, and a condensate output port.
[0028] Figure 4 The device described in the specific implementation manner is provided with a pH meter, a thermometer and a sight glass;
[0029] Figure 5 This is a structural schematic diagram of a device provided with a bypass valve according to a specific implementation method;
[0030] Figure 6 It is a structural schematic diagram of a specific implementation method in which the device is provided with a vent valve.
[0031] Description of reference numerals:
[0032] 10. Recovery kettle;
[0033] 101, first recycling input port; 102, second recycling input port; 103, third recycling input port; 104, recycling output port; 105, inner chamber;
[0034] 20. The first metering tank;
[0035] 201, first metering input port; 202, first metering output port;
[0036] 30. Second metering tank;
[0037] 301, second metering input port; 302, second metering output port;
[0038] 40. The third measuring tank;
[0039] 401, third metering input port; 402, third metering output port;
[0040] 50. Stirring mechanism;
[0041] 60. Temperature control chamber;
[0042] 601, steam input port; 602, condensate output port;
[0043] 70. pH meter; 71. Thermometer; 72. Sight glass; 73. Branch valve; 80. Vent valve. DETAILED DESCRIPTION
[0044] In order to explain the technical content, structural features, achieved objectives and effects of the technical solution in detail, the following is a detailed description in conjunction with specific embodiments and accompanying drawings.
[0045] Reference to "embodiment" herein means that the specific features, structures or characteristics described in conjunction with the embodiment may be included in at least one embodiment of the present application. The term "embodiment" appearing in various places in the specification does not necessarily refer to the same embodiment, nor does it particularly limit its independence or association with other embodiments. In principle, in the present application, as long as there is no technical contradiction or conflict, the various technical features mentioned in the embodiments can be combined in any way to form a corresponding implementable technical solution.
[0046] Unless otherwise defined, the technical terms used in this document have the same meanings as those generally understood by those skilled in the art to which this application belongs; the use of relevant terms in this document is only for describing specific embodiments and is not intended to limit this application.
[0047] In the description of this application, the term "and / or" is used to describe the logical relationship between objects, indicating that three relationships may exist, for example, A and / or B, which means: A exists, B exists, and A and B exist at the same time. In addition, the character " / " in this article generally indicates that the objects before and after are in a logical relationship of "or".
[0048] In the present application, terms such as “first” and “second” are merely used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship of quantity, priority or sequence between these entities or operations.
[0049] Without further limitations, in this application, the words "include", "comprises", "has" or other similar expressions used in the sentences are intended to cover non-exclusive inclusion. These expressions do not exclude the presence of additional elements in the process, method or product including the elements, so that the process, method or product including a series of elements may include not only those limited elements, but also other elements not explicitly listed, or also include elements inherent to such process, method or product.
[0050] Similar to the understanding in the Examination Guidelines, in this application, expressions such as "greater than", "less than", "exceed" and the like are understood to exclude the number itself; expressions such as "above", "below", "within" and the like are understood to include the number itself. In addition, in the description of the embodiments of this application, "multiple" means more than two (including two), and similar expressions related to "multiple" are also understood in this way, such as "multiple groups", "multiple times", etc., unless otherwise clearly and specifically limited.
[0051] In the description of the embodiments of the present application, space-related expressions used, such as "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "vertical", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicate the orientation or position relationship based on the orientation or position relationship shown in the specific embodiments or drawings, and are only for the convenience of describing the specific embodiments of the present application or facilitating the reader's understanding, and do not indicate or imply that the referred device or component must have a specific position, a specific orientation, or be constructed or operated in a specific orientation, and therefore cannot be understood as a limitation on the embodiments of the present application.
[0052] Unless otherwise expressly specified or limited, in the description of the embodiments of the present application, the terms such as "install", "connect", "connect", "fix", "set", etc. used should be understood in a broad sense. For example, the "connection" can be a fixed connection, a detachable connection, or an integrated setting; it can be a mechanical connection, an electrical connection, or a communication connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium; it can be the internal connection of two elements or the interaction relationship between two elements. For technicians in the technical field to which the present application belongs, the specific meanings of the above terms in the embodiments of the present application can be understood according to the specific circumstances.
[0053] It should be noted that the connection described below specifically refers to the realization of a passage through the sealed connection between the two ends of the pipe fitting and the two interfaces. The pipe fittings can refer to the relevant materials used for fluid transportation in the prior art, and the common ones are metal pipes, such as cast iron pipes, seamed steel pipes, copper pipes, aluminum pipes, lead pipes; or non-metal pipes, such as plastic pipes, glass pipes, ceramic pipes, cement pipes; in addition, hoses, such as metal hoses, canvas hoses, etc., can also be used when necessary. The new model also involves temperature control, and insulation measures can be implemented on the pipe fittings as needed, such as using insulation materials with low heat transfer coefficients for outer coating, or applying insulation coatings on the outer layer of the pipe fittings.
[0054] See also Figures 1 to 6 This embodiment provides a device for recovering piperidine from wastewater for direct application, comprising:
[0055] The recovery kettle 10 includes an inner chamber 105 and a first recovery input port 101, a second recovery input port 102, a third recovery input port 103 and a recovery output port 104 connected to the inner chamber 105;
[0056] A first metering tank 20, wherein the first metering tank 20 comprises a first metering input port 201 and a first metering output port 202, wherein the first metering input port 201 is used to input wastewater, and the first metering output port 202 is connected to the first recovery input port 101;
[0057] The second metering tank 30 includes a second metering input port 301 and a second metering output port 302. The second metering input port 301 is used to input a neutralizing agent, and the second metering output port 302 is connected to the second recovery input port 102. The neutralizing agent can be selected from one or more of lime water, sodium carbonate, flake caustic soda, and liquid caustic soda.
[0058] The third metering tank 40 includes a third metering input port 401 and a third metering output port 402. The third metering input port 401 is used to input an extractant, and the third metering output port 402 is connected to the third recovery input port 103. The extractant can be selected from one or more of dichloromethane, dichloroethane, petroleum ether, benzene, toluene, etc.
[0059] The recovery kettle 10 is mainly composed of an inner chamber 105 and four interfaces, including a first recovery input port 101, a second recovery input port 102, a third recovery input port 103 and a recovery output port 104. The inner chamber 105 of the recovery kettle 10 can be made of high-quality stainless steel material to ensure that the part in contact with the liquid has good corrosion resistance and high temperature resistance. The first recovery input port 101, the second recovery input port 102, the third recovery input port 103 and the recovery output port 104 are all tightly closed movable interfaces to ensure that there is no leakage during operation. Preferably, the first metering tank 20, the second metering tank 30 and the third metering tank 40 are all arranged above the recovery kettle 10, which is convenient for conveying wastewater, neutralizer and extractant by gravity, and has a simple structure and is easy to use.
[0060] The first metering tank 20, the second metering tank 30 and the third metering tank 40. Each metering tank has an input port and an output port. The metering tank can be made of corrosion-resistant plastic or stainless steel material to ensure that the part in contact with the liquid has good corrosion resistance and high temperature resistance. Preferably, the first recovery input port 101, the second recovery input port 102 and the third recovery input port 103 are all arranged at the top of the recovery kettle 10; the output port is arranged at the bottom of the recovery kettle 10, which is convenient for adding wastewater, neutralizer and extractant from the top of the inner chamber 105, and discharging the alkaline wastewater and piperidine extractant mixture in sequence at the bottom of the inner chamber 105, which is reasonably arranged and simple in structure.
[0061] The working principle of this embodiment is as follows: first, a certain mass of wastewater (containing about 0.18% piperidine) is added to the first metering tank 20 through the first metering input port 201, a certain mass of neutralizer is added to the second metering tank 30 through the second metering input port 301, and a certain mass of extractant is added to the third metering tank 40 through the third metering input port 401. After completing the above steps, the wastewater, the neutralizer and the extractant are metered in sequence and added to the recovery kettle 10 through the first recovery input port 101, the second recovery input port 102 and the third recovery input port 103 for mixing. After the mixing is completed, it is allowed to stand for a period of time, and the mixed solution is stratified. The solution is discharged through the output port according to the stratification, wherein the alkaline wastewater can be used to neutralize other acidic wastewater, and the piperidine extracted mixed solution can be directly reused as an auxiliary material in production.
[0062] The novel device is provided with a recovery kettle 10 which is connected with a first metering tank 20, a second metering tank 30 and a third metering tank 40 respectively, and wastewater, a neutralizing agent and an extracting agent are respectively input into the recovery kettle 10 through the first metering tank 20, the second metering tank 30 and the third metering tank 40, and the mixture is allowed to stand for stratification after being evenly mixed, and finally the alkaline wastewater and the piperidine extracting agent mixed solution are respectively discharged through the output port of the recovery kettle 10, so as to realize the extraction of low-content piperidine in the wastewater, avoid the high energy consumption and high investment of the distillation method for recovery, and at the same time, the piperidine solution recovered by the device can be used directly, avoiding the cumbersome operation and high operation cost of recovering piperidine by other means.
[0063] In order to make the mixing of wastewater, neutralizer and extractant more uniform and improve the mixing efficiency, in some embodiments, a stirring mechanism 50 is also included. The stirring mechanism 50 is arranged in the recovery kettle 10 and is used to stir the solution in the inner chamber 105. The stirring method of the stirring mechanism 50 can be anchor type, frame type, ultrasonic type, etc. Specifically, the anchor stirring mechanism 50 includes an anchor-shaped agitator and a motor. The anchor-shaped agitator consists of a central axis and several anchor-shaped blades and can rotate along the central axis. The motor drives the rotating central axis to make the anchor-shaped blades stir the solution in the inner chamber 105. The main advantage of the anchor stirring mechanism 50 is that it can effectively mix the solution and avoid local dead corners, thereby improving the stirring efficiency and extraction rate; the frame stirring mechanism 50 includes a fixed frame and a movable agitator. The movable agitator consists of a motor and several stirring blades and can move along the fixed frame. The motor drives the stirring blades to rotate, and the movable agitator moves along the fixed frame at the same time, thereby stirring the solution in the inner chamber 105. The main advantage of the frame stirring mechanism 50 is that it can adapt to inner chambers 105 of different capacities, provide uniform stirring effect, and control the stirring efficiency by adjusting the speed and moving path of the agitator; the ultrasonic stirring mechanism 50 includes an ultrasonic generator and an ultrasonic probe. The ultrasonic generator generates high-frequency vibrations, and the ultrasonic probe transmits the high-frequency vibrations to the solution in the inner chamber 105. The high-frequency vibrations will form a large number of tiny bubbles in the liquid, and these bubbles will burst in an instant, generating a huge energy release, thereby achieving the stirring and mixing of the liquid. The main advantage of the ultrasonic stirring mechanism 50 is that it can quickly mix the liquid, improve the stirring efficiency, and maintain the quality and purity of the liquid. The above three stirring mechanism 50 embodiments can all achieve stirring the solution in the inner chamber 105 and improve the extraction rate of piperidine. Which stirring method is specifically adopted depends on the actual needs in different situations.
[0064] In order to control the temperature of the inner chamber 105 of the recovery kettle 10 so as to maintain a high extraction efficiency, in some embodiments, the recovery kettle 10 further includes a temperature control chamber 60 and a steam input port 601 and a condensate output port 602 connected to the temperature control chamber 60, and the temperature control chamber 60 is arranged between the outer wall of the recovery kettle 10 and the inner chamber 105. The temperature control chamber 60 can be an annular cavity, arranged between the outer wall of the recovery kettle 10 and the inner chamber 105, and its main function is to control the temperature of the inner chamber 105. The material of the temperature control chamber 60 is usually stainless steel or other corrosion-resistant materials, and the temperature inside the temperature control chamber 60 can be controlled by heating or cooling. The steam input port 601 and the condensate output port 602 are respectively arranged at one end and the other end of the temperature control chamber 60. The steam input port 601 is a pipe connected to a steam source, which introduces steam into the temperature control chamber 60 to increase the temperature of the solution in the inner chamber 105 by heating it. The condensate outlet 602 is a pipe for discharging condensate, which discharges the condensate out of the temperature control chamber 60, thereby controlling the temperature of the inner chamber 105. The temperature control chamber 60 controls the temperature of the inner chamber 105 by controlling heating or cooling. During operation, the steam input port 601 introduces steam into the temperature control chamber 60, and heats the temperature control chamber 60 to increase the temperature of the inner chamber 105; while the condensate outlet 602 discharges the condensate out of the temperature control chamber 60, thereby reducing the temperature of the inner chamber 105. By continuously adjusting the flow rate and temperature of the steam input port 601 and the condensate outlet 602, the temperature of the inner chamber 105 can be accurately controlled. The arrangement of the temperature control chamber 60, the steam input port 601 and the condensate outlet 602 can ensure the temperature of the inner chamber 105 is stable, thereby improving the extraction rate and quality of piperidine, and also preventing the volatilization and decomposition of piperidine. In addition, the flow rate and temperature of the steam input port 601 and the condensate output port 602 can be adjusted according to actual needs, thereby achieving precise temperature control and improving work efficiency and production quality.
[0065] In some embodiments, a pH meter 70 is also included, and the pH meter 70 is arranged on the recovery kettle 10 to detect the pH value of the solution in the inner chamber 105. The pH meter 70 is an instrument for detecting the pH value of a liquid, and is usually composed of a pH sensor, a signal processor, and a display. In the device, the pH meter 70 is arranged on the recovery kettle 10 to detect the pH value of the solution in the inner chamber 105. The pH meter 70 detects the pH value of the solution through a pH sensor. The pH sensor is usually composed of a glass membrane, an electrode, and a reference electrode. When the pH sensor is placed in a solution, the glass membrane reacts chemically with the hydrogen ions in the solution, thereby generating a potential difference. The electrode and the reference electrode measure this potential difference and transmit the signal to the signal processor. The signal processor converts this signal into a pH value and displays the result on a display. The setting of the pH meter 70 can detect the pH value of the solution in the inner chamber 105 in a timely manner, thereby ensuring that the pH value of the solution is within a suitable range. In the piperidine recovery process, the change of pH value will affect the solubility and extraction rate of piperidine. Therefore, the input amount of neutralizing agent and extractant can be adjusted in time through the detection of pH meter 70, so as to improve the extraction rate and quality of piperidine. In addition, the use of pH meter 70 can improve the automation degree of recovery kettle 10, reduce the error of manual operation, and improve production efficiency and product quality.
[0066] In some embodiments, a thermometer 71 is also included, and the thermometer 71 is arranged on the recovery kettle 10 to detect the temperature of the solution in the inner chamber 105. The thermometer 71 is usually composed of a temperature sensor, a signal processor and a display. In this device, the thermometer 71 is arranged on the recovery kettle 10 to detect the temperature of the solution in the inner chamber 105. The thermometer 71 detects the temperature of the solution through a temperature sensor. The temperature sensor is usually composed of a thermistor, a thermocouple or an infrared sensor. When the temperature sensor is placed in the solution, a potential difference or a light signal is generated. The sensor transmits this signal to the signal processor, and the signal processor converts this signal into a temperature and displays the result on the display. The setting of the thermometer 71 can detect the temperature of the solution in the inner chamber 105 in time and ensure that the temperature of the solution is within a suitable range. In the piperidine recovery process, the change in temperature will affect the solubility and extraction rate of piperidine. Therefore, through the detection of the thermometer 71, the temperature and flow rate of heating or cooling can be adjusted in time, thereby improving the extraction rate and quality of piperidine. In addition, the use of the thermometer 71 can improve the automation level of the recovery kettle 10, reduce errors in manual operation, and improve production efficiency and product quality.
[0067] In some embodiments, a sight glass 72 is also included, and the sight glass 72 is arranged at the rear end of the output port. The pipeline sight glass 72 is a device for observing the internal situation of the pipeline, which is usually composed of a lens and a bracket. In this device, the pipeline sight glass 72 is arranged at the rear end of the output port of the recovery kettle 10, and is used to observe the flow of the recovered solution in the pipeline. The pipeline sight glass 72 projects the pipeline interior at the rear end of the output port into the field of view of the sight glass 72 in real time through an optical lens, so that the operator can observe the flow of the recovered solution in the pipeline. The inclination angle of the lens of the pipeline sight glass 72 can be changed by adjusting the angle of the bracket to better observe the flow in the pipeline. The setting of the pipeline sight glass 72 allows the operator to observe the flow of the recovered solution in the pipeline in real time, judge whether the recovery process is normal, find problems in time and make adjustments, and ensure the quality of the recovered piperidine. In addition, the use of the pipeline sight glass 72 can facilitate the operation of the operator, reduce the occurrence of misoperation, improve the automation of the recovery kettle 10, and improve production efficiency and product quality.
[0068] In some embodiments, a branch valve 73 is also included, and the branch valve 73 is arranged at the rear end of the output port. The branch valve 73 is used to divide the alkaline wastewater and the piperidine extractant mixed solution after stratification in the inner chamber 105 into two routes for delivery to the rear end. The branch valve 73 is a device for switching pipelines in the delivery system, which plays a role in changing the flow direction of the conveyed material. It adopts a plug-type structure, which is reliable in sealing and flexible in reversing. The gear rack swing cylinder or electric actuator is used to drive the plug reversing, and a magnetic switch is installed to indicate and control the reversing of the cylinder. The electromagnetic reversing valve controls the intake and exhaust to achieve reversing. The valve of the branch valve 73 can adjust the diversion ratio of the fluid by manual or automatic control, and the alkaline wastewater and the piperidine extractant mixed solution after stratification in the recovery kettle 10 are divided into two routes for delivery to the rear end. One route is delivered to the rear end for unextracted wastewater, and the other route is delivered to the rear end for a solution containing piperidine. The arrangement of the branch valve 73 allows the operator to control the diversion ratio of the recovered solution, so that the unextracted wastewater and the solution containing piperidine are respectively transported to the rear end, thereby ensuring the purity and quality of the recovered piperidine. In addition, the use of the branch valve 73 can facilitate the operation of the operator, reduce the occurrence of misoperation, improve the automation degree of the recovery kettle 10, and improve production efficiency and product quality.
[0069] In some embodiments, a vent valve 80 is also included, and the recovery kettle 10, the first metering tank 20, the second metering tank 30 and the third metering tank 40 are all provided with the vent valve 80. The vent valve 80 is a device for discharging the gas inside the system, which is usually composed of a valve and a pipeline. In the device, the vent valve 80 is arranged on the recovery kettle 10, the first metering tank 20, the second metering tank 30 and the third metering tank 40, and is used to discharge the gas inside the system. When gas is generated inside the system, the vent valve 80 can open the valve by manual or automatic control to discharge the gas from the system. In the recovery kettle 10, the vent valve 80 can discharge the gas generated during the recovery process to maintain the pressure balance in the system. In the metering tank, the vent valve 80 can discharge the gas generated during the metering process to ensure the accuracy of the metering. The setting of the vent valve 80 allows the operator to discharge the gas inside the system in time, maintain the pressure balance of the system, avoid the problem of bubbles in the recovery process, thereby improving the purity and quality of the recovered piperidine. In addition, the use of the vent valve 80 can facilitate the operation of the operator, reduce the occurrence of misoperation, improve the automation level of the recovery kettle 10, and improve production efficiency and product quality.
[0070] In some embodiments, a plurality of valves are further included, and the plurality of valves are respectively arranged at the front end of the first metering input port 201, the front end of the second metering input port 301, the front end of the third metering input port 401, the front end of the first recycling input port 101, the front end of the second recycling input port 102, the front end of the third recycling input port 103, and the rear end of the input port. The output and input of each interface are controlled by the valves, which is convenient and fast.
[0071] Taking the actual production process as an example, the specific operation process is as follows:
[0072] Open the vent valve 80 and the first metering output port 202 of the first metering tank 20 containing piperidine wastewater, the vent valve 80 and the first recovery input port 101 of the recovery kettle 10, and after transferring 2000-2050 kg of piperidine-containing wastewater into the recovery kettle 10, close the vent valve 80 and the first metering output port 202 of the first metering tank 20 and the first recovery input port 101 of the recovery kettle 10;
[0073] Turn on the stirring mechanism 50 to stir;
[0074] Open the second metering output port 302 of the second metering tank 30 and the second recovery input port 102 of the recovery kettle 10, and add 200-300 kg of liquid alkali into the recovery kettle 10 (the actual amount added is based on the pH value of the water phase being greater than 13);
[0075] Open the third metering output port 402 of the third metering tank 40 and the third recovery input port 103 of the recovery kettle 10, add 470-500 kg of toluene, continue stirring for 30-40 minutes after adding toluene, stop stirring, and let stand for more than 30 minutes;
[0076] After the wastewater is layered, the lower layer is strongly alkaline wastewater. The output port of the recovery kettle 10 is opened to discharge the lower alkaline wastewater and transport it to other sections through pipelines for neutralization of acidic wastewater. Thus, an extraction process is completed.
[0077] After the lower layer of strongly alkaline wastewater is output, the upper layer is the toluene piperidine solution, and the above extraction process is repeated once more;
[0078] After the two toluene piperidine solutions were combined, the piperidine content was about 4%, and the piperidine recovery rate was about 80%;
[0079] The obtained toluene piperidine solution (containing a very small amount of heptenone) is directly output to the heptenone synthesis section through the output port of the recovery kettle 10 according to the measured piperidine content, and is used in the heptenone synthesis.
[0080] It should be noted that although the above embodiments have been described in this article, this does not limit the scope of patent protection of the utility model. Therefore, based on the innovative concept of the utility model, changes and modifications to the embodiments described in this article, or equivalent structural or equivalent process changes made using the contents of the utility model specification and drawings, directly or indirectly applying the above technical solutions to other related technical fields are all included in the scope of protection of the utility model patent.
Claims
1. A device for recovering piperidine from wastewater for direct application, characterized in that: include, A recovery kettle, the recovery kettle comprising an inner chamber and a first recovery input port, a second recovery input port, a third recovery input port and a recovery output port connected to the inner chamber; A first metering tank, the first metering tank comprising a first metering input port and a first metering output port, the first metering input port is used to input wastewater, and the first metering output port is connected to the first recovery input port; A second metering tank, the second metering tank comprising a second metering input port and a second metering output port, the second metering input port is used to input a neutralizing agent, and the second metering output port is connected to the second recovery input port; The third metering tank comprises a third metering input port and a third metering output port. The third metering input port is used to input the extractant, and the third metering output port is connected with the third recovery input port.
2. A device for recovering piperidine from waste water and directly applying it according to claim 1, characterized in that: The invention also comprises a stirring mechanism, which is arranged in the recovery kettle and is used for stirring the solution in the inner chamber.
3. A device for recovering piperidine from waste water for direct application according to claim 1, characterized in that: The recovery kettle also includes a temperature control cavity and a steam input port and a condensate output port communicated with the temperature control cavity. The temperature control cavity is arranged between the outer wall of the recovery kettle and the inner chamber.
4. A device for recovering piperidine from waste water for direct application according to claim 1, characterized in that: Also included is a pH meter, which is disposed on the recovery kettle and is used to detect the pH value of the solution in the inner chamber.
5. A device for recovering piperidine from waste water for direct application according to claim 1, characterized in that: The recovery kettle also includes a thermometer, which is arranged on the recovery kettle and is used to detect the temperature of the solution in the inner chamber.
6. A device for recovering piperidine from waste water for direct application according to claim 1, characterized in that: Also included is a viewing mirror, which is arranged at the rear end of the output port.
7. A device for recovering piperidine from waste water for direct application according to claim 1, characterized in that: It also includes a branch valve, which is arranged at the rear end of the output port.
8. A device for recovering piperidine from waste water for direct application according to claim 1, characterized in that: The first metering tank, the second metering tank and the third metering tank are all arranged above the recovery kettle.
9. A device for recovering piperidine from waste water for direct application according to claim 1, characterized in that: The first recovery input port, the second recovery input port and the third recovery input port are all arranged at the top of the recovery kettle; the output port is arranged at the bottom of the recovery kettle.
10. The device for recovering piperidine from waste water for direct application according to claim 1, characterized in that: It also includes a vent valve, which is provided on the recovery kettle, the first metering tank, the second metering tank and the third metering tank.