ODS recovery device and method
By designing the ODS recycling device, using azeotropic fractionation method and atomization spraying technology of batch components, the problem of difficulty in recycling HF in ODS alternatives is solved, efficient recycling is achieved, and resource waste and environmental pollution are reduced.
Patent Information
- Application Number
- CN202310191751.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-02-27
- Publication Date
- 2025-04-08
- Estimated Expiration
- 2043-02-27
AI Technical Summary
In the production process of ODS alternatives, it is difficult to effectively recover HF azeotrope with the product, resulting in waste of resources and environmental pollution.
An ODS recycling device is designed, including a mixing cylinder, agitating assembly, a flow intercepting assembly, a spraying mechanism and a fractionation tower. Through azeotropic fractionation method and atomization spraying technology of batch components, efficient recovery of HF is achieved.
It improves the recycling efficiency of HF, reduces resource waste and environmental pollution, reduces production costs, and enhances the market competitiveness of products.
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Figure CN116726528B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chemical production, and in particular relates to an ODS recovery device and method. Background Art
[0002] The ODS column is an octadecylsilane bonded silica gel filler, also called a C18 column. It is a reverse phase column and is generally used for high performance liquid chromatography analysis or separation and extraction of traditional Chinese medicines.
[0003] In the production process of ODS substitutes, the main raw materials are usually alkanes and their halogenated alkanes, alkenes and their halogenated alkanes, and the target products are prepared through fluorination, addition, substitution or disproportionation reactions. In order to achieve a better fluorination effect, an excess of HF is generally used. After the reaction, the crude product obtained often contains a large amount of HF. Most of the HF can be separated by ordinary distillation methods, but a small amount of HF will still form an azeotrope with the product, which is difficult to separate by distillation. Selecting a suitable treatment method to recover this part of HF has become an important measure to save fluorite resources and improve the environment. It is also an important aspect for fluorine chemical companies to reduce production costs and improve product market competitiveness. At present, the methods for recovering HF in the azeotrope of ODS substitutes and HF at home and abroad mainly include water washing, extraction washing, azeotropic distillation and adsorption. The extraction washing method is also a relatively mature process. Concentrated sulfuric acid, hydrofluoric acid or adding fluoride salts to hydrofluoric acid can be selected as extractants.
[0004] In the patent with publication number CN200200910138775, the hydrogen fluoride in 1234yf is absorbed to about 15wt% by extraction with 80% sulfuric acid aqueous solution, and flash evaporated to 2.0wt% by heating at 140°C. The recovered HF contains 6000ppm of water intermittent components and 500ppm of sulfur impurities in the injection mechanism. The intermediate product in the equipment is flashed to obtain hydrogen fluoride with a water content less than 100ppm and sulfur impurities less than 50ppm, which is recovered and applied to the production process of 244bb; then dilute hydrofluoric acid is used as an extractant to extract hydrogen fluoride in 134a at 35-35°C, so that the final hydrofluoric acid can be concentrated to 70%; the required ODS product is obtained after extraction.
[0005] The azeotropic distillation method has the characteristics of simple equipment, easy operation, and small one-time investment. Because HF is toxic and needs to participate in the reaction in time, the traditional industry lacks the necessary mixing equipment when atomizing and mixing the reagents before azeotropy, resulting in the solvent being poured in at one time so that the extract cannot fully contact, affecting the fractionation efficiency of ODS during the azeotropic distillation operation, resulting in low product output. In addition, the reagent mixing is frequently manually operated, which is not easy for industrial production. Summary of the invention
[0006] The purpose of the present invention is to provide an ODS recovery device and method to solve the problems raised in the above background technology. To achieve the above purpose, the following technical solution is provided: an ODS recovery device and method, comprising:
[0007] Bracket, used for overall fixing of the device;
[0008] A mixing cylinder, arranged at the upper end of the support, for mixing ODS with a fractionation reagent;
[0009] The stirring component is arranged at the left end of the mixing cylinder, which is the same as the stirring during extraction;
[0010] A shutoff assembly, arranged at the upper end of the mixing cylinder, for the dripping of ODS;
[0011] The spray mechanism is arranged in the middle of the mixing barrel, and the spray mechanism is composed of an intermittent component, an intermittent mechanism, and a connecting component, and is used for atomizing, spraying and mixing the extraction reagent;
[0012] The distillation tower is arranged at the right end of the mixing cylinder and is used for azeotropic distillation of the mixed ODS.
[0013] In the present technical scheme, when the industry purifies and recycles ODS waste, the azeotropic distillation method is adopted. In the process of preliminary removal of impurities from ODS, the mixed liquid is poured in from the interception component, and the stirring component and the injection mechanism are started. The solvent is sprayed at the injection mechanism, and then it is dispersed by stirring and atomization and finally flows out of the mixing cylinder and is pumped to the distillation tower. The distillation tower then performs azeotropic distillation according to the difference in melting and boiling points.
[0014] In any of the above technical solutions, further, the intermittent component includes:
[0015] The pressure dividing block has a pressure dividing cavity inside, which is in the shape of a pot, and the upper end of which is connected to the outside world;
[0016] The separation cap is fixedly arranged in the middle of the pressure-dividing chamber, the middle part of which is hollow, and the pressure-dividing chamber is divided into two upper and lower chambers, and the lower end of the separation cap is trumpet-shaped;
[0017] A top block is fixedly arranged at the lower end wall of the pressure-dividing chamber and has a cylindrical hole in the middle;
[0018] A slide bar is slidably arranged in the top block, on which a partition is fixedly arranged, and the partition can be closed and sealed with the lower end of the partition cap;
[0019] The return spring is sleeved on the slide rod, and the upper and lower ends are respectively fixedly connected to the partition plate and the top block, and is always in a compressed pre-tightened state;
[0020] The connecting plate is horizontally fixedly connected to the lower end of the sliding rod, and a first arc block is provided at the upper end surface thereof, and the cross section of the first arc block is in the shape of an inclined ellipsoid arc;
[0021] The leakage holes are obliquely opened at the left and right end walls of the pressure-dividing chamber;
[0022] The liquid spray pipe is threadedly connected to the middle of the leakage hole, and a through hole is arranged in the middle thereof for guiding the liquid.
[0023] In the present technical solution, the reset spring is pre-tightened in the initial state, pressing the lower end of the partition and the partition cap to separate the pressure chamber into an upper and lower chamber. Then the first arc block is forced to move downward, driving the slide rod to move downward. At this time, the slide rod and the partition are forced to move downward as a whole, and compress the reset spring. At this time, the partition is disengaged from the partition cap. At this time, the fluid in the upper chamber is sucked in under the negative pressure generated when the partition moves downward rapidly, and the fluid originally placed in the lower chamber is squeezed out from the spray pipe. When the first arc block is no longer under force, the reset spring elastically resets the partition to press the partition cap again, and the upper and lower chambers are sealed.
[0024] In any of the above technical solutions, further, the connection component includes:
[0025] The threaded ring block is fixedly arranged on the outer ring end wall of the upper end of the pressure dividing block.
[0026] The rubber ring is sleeved on the upper end of the pressure dividing block, and the lower end is tightly attached to the pressure dividing block for sealing;
[0027] The positioning external threaded barrel is sleeved on the upper end of the pressure dividing block, the inner diameter of the positioning external threaded barrel fits the outer diameter of the upper end of the pressure dividing block, and the outside is connected to the solvent pressure tank;
[0028] Internal threaded barrel, the thread is positioned at the outer end of the external threaded barrel and the rubber ring.
[0029] In the present technical solution, when it is necessary to connect the intermittent components to atomize and spray the ODS solvent, the rubber ring is first placed on the upper end of the threaded ring block, and then the upper end of the pressure divider block is inserted into the positioning external threaded barrel. The inner diameters of the pressure divider block and the positioning external threaded barrel are non-circular, so there is only freedom in the insertion direction and no rotational freedom. After insertion, the internal threaded barrel is tightened and the entire connection assembly is fixed by a threaded connection.
[0030] In any of the above technical solutions, further, the intermittent mechanism includes:
[0031] The circular annular groove is horizontally opened in the middle of the front and rear end walls of the mixing cylinder, and the middle part is provided with an annular groove;
[0032] A ring block is rotatably arranged in the ring groove of the circular ring groove;
[0033] A stepper motor is fixedly connected to the middle of the extended end surface of the ring block and is coaxial with the ring groove of the circular ring groove;
[0034] The rotating arm is fixedly arranged at the inner end surface of the ring block and is in an I-shape;
[0035] The second arc block is fixedly arranged at the upper and lower ends of the rotating arm, is arc-shaped, and transmits power to the first arc block on an inclined surface.
[0036] In the present technical solution, when the stepper motor is started, the ring block is driven to rotate around the center of the annular groove, and then the rotating arm and the second arc block rotate. When the second arc block rotates, it performs an inclined surface transmission with the arc surface of the first arc block. Because the movement direction of the first arc block is the axial direction of the slide rod, the first arc block moves downward. When the second arc block rotates a certain angle, the inclined surface of the second arc block no longer contacts the inclined surface of the first arc block. At this time, the first arc block is no longer subjected to force and rebounds and resets under the elastic force of the reset spring.
[0037] In any of the above technical solutions, further, the mixing barrel includes:
[0038] A material trough is fixedly arranged at the left end of the bracket;
[0039] A pipeline is provided between the material tank and the mixing cylinder for communication;
[0040] A cut-off pipe is arranged in the middle of the pipeline;
[0041] The flow limiting block is slidably arranged in the middle of the intercepting pipe, a spring is arranged at the lower end, and a nut is arranged at the upper end.
[0042] In the technical solution, the on-off path between the middle channel of the intercepting pipe and the pipeline is controlled by adjusting the pre-tightening nut at the upper end of the intercepting pipe, thereby achieving the effect of flow regulation.
[0043] The stirring assembly includes:
[0044] The motor is fixedly arranged at the right end of the bracket;
[0045] The stirring roller is rotatably arranged in the mixing drum and is driven by a belt sleeved on the motor and the stirring roller;
[0046] The stirring blades are evenly arranged on the stirring roller and are used for stirring and mixing the ODS.
[0047] In the technical solution, when stirring is required, the motor is started to drive the belt and the stirring roller to rotate, and the stirring blades fully stir the ODS in the mixing drum.
[0048] A transversely arranged dripping head is provided at the upper end of the inner end wall of the mixing cylinder, and a pipeline is connected thereto, and a liquid delivery pump is provided at the lower end of the mixing cylinder for pumping and delivering the ODS mixed in the mixing cylinder.
[0049] In any of the above technical solutions, further, the fractionation tower comprises:
[0050] The azeotropic chamber is fixedly arranged at the right end of the bracket, and the liquid delivery pump is connected to the azeotropic chamber for azeotropic heating of ODS;
[0051] The discharge port is fixedly arranged at the upper end of the distillation tower and is used for collecting the fractionated and condensed ODS.
[0052] A method for using an ODS recovery device comprises the following steps:
[0053] Step 1: Pour the mixed liquid of ODS and organic matter from the material tank, and then rotate the nut to adjust the liquid flow rate in the intercepting tube;
[0054] Step 2: Start the stepper motor, and the intermittent mechanism rotates, and the intermittent inclined surface of the intermittent component is transmitted, so that the vaporized solvent is sprayed out from the intermittent component through the connecting component and fully contacts with the ODS at the interception component;
[0055] Step 3: Start the stepper motor and the liquid delivery pump at the same time, so that the inorganic matter of ODS is first dissolved by the stirring component, and then pumped to the azeotropic chamber by the liquid delivery pump;
[0056] Step 4: Heat the mixture in the azeotropic chamber for azeotropic distillation, adjust the temperature in the azeotropic chamber according to the different melting and boiling points of the mixture, collect it at the discharge port, and extract the more concentrated ODS in the azeotropic chamber after diversion.
[0057] The beneficial effects of the present invention are as follows: through the intermittent component, when the ODS solvent is mixed and sprayed, the chamber is sealed by the slide rod and the partition, and the spring is sleeved in the slide rod, and the intermittent opening and closing of the intermittent component is completed by combining the first arc block and using the arc surface between the second arc block and the first arc block for inclined transmission; and then the stirring component is used to achieve stirring through belt drive, and when the belt drive is overloaded, the belt slips to protect the transmission end. BRIEF DESCRIPTION OF THE DRAWINGS
[0058] Figure 1 It is a schematic diagram of the internal structure of the present invention;
[0059] Figure 2 It is a structural schematic diagram of the injection mechanism in the present invention;
[0060] Figure 3 yes Figure 2 An enlarged schematic diagram of the structure of the middle injection mechanism;
[0061] Figure 4 It is a structural schematic diagram of the connection component in the present invention;
[0062] Figure 5 It is a three-dimensional schematic diagram of the second arc block in the present invention.
[0063] The reference numerals in the figure are: 100, bracket; 200, mixing barrel; 210, liquid delivery pump; 300, stirring assembly; 301, motor; 302, stirring roller; 303, belt; 304, stirring blade; 400, interception assembly; 401, material tank; 402, pipeline; 403, interception pipe; 404, flow limiting block; 405, spring; 500, injection mechanism; 600, intermittent assembly; 601, pressure dividing block; 602, pressure dividing chamber; 603, separation cap; 604, partition; 605, Top block; 606, slide bar; 607, return spring; 608, connecting plate; 609, first arc block; 610, drain hole; 611, spray pipe; 700, intermittent mechanism; 701, annular groove; 702, ring block; 703, stepping motor; 704, rotating arm; 705, second arc block; 800, connecting assembly; 801, threaded ring block; 802, rubber ring; 803, positioning external threaded barrel; 804, internal threaded barrel; 900, distillation tower; 901, azeotropic chamber; 902, discharge port. DETAILED DESCRIPTION
[0064] The following will be combined with the drawings in the embodiments of the present application to clearly describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments in the present application belong to the scope of protection of this application.
[0065] In the description of the present application, it should be noted that the terms used herein are only for describing specific embodiments, and are not intended to limit the exemplary embodiments according to the present application. For ease of description, the sizes of the various parts shown in the drawings are not drawn according to the actual proportional relationship. The technology, methods and equipment known to ordinary technicians in the relevant field may not be discussed in detail, but in appropriate cases, the technology, methods and equipment should be regarded as part of the authorization specification. In all examples shown and discussed here, any specific value should be interpreted as merely exemplary, rather than as a limitation. Therefore, other examples of the exemplary embodiments may have different values. It should be noted that similar numbers and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further discussed in subsequent drawings.
[0066] like Figure 1 and 2 As shown, this embodiment provides an ODS recovery device and method, including:
[0067] Bracket 100, used for overall fixing of the device;
[0068] A mixing cylinder 200 is disposed at the upper end of the support 100 and is used for mixing ODS and fractionation reagents;
[0069] A stirring assembly 300 is disposed at the left end of the mixing cylinder 200 and is used for stirring during extraction;
[0070] The interception assembly 400 is disposed at the upper end of the mixing cylinder 200 and is used for dripping of ODS;
[0071] The spray mechanism 500 is disposed in the middle of the mixing barrel 200. The spray mechanism 500 is composed of an intermittent assembly 600, an intermittent mechanism 700, and a connecting assembly 800, and is used for atomizing, spraying and mixing the extraction reagent;
[0072] The distillation tower 900 is disposed at the right end of the mixing cylinder 200 and is used for azeotropic distillation of the mixed ODS.
[0073] In the present technical solution, when the industry purifies and recycles ODS waste, an azeotropic distillation method is adopted. In the process of preliminary impurity removal of ODS, the mixed liquid is poured into the interception component 400, and the stirring component 300 and the injection mechanism 500 are started. The solvent is sprayed at the injection mechanism 500, and then dispersed by stirring and atomization, and finally flows out of the mixing cylinder 200 and is pumped to the distillation tower 900. The distillation tower 900 then performs azeotropic distillation according to the difference in melting and boiling points.
[0074] like Figure 2 and 3 As shown, specifically, the intermittent assembly 600 includes:
[0075] The pressure dividing block 601 has a pressure dividing cavity 602 inside, and the pressure dividing cavity 602 is in the shape of a pot, and the upper end is connected to the outside;
[0076] The separation cap 603 is fixedly arranged in the middle of the pressure dividing chamber 602, and the middle part is hollow, so as to divide the pressure dividing chamber 602 into two upper and lower chambers, and the lower end of the separation cap 603 is horn-shaped;
[0077] The top block 605 is fixedly arranged at the lower end wall of the pressure dividing chamber 602, and has a cylindrical hole in the middle;
[0078] A slide bar 606 is slidably disposed in the top block 605, on which a partition plate 604 is fixedly disposed, and the partition plate 604 can be closed and sealed with the lower end of the partition cap 603;
[0079] The return spring 607 is sleeved on the slide bar 606, and the upper and lower ends are respectively fixedly connected to the partition plate 604 and the top block 605, and is always in a compressed pre-tightened state;
[0080] The connecting plate 608 is horizontally fixedly connected to the lower end of the sliding rod 606, and a first arc block 609 is provided at the upper end surface thereof. The cross section of the first arc block 609 is in the shape of an inclined ellipsoid arc;
[0081] The leakage holes 610 are obliquely opened at the left and right end walls of the pressure-dividing chamber 602;
[0082] The liquid spray pipe 611 is threadedly connected to the middle of the leakage hole 610, and a through hole is provided in the middle thereof for guiding the liquid.
[0083] In the present technical scheme, the reset spring 607 is pre-tightened in the initial state, pressing against the lower end of the partition 604 and the partition cap 603, so that the pressure chamber 602 is divided into an upper and lower chamber. Then the first arc block 609 is forced to move downward, driving the slide bar 606 to move downward. At this time, the slide bar 606 and the partition 604 are forced to move downward as a whole, and compress the reset spring 607. At this time, the partition 604 is disengaged from the partition cap 603. At this time, the fluid in the upper chamber is sucked in under the negative pressure generated when the partition 604 moves downward rapidly, and the fluid originally placed in the lower chamber is squeezed out from the spray pipe 611. When the first arc block 609 is no longer under force, the reset spring 607 elastically resets the partition 604 to press the partition cap 603 again, and the upper and lower chambers are sealed.
[0084] In a preferred embodiment of the present invention:
[0085] like Figure 4 As shown, specifically, the connection component 800 includes:
[0086] The threaded ring block 801 is fixedly mounted on the outer ring end wall of the upper end of the pressure dividing block 601.
[0087] The rubber ring 802 is sleeved on the upper end of the pressure dividing block 601, and the lower end is tightly attached to the pressure dividing block 601 for sealing;
[0088] The positioning external threaded barrel 803 is sleeved on the upper end of the pressure dividing block 601, the inner diameter of the positioning external threaded barrel 803 is in close contact with the outer diameter of the upper end of the pressure dividing block 601, and the outside is connected to the solvent pressure tank;
[0089] The inner threaded tube 804 has threads which are arranged at the outer ends of the outer threaded tube 803 and the rubber ring 802 for positioning.
[0090] In the present technical solution, when it is necessary to connect the intermittent component 600 to atomize and spray the ODS solvent, the rubber ring 802 is first sleeved on the upper end of the threaded ring block 801, and then the upper end of the pressure divider block 601 is inserted into the positioning external threaded barrel 803. The inner diameters of the pressure divider block 601 and the positioning external threaded barrel 803 are non-circular, so there is only freedom in the insertion direction and no rotational freedom. After insertion, the internal threaded barrel 804 is tightened and the entire connecting component 800 is fixed by threaded connection.
[0091] In a preferred embodiment of the present invention:
[0092] like Figure 2 As shown, specifically, the intermittent mechanism 700 includes:
[0093] The annular groove 701 is horizontally opened in the middle of the front and rear end walls of the mixing cylinder 200, and the middle part is provided with an annular groove;
[0094] The ring block 702 is rotatably disposed in the ring groove of the circular ring groove 701;
[0095] The stepper motor 703 is fixedly connected to the middle of the extended end surface of the ring block 702 and is coaxial with the ring groove of the circular ring groove 701;
[0096] The rotating arm 704 is fixedly arranged at the inner end surface of the ring block 702 and is in an I-shape;
[0097] The second arc block 705 is fixedly disposed at the upper and lower ends of the rotating arm 704 , is arc-shaped, and transmits power to the first arc block 609 via an inclined surface.
[0098] In the present technical solution, when the stepper motor 703 is started, the ring block 702 is driven to rotate around the center of the annular groove 701, and then the rotating arm 704 and the second arc block 705 are rotated. When the second arc block 705 rotates, it performs an inclined surface transmission with the arc surface of the first arc block 609. Because the movement direction of the first arc block 609 is the axial direction of the slide rod 606, the first arc block 609 moves downward. When the second arc block 705 rotates a certain angle, the inclined surface of the second arc block 705 no longer contacts the inclined surface of the first arc block 609. At this time, the first arc block 609 is no longer subjected to force and rebounds and resets under the elastic force of the reset spring 607.
[0099] In a preferred embodiment of the present invention:
[0100] like Figure 1 As shown, specifically, the mixing cartridge 200 includes:
[0101] The material trough 401 is fixedly arranged at the left end of the bracket 100;
[0102] A pipe 402 is provided between the material tank 401 and the mixing cylinder 200 for communication;
[0103] The intercepting pipe 403 is arranged in the middle of the pipeline 402;
[0104] The flow limiting block 404 is slidably disposed in the middle of the intercepting pipe 403, with a spring 405 disposed at the lower end and a nut disposed at the upper end.
[0105] In the present technical solution, the on-off path between the middle channel of the intercepting tube 403 and the pipeline 402 is controlled by adjusting the pre-tightening nut at the upper end of the intercepting tube 403, thereby achieving the effect of flow regulation.
[0106] The stirring assembly 300 includes:
[0107] The motor 301 is fixedly arranged at the right end of the bracket 100;
[0108] The stirring roller 302 is rotatably disposed in the mixing drum 200 and is driven by a belt 303 sleeved on the motor 301 and the stirring roller 302;
[0109] The stirring blades 304 are evenly arranged on the stirring roller 302 and are used for stirring and mixing the ODS.
[0110] In the present technical solution, when stirring is required, the motor 301 is started to drive the belt 303 and the stirring roller 302 to rotate, and at this time, the stirring blades 304 fully stir the ODS in the mixing drum 200 .
[0111] A transversely arranged dripping head is provided at the upper end of the inner end wall of the mixing barrel 200 , and a pipeline 402 is connected thereto. A liquid delivery pump 210 is provided at the lower end of the mixing barrel 200 for pumping and delivering the ODS mixed in the mixing barrel 200 .
[0112] like Figure 2 As shown, specifically, the fractionation tower 900 includes:
[0113] The azeotropic chamber 901 is fixedly arranged at the right end of the bracket 100, and the liquid delivery pump 210 is connected to the azeotropic chamber 901 for azeotropic heating of ODS;
[0114] The discharge port 902 is fixedly disposed at the upper end of the distillation tower 900 and is used for collecting the fractionated and condensed ODS.
[0115] A method for using an ODS recovery device:
[0116] Step 1: Pour the mixed liquid of ODS and organic matter from the material tank 401, and then rotate the nut to adjust the liquid flow rate in the intercepting pipe 403;
[0117] Step 2: Start the stepper motor 703, and the intermittent mechanism 700 rotates, and the intermittent component 600 is intermittently inclined, so that the vaporized solvent is sprayed out from the intermittent component 600 through the connecting component 800 and fully contacts with the ODS at the intercepting component 400;
[0118] Step 3: Start the stepper motor 703 and the motor 301 at the same time as the liquid delivery pump 210, so that the inorganic matter of ODS is first dissolved by the stirring assembly 300, and then pumped to the azeotropic chamber 901 by the liquid delivery pump 210;
[0119] Step 4: The mixture is heated in the azeotropic chamber 901 for azeotropic fractionation, and the temperature in the azeotropic chamber 901 is adjusted according to the different melting and boiling points of the mixture, so that it is collected at the discharge port 902. After diversion, the more concentrated ODS in the azeotropic chamber 901 is extracted.
[0120] The embodiments of the present application are described above in conjunction with the accompanying drawings. In the absence of conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. The present application is not limited to the above-mentioned specific implementation methods. The above-mentioned specific implementation methods are merely illustrative and not restrictive. Under the guidance of the present application, ordinary technicians in this field can also make many forms without departing from the purpose of the present application and the scope of protection of the claims, all of which are within the protection of the present application.
Claims
1. An ODS recovery device, characterized in that: include: A bracket (100) for overall fixing of the device; A mixing cylinder (200), arranged at the upper end of the support (100), for mixing ODS and fractionation reagents; A stirring assembly (300) is arranged at the left end of the mixing cylinder (200) and is used for stirring during extraction; A shutoff assembly (400) is disposed at the upper end of the mixing cylinder (200) and is used for dripping ODS; The spray mechanism (500) is arranged in the middle of the mixing cylinder (200), and the spray mechanism (500) is composed of an intermittent component (600), an intermittent mechanism (700), and a connecting component (800), and is used for atomizing, spraying and mixing the extraction reagent; A fractionation tower (900), disposed at the right end of the mixing cylinder (200), for azeotropic fractionation of the mixed ODS; The intermittent component (600) comprises: a pressure dividing block (601) having a pressure dividing cavity (602) disposed therein, the pressure dividing cavity (602) being in the shape of a pot, the upper end of which is in communication with the outside; A separation cap (603) is fixedly arranged in the middle of the pressure-dividing chamber (602), the middle of which is hollow, and separates the pressure-dividing chamber (602) into two upper and lower chambers, and the lower end of the separation cap (603) is horn-shaped; A top block (605) is fixedly arranged at the lower end wall of the pressure dividing chamber (602), and a cylindrical hole is provided in the middle thereof; A sliding rod (606) is slidably disposed in the top block (605), on which a partition plate (604) is fixedly disposed, and the partition plate (604) can be closed and sealed with the lower end of the partition cap (603); The return spring (607) is sleeved on the slide rod (606), and the upper and lower ends are respectively fixedly connected to the partition plate (604) and the top block (605), and is always in a compressed pre-tightened state; A connecting plate (608) is horizontally fixedly connected to the lower end of the sliding rod (606), and a first arc block (609) is provided at the upper end surface thereof, wherein the cross section of the first arc block (609) is in the shape of an inclined ellipsoid arc; Leakage holes (610) are obliquely provided on the left and right end walls of the pressure-dividing chamber (602); A liquid spray pipe (611) is threadedly connected to the middle of the leakage hole (610), and a through hole is provided in the middle thereof for guiding the liquid; The intermittent mechanism (700) comprises: a circular annular groove (701) horizontally opened in the middle of the front and rear end walls of the mixing cylinder (200), wherein the middle thereof is provided with an annular groove; A ring block (702) is rotatably disposed in the ring groove of the circular ring groove (701); A stepping motor (703) is fixedly connected to the middle of the extended end surface of the ring block (702) and is coaxial with the annular groove (701); The rotating arm (704) is fixedly arranged on the inner end surface of the ring block (702) and is in an I-shape; The second arc block (705) is fixedly arranged at the upper and lower ends of the rotating arm (704), is arc-shaped, and is transmitted with the first arc block (609) in an inclined plane.
2. An ODS recovery device according to claim 1, characterized in that: The connection assembly (800) comprises: a threaded ring block (801) fixedly arranged on the outer ring end wall of the upper end of the pressure dividing block (601); a rubber ring (802) sleeved on the upper end of the pressure dividing block (601), with the lower end tightly attached to the pressure dividing block (601) for sealing; A positioning external threaded barrel (803) is sleeved on the upper end of the pressure dividing block (601), the inner diameter of the positioning external threaded barrel (803) is in close contact with the outer diameter of the upper end of the pressure dividing block (601), and the outside is connected to the solvent pressure tank; The internal threaded barrel (804) has threads on the outer ends of the positioning external threaded barrel (803) and the rubber ring (802).
3. An ODS recovery device according to claim 2, characterized in that: The intercepting assembly (400) comprises: a material holding trough (401) fixedly arranged at the left end of the bracket (100); A pipeline (402) is provided between the material storage tank (401) and the mixing cylinder (200) for communication; A cut-off pipe (403) is arranged in the middle of the pipeline (402); The flow limiting block (404) is slidably arranged in the middle of the intercepting pipe (403), a spring (405) is arranged at the lower end, and a nut is arranged at the upper end.
4. An ODS recovery device according to claim 3, characterized in that: The stirring assembly (300) comprises: a motor (301) fixedly arranged at the right end of the bracket (100); A stirring roller (302) is rotatably disposed in the mixing drum (200) and is driven by a belt (303) sleeved on the motor (301) and the stirring roller (302); The stirring blades (304) are evenly arranged on the stirring roller (302) and are used for stirring and mixing the ODS.
5. An ODS recovery device according to claim 4, characterized in that: The upper end of the inner end wall of the mixing cylinder (200) is provided with a transversely arranged dripping head, and the pipeline (402) is connected to it, and the lower end of the mixing cylinder (200) is provided with a liquid delivery pump (210) for pumping and delivering the ODS mixed in the mixing cylinder (200).
6. An ODS recovery device according to claim 5, characterized in that: The fractionation tower (900) comprises: an azeotropic chamber (901) fixedly arranged at the right end of the support (100), and the liquid delivery pump (210) is connected to the azeotropic chamber (901) for azeotropic heating of ODS; The discharge port (902) is fixedly arranged at the upper end of the distillation tower (900) and is used for collecting the fractionated and condensed ODS.
7. A method for using the ODS recovery device according to claim 6, characterized in that: Step 1: Pour the mixed liquid of ODS and organic matter from the material tank (401), and then rotate the nut to adjust the liquid flow rate in the intercepting pipe (403); Step 2: Start the stepper motor (703), at which time the intermittent mechanism (700) rotates and transmits intermittently with the intermittent component (600) in an intermittent inclined plane, so that the vaporized solvent is sprayed out from the intermittent component (600) through the connecting component (800) and fully contacts with the ODS at the intercepting component (400); Step 3: Start the stepper motor (703) and the motor (301) at the same time as the liquid delivery pump (210), so that the inorganic matter of ODS is first dissolved by the stirring assembly (300), and then pumped to the azeotropic chamber (901) by the liquid delivery pump (210); Step 4: The mixture is heated in the azeotropic chamber (901) for azeotropic fractionation, and the temperature in the azeotropic chamber (901) is adjusted according to the different melting and boiling points of the mixture, so that it is collected at the discharge port (902). After diversion, the more concentrated ODS in the azeotropic chamber (901) is extracted.
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Energy-saving and efficient aromatic hydrocarbon extraction system
CN215462184U