Treatment equipment for ethanol and water mixed mother liquor and purification method for sodium nitrate and potassium nitrate
By using inclined plates and linkage plates in the ethanol-water mixed mother liquor treatment equipment to control the precipitation of flocculation groups, the problem of difficult waste liquid after ethanol distillation is solved, and efficient and stable flocculation effect is achieved, which facilitates the discharge and recycling of waste liquid.
Patent Information
- Application Number
- CN202510599052.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-10
- Publication Date
- 2025-07-04
- Estimated Expiration
- 2045-05-10
AI Technical Summary
In the prior art, the residual waste liquid of ethanol-water mixed mother liquor is not convenient for flocculation treatment after ethanol distillation, especially the fine flocculation group is prone to surging upward, affecting the overall treatment effect.
A treatment device including a flocculation box, a flocculation frame and a driving mechanism is designed. The inclined plates and linkage plates are arranged in an equidistant manner to control the flip of the inclined plates to block and precipitate fine flocculation groups. Combined with the use of distillation and flocculant, the efficient and stable flocculation treatment is achieved.
It ensures efficient flocculation treatment of ethanol-water mixed mother liquor, avoids congestion of flocculation, facilitates subsequent discharge or recycling, and improves the stability and efficiency of waste liquid treatment.
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Figure CN120247200A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of waste liquid treatment, and particularly to a treatment device for an ethanol and water mixed mother liquor and a purification method for sodium nitrate and potassium nitrate. Background Art
[0002] The alcohol precipitation method (also known as the alcohol washing method) is a separation technique based on the regulation of solvent polarity. By adding an alcohol solvent to a mixed solution, the polarity environment of the system is changed, thereby reducing the solubility of the target substance and promoting its selective precipitation, especially suitable for the separation of potassium nitrate (KNO3) and sodium nitrate (NaNO3).
[0003] During the process of separating and purifying sodium nitrate and potassium nitrate using the alcohol precipitation method, an ethanol-water mixed mother liquor will be generated, and this mixed waste liquid needs to be distilled and purified for reuse. Especially when the separation of ethanol in the ethanol-water mixed mother liquor is completed, if the remaining waste liquid is not promptly treated and discharged, it will produce polluted wastewater. Therefore, various means are needed to treat the waste liquid after separating ethanol before it can be discharged or recycled.
[0004] In the prior art, the waste liquid left after distillation contains a small amount of impurities (such as metal ions, organic substances), and it is necessary to first use a flocculation method to flocculate the impurities in the waste liquid into clusters, which is convenient for subsequent waste liquid treatment. When a PAM-type flocculant is used in the treatment process, the small flocculation clusters are extremely easy to surge upwards, thus affecting the overall treatment effect of the waste liquid.
[0005] Therefore, it is necessary to provide a treatment device for an ethanol and water mixed mother liquor and a purification method for sodium nitrate and potassium nitrate to solve the above technical problems. Summary of the Invention
[0006] The present invention provides a treatment device for an ethanol and water mixed mother liquor and a purification method for sodium nitrate and potassium nitrate, which solves the technical problem that the residual waste liquid is not convenient for flocculation treatment after the distillation of ethanol in the ethanol-water mixed mother liquor in the related art.
[0007] To solve the above technical problems, the treatment device for an ethanol and water mixed mother liquor provided by the present invention includes a flocculation tank, a flocculation frame, and a driving mechanism;
[0008] An installation plate is installed on the top of the flocculation frame through bolts. The driving mechanism includes an installation frame installed on the upper surface of the installation plate. The inner walls of the installation frame are respectively fixedly provided with a top plate and a bottom plate. A double-headed motor is installed between the top plate and the bottom plate inside the installation frame through bolts. The top output shaft of the double-headed motor is keyed to a first ratchet wheel. The outer wall of the first ratchet wheel is meshed with a first ratchet ring. The outer wall of the first ratchet ring is keyed to a cam;
[0009] The bottom output shaft keyway of the double-headed motor is connected with a second ratchet wheel, the outer wall of the second ratchet wheel is meshed and connected with a second ratchet tooth ring, and the bottom of the second ratchet tooth ring is integrally provided with a first belt pulley;
[0010] A partition is fixedly arranged on the inner wall of the flocculation tank and on one side of the flocculation frame. A plurality of equally spaced inclined plates are rotatably connected to the right side of the partition on the inner wall of the flocculation tank. A limiting plate is fixedly arranged above the inclined plates on the inner wall of the flocculation tank. A plurality of linkage plates are slidably connected inside the limiting plate. A connecting plate is fixedly arranged at the top of the plurality of linkage plates. A groove plate is fixedly arranged on the outer wall of the flocculation tank. A slider is fixedly arranged on the side wall of the connecting plate. A vertical rod is fixedly arranged at the top of the connecting plate. A top rod is fixedly arranged at the top of the vertical rod. A guide wheel is installed at the middle position of the top rod. Limiting rods are fixedly arranged at the front and rear ends above the plurality of inclined plates. A liquid outlet pipe is installed on the side wall of the flocculation tank.
[0011] Preferably, the outer wall of the first ratchet tooth ring is rotatably connected with the top plate through a bearing, and the outer wall of the second ratchet tooth ring is rotatably connected with the bottom plate through a bearing.
[0012] Preferably, the outer wall of the guide wheel is mutually attached to the outer wall of the cam. The slider is horizontally slidably connected with the groove plate through a spring. The outer walls on both sides of the limiting rod are mutually attached to the inner walls on both sides of the linkage plate.
[0013] Preferably, a flocculation mechanism is installed inside the flocculation frame. The flocculation mechanism includes a rotating rod fixedly arranged at the keyway connection and the center of the first belt pulley. A plurality of equally spaced annularly distributed support rods are fixedly arranged on the outer wall of the rotating rod. A toothed ring is installed on the inner wall of the flocculation frame. Two gears are meshed and connected above the toothed ring. An installation block is fixedly arranged at the bottom end of the rotating rod. Flocculation plates are rotatably connected to both sides of the installation block.
[0014] Preferably, the centers of the two flocculation plates are fixedly connected with the centers of the two gears respectively. The outer wall of the rotating rod is rotatably connected with the installation plate through a bearing.
[0015] Preferably, it further includes a base, a distillation mechanism and a medicine adding mechanism. The distillation mechanism includes a water bath bucket placed on the upper surface of the base. An electric heating tube is installed inside the water bath bucket. A sealing plate is installed on the top of the water bath bucket through bolts. A distillation bucket is integrally arranged at the center of the sealing plate. An end cover is installed on the top of the distillation bucket through bolts. An injection pipe, a discharge pipe and a distillation pipe are installed through the end cover. A condensing pipe is installed on the outer wall of the distillation pipe. An exhaust mechanism is installed inside the water bath bucket;
[0016] The exhaust mechanism includes an exhaust pipe fixed on the inner wall of the water bath barrel. Inside the water bath barrel and at the outlet end of the exhaust pipe, a fixed pipe is fixedly installed. Two sliding grooves are formed on the inner wall of the fixed pipe, and a sliding pipe is slidably connected inside the two sliding grooves. Through holes are formed on the outer wall of the sliding pipe.
[0017] Preferably, a positioning frame is fixedly installed on the upper surface of the base and on one side of the water bath barrel. A condensation box is installed inside the positioning frame. A clamping plate is fixedly installed on the outer wall of the positioning frame. The chemical addition mechanism includes a side plate fixed on the side wall of the flocculation box and below the clamping plate. A second pulley is rotatably connected to the top of the side plate. A belt is sleeved on the outer walls of the first pulley and the second pulley. A mixing cylinder is fixedly installed on the inner wall of the clamping plate. A screw rod is keyway-connected to the axis of the second pulley. A chemical addition pipe is installed on the top of the mixing cylinder, and an inclined chemical discharge pipe is installed below the mixing cylinder.
[0018] Preferably, both sides of the sliding pipe are slidably connected to the two sliding grooves through clamping blocks. Both the upper and lower ends of the screw rod are rotatably connected to the mixing cylinder through bearings. The exhaust pipe and the condensation box are sealed and installed above. The bottom of the condensation box is sealed and installed with the side wall of the mixing cylinder.
[0019] The purification method of sodium nitrate and potassium nitrate includes the following steps:
[0020] S1: Prepare a mixture of sodium nitrate and potassium nitrate, and mechanically stir until completely dissolved to form a mixed solution of sodium nitrate and potassium nitrate;
[0021] S2: Filter the mixed solution in S1 to remove insoluble impurities;
[0022] S3: Transfer the filtrate in S2 to a constant temperature water bath reactor, control the temperature at 25°C, slowly add ethanol at a ratio of the solution mass to the mass of absolute ethanol of 1:0.5 - 1, and continuously stir at a rate of 200 rpm / min. After the addition of ethanol is completed, continue to stir for ten minutes, and then let it stand at 5°C - 50°C for 30 minutes to precipitate white flocculent potassium nitrate;
[0023] S4: Perform vacuum filtration on the mixed system after standing in S3 to separate and obtain crude potassium nitrate solid (filter cake) and the filtrate containing sodium nitrate;
[0024] S5: Transfer the filtrate obtained in S4 to a rotary evaporator, concentrate it under reduced pressure at 80°C and -0.09 MPa, evaporate 70% - 90% of the original volume, cool the remaining concentrated solution to 10°C to precipitate sodium nitrate crystals, and obtain crude sodium nitrate solid after filtration.
[0025] S6: adding the crude potassium nitrate obtained in S4 to a saturated aqueous solution of potassium nitrate at a solid-liquid mass ratio of 1:0.5-2, stirring at 250 rpm / min for 20 minutes, filtering and drying to obtain high-purity potassium nitrate crystals; adding the crude sodium nitrate obtained in S5 to a saturated sodium nitrate solution of sodium nitrate at 40° C. at a solid-liquid mass ratio of 1:0.5-2, stirring at 200 rpm / min for 15 minutes, filtering, and drying to obtain high-purity sodium nitrate crystals;
[0026] S7: The ethanol-water mixed mother liquor produced in S3 and S5 is recovered and reused in the ethanol precipitation process of S3 after distillation and purification, thereby realizing solvent recycling. In this step, it is necessary to operate and use the treatment equipment of the ethanol and water mixed mother liquor.
[0027] Compared with the related art, the treatment equipment for the mixed mother liquor of ethanol and water and the method for purifying sodium nitrate and potassium nitrate provided by the present invention have the following beneficial effects:
[0028] Sloped plates are arranged equidistantly to ensure that large flocculants can settle inside the flocculation box. During the overflow and drainage process, the internal water body of the flocculation box will change, and small flocculants will surge upward. Initially, the inclined plates with a large slope can block and capture the flocculants surging upward to prevent the flocculants from overflowing with the water through the inclined plates. At the same time, a linkage plate can be used to control multiple inclined plates to synchronously flip and change the slope to make it smaller. In this way, the flocculants captured on the inclined plates can be shaken to settle downward to avoid congestion of the flocculants and ensure rapid overflow and drainage. Therefore, this design can flocculate the waste liquid very well, ensure efficient and stable flocculation, and control the wastewater very well, which is convenient for subsequent discharge or recycling. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying creative work.
[0030] Figure 1 A schematic diagram of the best structure provided by the present invention;
[0031] Figure 2 for Figure 1 The enlarged structural diagram of point A shown;
[0032] Figure 3 for Figure 1 The schematic diagram of the driving mechanism structure shown;
[0033] Figure 4Schematic diagram of the bottom structure of the driving mechanism shown in Figure 3 ;
[0034] Figure 5 Schematic diagram of the top structure of the driving mechanism shown in Figure 3 ;
[0035] Figure 6 Schematic diagram of the sectional structure of the flocculation tank provided by the present invention;
[0036] Figure 7 Schematic diagram of the enlarged structure at position B shown in Figure 6 ;
[0037] Figure 8 Schematic diagram of the enlarged structure at position C shown in Figure 6 ;
[0038] Figure 9 Schematic diagram of the initial state of the inclined plate shown in Figure 6 ;
[0039] Figure 10 Schematic diagram of the working state of controlling the flipping of the inclined plate when the cam rotates shown in Figure 9 ;
[0040] Figure 11 Schematic diagram of the structure of the distillation mechanism shown in Figure 1 ;
[0041] Figure 12 Schematic diagram of the disassembled structure of the distillation mechanism shown in Figure 11 ;
[0042] Figure 13 Schematic diagram of the working of the exhaust mechanism, where (a) represents the initial working state diagram of the exhaust mechanism when the water bath bucket is not heated, and (b) is the exhaust working state diagram of the exhaust mechanism when the steam is ejected;
[0043] Figure 14 Schematic diagram of the structure of the flocculation mechanism provided by the present invention;
[0044] Figure 15 Schematic diagram of the structure of the chemical dosing mechanism provided by the present invention.
[0045] Explanation of the reference numerals in the drawings:
[0046] 1. Flocculation tank, 2. Mounting plate;
[0047] 3. Driving mechanism, 31. Mounting frame, 32. Top plate, 33. Bottom plate, 34. Double-headed motor, 35. First ratchet wheel, 36. First ratchet ring, 37. Cam, 38. Second ratchet wheel, 39. Second ratchet ring, 310. First pulley, 311. Belt;
[0048] 4. Flocculation mechanism, 41. Rotating rod, 42. Support rod, 43. Toothed ring, 44. Mounting block, 45. Gear, 46. Flocculation plate;
[0049] 5. Base;
[0050] 6. Distillation mechanism, 61. Water bath bucket, 62. Sealing plate, 63. Distillation bucket, 64. End cover, 65. Injection pipe, 66. Discharge pipe, 67. Distillation pipe, 68. Condensing pipe, 69. Electric heating pipe;
[0051] 7. Chemical adding mechanism, 71. Side plate, 72. Second belt pulley, 73. Mixing cylinder, 74. Screw rod, 75. Chemical adding pipe, 76. Chemical discharging pipe;
[0052] 8. Exhaust mechanism, 81. Fixed pipe, 82. Exhaust pipe, 83. Chute, 84. Sliding pipe, 85. Through hole;
[0053] 9. Flocculation frame, 10. Liquid outlet pipe, 11. Limit plate, 12. Inclined plate, 13. Linking plate, 14. Connecting plate, 15. Grooved plate, 16. Slide block, 17. Vertical rod, 18. Top rod, 19. Guide wheel, 20. Partition board, 21. Limiting rod, 22. Positioning frame, 23. Clamping plate, 24. Condensing box.
[0054] The realization, functional features and advantages of the purpose of the present invention will be further described with reference to the embodiments and the accompanying drawings. Specific embodiments
[0055] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0056] The present invention provides a processing device for ethanol and water mixed mother liquor and a purification method for sodium nitrate and potassium nitrate.
[0057] First embodiment:
[0058] The purification method for sodium nitrate and potassium nitrate includes the following steps:
[0059] S1: Prepare a mixture of sodium nitrate and potassium nitrate, and mechanically stir until completely dissolved to form a mixed solution of sodium nitrate and potassium nitrate;
[0060] S2: Filter the mixed solution in S1 to remove insoluble impurities;
[0061] S3: Transfer the filtrate of S2 to a constant temperature water bath reactor, control the temperature at 25°C, slowly add ethanol at a ratio of the solution mass to the mass of anhydrous ethanol of 1:0.5 - 1, while continuously stirring at a rate of 200 rpm / min. After the addition of ethanol is complete, continue stirring for ten minutes, and then let it stand for 30 minutes at 5°C - 50°C to precipitate white flocculent potassium nitrate;
[0062] S4: Vacuum filter the mixed system after standing in S3 to separate the crude potassium nitrate solid (filter cake) and the filtrate containing sodium nitrate;
[0063] S5: Transfer the filtrate obtained in S4 to a rotary evaporator, concentrate it under reduced pressure at 80°C and -0.09 MPa, evaporate 70% - 90% of the original volume, cool the remaining concentrated solution to 10°C to precipitate sodium nitrate crystals, and obtain crude sodium nitrate solid after filtration.
[0064] S6: Add the crude potassium nitrate obtained in S4 to a saturated aqueous solution of potassium nitrate at a solid-liquid mass ratio of 1:0.5 - 2, stir at 250 rpm / min for 20 minutes, filter and dry to obtain high-purity potassium nitrate crystals; add the crude sodium nitrate obtained in S5 to a saturated sodium nitrate solution at 40°C at a solid-liquid mass ratio of 1:0.5 - 2, stir at 200 rpm / min for 15 minutes, filter, and obtain high-purity sodium nitrate crystals after drying;
[0065] S7: Recover the ethanol-water mixed mother liquor generated in S3 and S5, and after distillation and purification, reuse it in the ethanol precipitation process of S3 to achieve solvent recycling. In this step, it is necessary to operate in combination with the processing equipment for the ethanol-water mixed mother liquor.
[0066] Embodiment:
[0067] (1): Weigh sodium nitrate and potassium nitrate, add deionized water and dissolve them completely. Stir at 60 °C until completely dissolved to form a mixed solution. Remove insoluble impurities by filtration to obtain a clear filtrate. Transfer the filtrate to a water bath, control the temperature at 25 °C, and slowly add ethanol at a ratio of the solution mass to the mass of absolute ethanol of 1:0.5 - 1 while mechanically stirring at a rate of 200 rpm / min. After adding, continue stirring for 10 min, let it stand at 25 °C for 30 min, and observe the precipitation of white flocculent precipitate. Separate the precipitate (crude potassium nitrate) and the filtrate (containing sodium nitrate) by vacuum filtration. Transfer the filtrate to a rotary evaporator, concentrate it under reduced pressure by 80% of the original volume, cool to 10 °C to precipitate crystals, and filter to obtain crude sodium nitrate. Add the crude potassium nitrate to a pre-prepared saturated aqueous solution of potassium nitrate with a solid-liquid ratio of (1:0.5 - 2), stir at 250 rpm / min for 20 min, filter, and dry to obtain high-purity potassium nitrate. Add the crude sodium nitrate to a saturated ethanol solution of sodium nitrate with a solid-liquid ratio of (1:0.5 - 2), stir at 200 rpm / min for 15 min, filter and dry to obtain high-purity sodium nitrate. The recovery rates of the final products potassium nitrate and sodium nitrate are both above 50%, and the purity can reach over 99% after being washed with a saturated nitrate solution.
[0068]
[0069]
[0070] (2): What is changed in this method is the standing temperature. Weigh sodium nitrate and potassium nitrate, add deionized water and dissolve them completely. Stir at 60 °C until completely dissolved to form a mixed solution. Remove insoluble impurities by filtration to obtain a clear filtrate. Transfer the filtrate to a water bath, control the temperature at 25 °C, and slowly add ethanol at a ratio of the solution mass to the mass of absolute ethanol of 1:(0.5 - 1) while mechanically stirring at a rate of 200 rpm / min. After adding, continue stirring for 10 min, let it stand at 5 °C for 30 min, and observe the precipitation of white flocculent precipitate. Separate the precipitate (crude potassium nitrate) and the filtrate (containing sodium nitrate) by vacuum filtration. Transfer the filtrate to a rotary evaporator, concentrate it under reduced pressure by 80% of the original volume, cool to 10 °C to precipitate crystals, and filter to obtain crude sodium nitrate. Add the crude potassium nitrate to a pre-prepared saturated aqueous solution of potassium nitrate with a solid-liquid ratio of (1:0.5 - 2), stir at 250 rpm / min for 20 min, filter, and dry to obtain high-purity potassium nitrate. Add the crude sodium nitrate to a saturated ethanol solution of sodium nitrate with a solid-liquid ratio of (1:0.5 - 2), stir at 200 rpm / min for 15 min, filter and dry to obtain high-purity sodium nitrate. The recovery rates of the final products potassium nitrate and sodium nitrate are both above 50%, and the purity can reach over 99% after being washed with a saturated nitrate solution.
[0071]
[0072] (3): What this method changes is the concentration degree. Weigh sodium nitrate and potassium nitrate, add deionized water and dissolve them completely. Stir at 60 °C until completely dissolved to form a mixed solution. Remove insoluble impurities by filtration to obtain a clear filtrate. Transfer the filtrate to a water bath, control the temperature at 25 °C, slowly add ethanol at a ratio of the solution mass to the mass of anhydrous ethanol of 1:(0.5 - 1), and mechanically stir at a rate of 200 rpm / min simultaneously. After adding, continue to stir for 10 min, let it stand at 25 °C for 30 min, and observe that white flocculent precipitates precipitate out. Separate the precipitate (crude potassium nitrate) and the filtrate (containing sodium nitrate) by vacuum filtration. Transfer the filtrate to a rotary evaporator, concentrate it under reduced pressure by 90% of the original volume, cool it to 10 °C, and crystals precipitate out. Filter to obtain crude sodium nitrate. Add the crude potassium nitrate to a pre-prepared saturated aqueous solution of potassium nitrate, with a solid-liquid ratio of (1:0.5 - 2), stir at 250 rpm / min for 20 min, filter, and dry to obtain high-purity potassium nitrate. Add the crude sodium nitrate to a saturated ethanol solution of sodium nitrate, with a solid-liquid ratio of (1:0.5 - 2), stir at 200 rpm / min for 15 min, filter and dry to obtain high-purity sodium nitrate. The recovery rates of the final products potassium nitrate and sodium nitrate are both above 50%, and the purity can reach over 99% after being washed with a saturated nitrate solution.
[0073]
[0074] This example:
[0075] For the separation of potassium nitrate (KNO3) and sodium nitrate (NaNO3), traditional methods mostly rely on the temperature-dependent differences in their solubilities (such as evaporation concentration crystallization or cooling crystallization). However, when the solubility differences between the two salts are small (such as the solubilities of potassium nitrate and sodium nitrate being similar at room temperature), traditional methods have low separation efficiency, high energy consumption, and questionable purity. The alcohol precipitation method reduces the polarity of the aqueous solution by introducing alcohol solvents (such as ethanol, methanol, etc.), and realizes efficient separation by taking advantage of the significant differences in the solubilities of the two nitrates in the alcohol-water mixed system. The solvent alcohols can be recovered by distillation and reused;
[0076] Evaporation concentration crystallization: By heating and concentrating the solution, the salt with lower solubility (such as sodium nitrate) precipitates out first. However, the solubility changes of potassium nitrate and sodium nitrate with temperature have a small difference (especially in the medium and low temperature ranges), resulting in incomplete separation, requiring multiple recrystallizations, high energy consumption, and low yield;
[0077] Cooling crystallization: It is suitable for substances such as potassium nitrate whose solubility changes significantly with temperature, but has a poor separation effect on sodium nitrate and requires long-term temperature control, with low efficiency;
[0078] The basic solution of the present invention is alcohol precipitation method + washing with saturated nitrate solution. Most of potassium nitrate can be filtered out after the alcohol precipitation method. Secondly, from the perspective of energy consumption, the high-energy-consuming conditions of high-temperature concentration + cooling crystallization are avoided for separating potassium nitrate. The filtrate obtained after the alcohol precipitation method can be evaporated and concentrated to obtain sodium nitrate. The purity of sodium nitrate and potassium nitrate can reach over 95%. Then, by washing with the corresponding saturated solution, the purity can reach over 99%.
[0079] Second Embodiment:
[0080] Please refer to Figure 1 、 Figure 2 、 Figure 11 and Figure 12 . The treatment equipment for the ethanol and water mixed mother liquor further includes a base 5, a distillation mechanism 6 and a dosing mechanism 7. The distillation mechanism 6 includes a water bath barrel 61 placed on the upper surface of the base 5. An electric heating tube 69 is installed inside the water bath barrel 61. A sealing plate 62 is installed at the top of the water bath barrel 61 through bolts. A distillation barrel 63 is integrally provided at the center of the sealing plate 62. An end cover 64 is installed at the top of the distillation barrel 63 through bolts. An injection pipe 65, a discharge pipe 66 and a distillation pipe 67 are installed through the end cover 64. A condensing pipe 68 is installed on the outer wall of the distillation pipe 67. An exhaust mechanism 8 is installed inside the water bath barrel 61.
[0081] Please refer to Figure 11 and Figure 12 : In step S7 of the first embodiment, before distillation, the end cover 64 and the distillation barrel 63 need to be sealed and installed. After installation, clear water needs to be added inside the water bath barrel 61 (the water level should not be higher than the exhaust mechanism 8). Then, the entire distillation barrel 63 needs to be placed inside the water bath barrel 61 and pass through the electric heating tube 69;
[0082] In step S7 of the first embodiment, the generated ethanol-water mixed mother liquor is injected into the distillation barrel 63 through the injection pipe 65 (the volume of the ethanol-water mixed mother liquor does not exceed 2 / 3 of the capacity of the distillation barrel 63). Then, the user controls the temperature rise inside the water bath barrel 61 by heating the electric heating tube 69 to heat the distillation barrel 63 (slowly raise the temperature to the boiling point of ethanol 78.3 °C, control the temperature to avoid violent boiling, and zeolite can be added);
[0083] The ethanol generated by distillation will enter the curved distillation pipe 67. The outer wall of the distillation pipe 67 is cooled by the condensing pipe 68, so that the distilled ethanol is condensed into a liquid for recovery. Finally, the residual waste liquid without ethanol is inside the distillation barrel 63. The residual waste liquid inside the distillation barrel 63 can be pumped out through the discharge pipe 66 and stored centrally for subsequent treatment.
[0084] The exhaust mechanism 8 includes an exhaust pipe 82 fixedly mounted on the inner wall of the water bath tub 61. A fixed pipe 81 is fixedly mounted inside the water bath tub 61 and at the exhaust end of the exhaust pipe 82. Two slide grooves 83 are formed on the inner wall of the fixed pipe 81. A sliding pipe 84 is slidably connected inside the two slide grooves 83. A through hole 85 is formed on the outer wall of the sliding pipe 84.
[0085] See also Figure 12 and Figure 13 : In order to ensure the internal environment of the distillation barrel 63 is stable, an exhaust mechanism 8 is usually provided. Since a large amount of steam is generated inside the water bath barrel 61 when it is heated, the internal pressure will be too high, and the generated steam will push the sliding tube 84 upward;
[0086] See also Figure 13 (a): In the initial state, the through hole 85 and the exhaust pipe 82 are separated, so the entire interior of the water bath 61 is sealed and the internal and external pressures are balanced;
[0087] See also Figure 13 (b) in the figure: the steam generated when the water bath 61 is heated will form a pressure difference between the inside and the outside, and the steam will push the sliding tube 84 upward. At this time, the sliding tube 84 will slide vertically upward along the slide groove 83. When sliding, the through hole 85 will be staggered with the inner hole of the exhaust pipe 82, and the excess steam will pass through the through hole 85 from the inside of the sliding tube 84 and finally be exhausted from the exhaust pipe 82.
[0088] It is understandable that since the slide groove 83 is not designed as a through groove, when the temperature inside the water bath 61 decreases and the pressure remains constant, the sliding tube 84 will automatically return to the initial state.
[0089] In this embodiment, the ethanol-water mixed mother liquor is distilled by water bath heating. The ethanol can be well distilled and precipitated while the heating is stable, and the ethanol can be fully recovered and reused. Secondly, an exhaust device that can automatically rise and fall according to the steam pressure is provided to discharge the steam generated by the water bath heating, so as to achieve the balance of internal and external pressures of the water bath heating, which can be used to accurately adjust the temperature to avoid boiling caused by excessive temperature, and also increase the stability and safety of the entire distillation process.
[0090] Third embodiment:
[0091] See also Figures 1 to 10 and Figure 14 , comprising a flocculation box 1, a flocculation frame 9 and a driving mechanism 3;
[0092] The top of the flocculation frame 9 is installed with a mounting plate 2 through bolts. The driving mechanism 3 includes a mounting frame 31 installed on the upper surface of the mounting plate 2. The inner walls of the mounting frame 31 are respectively fixed with a top plate 32 and a bottom plate 33. A double-headed motor 34 is installed between the top plate 32 and the bottom plate 33 inside the mounting frame 31 through bolts. The top output shaft of the double-headed motor 34 is keyed to a first ratchet wheel 35. The outer wall of the first ratchet wheel 35 is meshed with a first ratchet ring 36. The outer wall of the first ratchet ring 36 is keyed to a cam 37.
[0093] The bottom output shaft of the double-headed motor 34 is keyed to a second ratchet wheel 38. The outer wall of the second ratchet wheel 38 is meshed with a second ratchet ring 39. The bottom of the second ratchet ring 39 is integrally provided with a first belt pulley 310.
[0094] Please refer Figure 1 and Figure 2 : Under the process of the second embodiment, residual waste liquid losing ethanol will be generated. When the waste liquid is collected to meet the carrying capacity of the flocculation tank 1, the user needs to add the waste liquid into the flocculation tank 1 through the flocculation frame 9 for flocculation treatment.
[0095] Please refer to Figures 3 to 5 : Starting the double-headed motor 34 can control the free clockwise or counterclockwise rotational movement of the upper and lower ends of the double-headed motor 34. Since the helical tooth setting directions of the first ratchet wheel 35 and the second ratchet wheel 38 are different, when the double-headed motor 34 rotates clockwise, the second ratchet wheel 38 will rotate clockwise within the second ratchet ring 39, thus forming an avoidance to ensure that the second ratchet wheel 38 will not affect the rotation of the second ratchet ring 39. Then, the clockwise rotating first ratchet wheel 35 will affect and control the first ratchet ring 36 to drive the outer cam 37 to rotate synchronously clockwise.
[0096] If it rotates counterclockwise, the cam 37 will not rotate, while the second ratchet wheel 38 at the bottom of the double-headed motor 34 will counterclockwise affect and drive the second ratchet ring 39 and the first belt pulley 310 to rotate counterclockwise.
[0097] The flocculation mechanism 4 is installed inside the flocculation frame 9. The flocculation mechanism 4 includes a rotating rod 41 fixedly installed at the keyway connection with the axis of the first belt pulley 310. The outer wall of the rotating rod 41 is fixedly provided with equally spaced annularly distributed support rods 42. A toothed ring 43 is installed on the inner wall of the flocculation frame 9. Two gears 45 are meshed above the toothed ring 43. The bottom end of the rotating rod 41 is fixedly provided with a mounting block 44. Both sides of the mounting block 44 are rotatably connected with flocculation plates 46.
[0098] Please refer to Figure 4 and Figure 14When the first pulley 310 rotates, the first pulley 310 will synchronously drive the rotating rod 41 at the bottom to rotate. When the rotating rod 41 rotates, the support rod 42 on the outside of the rotating rod 41 and the mounting block 44 at the bottom will also rotate together. When the mounting block 44 rotates, it will drive the flocculation plates 46 on both sides to rotate. When the flocculation plates 46 rotate, they will drive the gears 45 installed respectively to rotate along the axis of the toothed ring 43. A meshing rotation is formed between the gear 45 and the toothed ring 43, and the flocculation plates 46 installed respectively are controlled to rotate in the vertical direction, so that the waste liquid and flocculant in the flocculation frame 9 are fully contacted and mixed.
[0099] A partition 20 is fixedly provided on the inner wall of the flocculation box 1 and located on one side of the flocculation frame 9, and an equidistantly arranged inclined plate 12 is rotatably connected to the inner wall of the flocculation box 1 and located on the right side of the partition 20. A limit plate 11 is fixedly provided on the inner wall of the flocculation box 1 and located above the inclined plate 12. A plurality of linkage plates 13 are slidably connected inside the limit plate 11, and a connecting plate 14 is fixedly provided on the top of the plurality of linkage plates 13. A groove plate 15 is fixedly provided on the outer wall of the flocculation box 1, and a sliding block 16 is fixedly provided on the side wall of the connecting plate 14. A vertical rod 17 is fixedly provided on the top of the connecting plate 14, and a top rod 18 is fixedly provided on the top of the vertical rod 17. A guide wheel 19 is installed in the middle position of the top rod 18. Limit rods 21 are fixedly provided on the front and rear ends above the plurality of inclined plates 12, and a liquid outlet pipe 10 is installed on the side wall of the flocculation box 1.
[0100] The outer wall of the first ratchet ring 36 is rotatably connected to the top plate 32 via a bearing, and the outer wall of the second ratchet ring 39 is rotatably connected to the bottom plate 33 via a bearing.
[0101] The outer wall of the guide wheel 19 fits with the outer wall of the cam 37 , the slider 16 is horizontally slidably connected to the slot plate 15 via a spring, and the outer walls on both sides of the limiting rod 21 fit with the inner walls on both sides of the linkage plate 13 .
[0102] See also Figures 6 to 10 : When the flocculant and the waste liquid are mixed, the liquid will automatically form flocs inside the flocculation box 1, gathering the impurities together. Since the density of the flocs and the liquid is different, the flocs will settle at the bottom of the flocculation box 1, and the liquid will be discharged through the liquid outlet pipe 10 by overflow;
[0103] Please refer again Figure 9 : In the initial state, a plurality of inclined plates 12 are arranged on the inner wall of the flocculation box 1, and the flocculated liquid will overflow upward through the inclined plates 12 and can be discharged only after passing through the inclined plates 12;
[0104] The fine floccules at the bottom will surge upward, and the multiple inclined plates 12 can block and capture the fine floccules surging upward;
[0105] Please refer againFigure 10 When the cam 37 rotates clockwise, the long end of the cam 37 will contact the guide wheel 19 and move it to the right. The guide wheel 19 can control the linkage of the ejector rod 18 and the vertical rod 17 to control the connecting plate 14, so that multiple linkage plates 13 drive the corresponding limiting rods 21 to control the corresponding inclined plate 12 to rotate clockwise inside the flocculation tank 1, changing the inclination of the inclined plate 12.
[0106] Please refer to Figure 7 and Figure 8 : Each limiting rod 21 and the linkage plate 13 are in a fitting limit. In this way, when the linkage plate 13 moves left and right, it can control the limiting rod 21 to slide along the vertical direction of the linkage plate 13. In this way, when the linkage plate 13 moves, it can also ensure that the inclined plate 12 can be smoothly flipped, avoiding interference;
[0107] At the same time, an elastic sliding is adopted between the connecting plate 14 and the flocculation tank 1, which can always ensure that the guide wheel 19 is attached to the outer wall of the cam 37, and the inclined plate 12 can automatically reset even after flipping.
[0108] In this embodiment: The upper and lower output shafts of the double-headed motor 34 can be rotated in a partitioned manner. When the double-headed motor 34 rotates clockwise, the cam 37 rotates. When the double-headed motor 34 rotates counterclockwise, the first belt pulley 310 rotates;
[0109] When the first belt pulley 310 rotates, it can control the rotating rod 41 to realize the linkage rotation of the support rod 42 and the flocculation plate 46. Since the rotation direction of the support rod 42 is horizontal rotation, and the rotation of the flocculation plate 46 is vertical rotation, the flocculant and the waste liquid can be premixed by the support rod 42 first. Then, when the mixed liquid enters the flocculation plate 46, the mixed liquid falling on the flocculation plate 46 will be secondarily mixed by the vertically rotating flocculation plate 46. Secondly, the flocculation plate 46 can also rotate horizontally, so that the flocculant and the waste liquid can be rotated and mixed irregularly, ensuring full mixing, improving the flocculation effect, and avoiding uneven distribution of the flocculant;
[0110] Meanwhile, during the flocculation process, inclined plates 12 are arranged at equal intervals to ensure that large flocculent masses can precipitate inside the flocculation tank 1. During the overflow drainage process, the water body inside the flocculation tank 1 changes, and the small flocculent masses will surge upward. Initially, the inclined plates 12 with a large slope can block and capture the upward surging flocculent masses to prevent the flocculent masses from overflowing with the water flow through the inclined plates 12. At the same time, a linkage plate 13 can be used to control the linkage and synchronous flipping of multiple inclined plates 12 to reduce the slope, so that the captured flocculent masses on the inclined plates 12 can be jolted and precipitated downward to avoid congestion of the flocculent masses and ensure rapid overflow drainage. Therefore, such a design can effectively perform flocculation treatment on the waste liquid, ensure high-efficiency and stable flocculation, and can well control the wastewater, facilitating subsequent discharge or recycling and reuse.
[0111] Fourth Embodiment:
[0112] On the upper surface of the base 5 and on one side of the water bath barrel 61, a positioning frame 22 is fixedly installed. Inside the positioning frame 22, a condensation box 24 is installed. On the outer wall of the positioning frame 22, a clamping plate 23 is fixedly installed. The chemical dosing mechanism 7 includes a side plate 71 fixedly installed on the side wall of the flocculation tank 1 and below the clamping plate 23. At the top of the side plate 71, a second pulley 72 is rotatably connected. A belt 311 is sleeved on the outer walls of the first pulley 310 and the second pulley 72. Inside the inner wall of the clamping plate 23, a mixing cylinder 73 is fixedly installed. At the keyway of the axis of the second pulley 72, a screw rod 74 is key-connected. At the top of the mixing cylinder 73, a chemical dosing pipe 75 is installed. Below the mixing cylinder 73, an inclined chemical discharging pipe 76 is installed.
[0113] Both sides of the sliding pipe 84 are slidably connected to the two chutes 83 through clamping blocks. The upper and lower ends of the screw rod 74 are rotatably connected to the mixing cylinder 73 through bearings. The exhaust pipe 82 is hermetically installed above the condensation box 24, and the bottom of the condensation box 24 is hermetically installed with the side wall of the mixing cylinder 73.
[0114] Please refer to Figures 3, Figure 4 、 Figure 11 and Figure 15 : During the working process of the second embodiment, the steam generated when the water bath barrel 61 is heated will be discharged into the condensation box 24 through the exhaust mechanism 8 and condensed by the condensation box 24 to form distilled water, which is stored inside the condensation box 24;
[0115] During the operation of the third embodiment, when the first pulley 310 rotates, the transmission control belt 311 drives the second pulley 72 to drive the screw rod 74 to rotate inside the mixing barrel 73. At this time, PAM type flocculation powder (other powder type flocculants are also acceptable) can be added to the mixing barrel 73 through the dosing tube 75, and the distilled water inside the condensation box 24 will enter the mixing barrel 73. When the screw rod 74 rotates, the distilled water and the flocculant can be fully mixed and transported downward. When the mixed flocculant enters the position of the lower drug tube 76, it will enter the flocculation frame 9 through the lower drug tube 76 to contact and mix with the waste liquid.
[0116] In this embodiment, the distillation process and the water treatment process are linked and combined to work. The steam generated during the distillation process can be fully recovered to form condensed distilled water, making full use of the waste heat and waste gas recovery, and the generated distilled water can be stored in the condensation box 24, which can not only be used for experimental water, but also can be connected with the mixing cylinder 73. When the flocculation mechanism 4 is in the process of rotating work, it will drive the spiral rod 74 to rotate to achieve dilution and dissolution between the flocculant and the distilled water, and the drug and the waste liquid are mixed and flocculated. This design can be used for a variety of flocculants. Not only can powder flocculation be used, but solvent flocculation can also achieve drug flocculation. Secondly, the recycled distilled water is used for flocculation and mixing. The distilled water can ensure the stability between molecules. At the same time, it comes from recycled water, which can be more environmentally friendly.
[0117] The above description is only a preferred embodiment of the present invention, and does not limit the patent scope of the present invention. All equivalent structural changes made by using the contents of the present invention specification and drawings under the concept of the present invention, or directly / indirectly applied in other related technical fields are included in the patent protection scope of the present invention.
Claims
1. Processing equipment for ethanol and water mixed mother liquor, characterized in that, It includes a flocculation tank, a flocculation frame and a driving mechanism; An installation plate is installed on the top of the flocculation frame through bolts. The driving mechanism includes an installation frame installed on the upper surface of the installation plate. A top plate and a bottom plate are respectively fixed on the inner wall of the installation frame. A double-headed motor is installed between the top plate and the bottom plate inside the installation frame through bolts. A first ratchet is key-connected to the top output shaft of the double-headed motor. A first ratchet ring is meshed with the outer wall of the first ratchet. A cam is key-connected to the outer wall of the first ratchet ring; A second ratchet is key-connected to the bottom output shaft of the double-headed motor. A second ratchet ring is meshed with the outer wall of the second ratchet. A first belt pulley is integrally arranged at the bottom of the second ratchet ring; A partition is fixed on the inner wall of the flocculation tank on one side of the flocculation frame. A plurality of equally spaced inclined plates are rotatably connected to the right side of the partition on the inner wall of the flocculation tank. A limiting plate is fixed above the inclined plates on the inner wall of the flocculation tank. A plurality of linkage plates are slidably connected inside the limiting plate. A connecting plate is fixed on the top of the plurality of linkage plates. A groove plate is fixed on the outer wall of the flocculation tank. A slider is fixed on the side wall of the connecting plate. A vertical rod is fixed on the top of the connecting plate. A top rod is fixed on the top of the vertical rod. A guide wheel is installed at the middle position of the top rod. Limiting rods are fixed at the front and rear ends above the plurality of inclined plates. A liquid outlet pipe is installed on the side wall of the flocculation tank.
2. The treatment device for the ethanol and water mixed mother liquor according to claim 1, characterized in that, The outer wall of the first ratchet ring is rotatably connected to the top plate through a bearing. The outer wall of the second ratchet ring is rotatably connected to the bottom plate through a bearing.
3. The treatment device for the ethanol and water mixed mother liquor according to claim 1, characterized in that The outer wall of the guide wheel is in mutual fit with the outer wall of the cam. The slider is horizontally slidably connected to the groove plate through a spring. The outer walls on both sides of the limiting rod are in mutual fit with the inner walls on both sides of the linkage plate.
4. The processing equipment for the ethanol and water mixed mother liquor according to claim 1, wherein A flocculation mechanism is installed inside the flocculation frame. The flocculation mechanism includes a rotating rod fixedly installed at the key connection with the axis of the first belt pulley. A plurality of equally spaced annularly distributed support rods are fixed on the outer wall of the rotating rod. A toothed ring is installed on the inner wall of the flocculation frame. Two gears are meshed above the toothed ring. An installation block is fixed at the bottom end of the rotating rod. Flocculation plates are rotatably connected to both sides of the installation block.
5. The treatment equipment for the ethanol and water mixed mother liquor according to claim 4, characterized in that, The axes of the two flocculation plates are fixedly connected to the axes of the two gears. The outer wall of the rotating rod is rotatably connected to the installation plate through a bearing.
6. The treatment device for the ethanol and water mixed mother liquor according to claim 1, characterized in that, It also includes a base, a distillation mechanism and a medicine adding mechanism. The distillation mechanism includes a water bath bucket placed on the upper surface of the base. An electric heating tube is installed inside the water bath bucket. A sealing plate is installed on the top of the water bath bucket through bolts. A distillation bucket is integrally arranged at the axis of the sealing plate. An end cover is installed on the top of the distillation bucket through bolts. An injection pipe, a discharge pipe and a distillation pipe are installed through the end cover. A condensing pipe is installed on the outer wall of the distillation pipe. An exhaust mechanism is installed inside the water bath bucket; The exhaust mechanism includes an exhaust pipe fixed on the inner wall of the water bath bucket. A fixed pipe is fixed at the air outlet end of the exhaust pipe inside the water bath bucket. Two chutes are opened on the inner wall of the fixed pipe. A sliding pipe is slidably connected inside the two chutes. A through hole is opened on the outer wall of the sliding pipe.
7. The treatment device for the ethanol and water mixed mother liquor according to claim 6, characterized in that, On the upper surface of the base and on one side of the water bath barrel, a positioning frame is fixedly installed. Inside the positioning frame, a condensation box is installed. On the outer wall of the positioning frame, a clamping plate is fixedly installed. The chemical addition mechanism includes a side plate fixedly installed on the side wall of the flocculation box and below the clamping plate. At the top of the side plate, a second pulley is rotatably connected. A belt is sleeved on the outer walls of the first pulley and the second pulley. Inside the clamping plate, a mixing cylinder is fixedly installed. At the keyway of the axis of the second pulley, a spiral rod is connected. On the top of the mixing cylinder, a chemical addition pipe is installed. Below the mixing cylinder, an inclined chemical discharging pipe is installed.
8. The processing equipment for the ethanol and water mixed mother liquor according to claim 7, characterized in that, On both sides of the sliding pipe, it is slidably connected to the two chutes through clamping blocks. The upper and lower ends of the spiral rod are rotatably connected to the mixing cylinder through bearings. The exhaust pipe is hermetically installed above the condensation box. The bottom of the condensation box is hermetically installed with the side wall of the mixing cylinder.
9. A method for purifying sodium nitrate and potassium nitrate, characterized in that, The purification method of sodium nitrate and potassium nitrate includes the treatment equipment for the ethanol and water mixed mother liquor as described in any one of claims 1-8, and includes the following steps: S1: Prepare a mixture of sodium nitrate and potassium nitrate, and mechanically stir until completely dissolved to form a mixed solution of sodium nitrate and potassium nitrate; S2: Filter the mixed solution in S1 to remove insoluble impurities; S3: Transfer the filtrate in S2 to a constant temperature water bath reactor, control the temperature at 25°C, slowly dropwise add ethanol at a ratio of the solution mass to the mass of anhydrous ethanol of 1:0.5-1, and continuously stir at a rate of 200 rpm / min. After the addition of ethanol is completed, continue to stir for ten minutes, and then let it stand at 5°C-50°C for 30 minutes to precipitate white flocculent potassium nitrate precipitate; S4: Perform vacuum filtration on the mixed system after standing in S3 to separate and obtain crude potassium nitrate solid (filter cake) and the filtrate containing sodium nitrate; S5: Transfer the filtrate obtained in S4 to a rotary evaporator, and under the conditions of 80°C and -0.09 MPa, perform vacuum concentration to evaporate 70%-90% of the original volume. After the remaining concentrated solution is cooled to 10°C, sodium nitrate crystals precipitate, and after filtration, crude sodium nitrate solid is obtained. S6: Add the crude potassium nitrate obtained in S4 to a saturated aqueous solution of potassium nitrate at a solid-liquid mass ratio of 1:0.5-2, stir at 250 rpm / min for 20 minutes, filter and dry to obtain high-purity potassium nitrate crystals; add the crude sodium nitrate obtained in S5 to a saturated sodium nitrate solution at 40°C at a solid-liquid mass ratio of 1:0.5-2, stir at 200 rpm / min for 15 minutes, filter, and dry to obtain high-purity sodium nitrate crystals; S7: Recover the ethanol-water mixed mother liquor generated in S3 and S5, and after distillation and purification, reuse it in the ethanol precipitation process of S3 to realize solvent recycling. In this step, it is necessary to operate in combination with the treatment equipment for the ethanol and water mixed mother liquor.
Citation Information
Patent Citations
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CN119954347A
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KR101345262B1
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