Treatment equipment for mixed mother liquor of ethanol and water and purification method for sodium nitrate and potassium nitrate

Abstract

The present invention provides a treatment device for a mixed mother liquor of ethanol and water and a method for purifying sodium nitrate and potassium nitrate, and relates to the technical field of waste liquid treatment, including a flocculation box, a flocculation frame, and a driving mechanism; the top of the flocculation frame is fixed with a mounting plate by bolts, and the driving mechanism includes a mounting frame installed on the upper surface of the mounting plate, and the inner wall of the mounting frame is fixed with a top plate and a bottom plate. In the process of overflow drainage in this case, the internal water body of the flocculation box will change, and small flocculants will surge upward. Initially, the inclined plate with a large slope can block and capture the flocculants that surge upward, preventing the flocculants from overflowing through the inclined plate and following the water flow. At the same time, a linkage plate can be used to control multiple inclined plates to synchronously flip and change the slope, and the flocculants captured on the inclined plate are shaken to precipitate downward, ensuring rapid overflow drainage. Therefore, such a design can perform good flocculation treatment on the waste liquid, ensure efficient and stable flocculation, and facilitate subsequent discharge or recycling and reuse.

Description

Technical Field

[0001] The invention relates to the technical field of waste liquid treatment, in particular to equipment for treating a mixed mother liquor of ethanol and water and a method for purifying sodium nitrate and potassium nitrate. Background Art

[0002] Alcohol precipitation (also known as alcohol washing) is a separation technology based on solvent polarity regulation. By adding alcohol solvents to the mixed solution, the polarity environment of the system is changed, thereby reducing the solubility of the target substance and promoting its selective precipitation. It is particularly 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 by alcohol precipitation, an ethanol-water mixed mother liquor is generated, which needs to be distilled and purified for reuse. In particular, after the ethanol in the ethanol-water mixed mother liquor is separated, if the remaining waste liquid is not treated and discharged in time, it will produce polluted wastewater. Therefore, it is necessary to use multiple means to treat the waste liquid after the ethanol is separated before it can be discharged or recycled for reuse.

[0004] In the prior art, the waste liquid left after distillation contains a small amount of impurities (such as metal ions and organic matter). Flocculation is required to flocculate the impurities in the waste liquid into clumps to facilitate subsequent waste liquid treatment. During the treatment process of the PAM flocculant, the small flocculants are very likely to surge upward, thereby affecting the overall treatment effect of the waste liquid.

[0005] Therefore, it is necessary to provide a treatment plant for a mixed mother liquor of ethanol and water and a method for purifying sodium nitrate and potassium nitrate to solve the above-mentioned technical problems. Summary of the Invention

[0006] The present invention provides equipment for treating a mixed mother liquor of ethanol and water and a method for purifying sodium nitrate and potassium nitrate, thereby solving the technical problem in the related art that, after the ethanol in the mixed mother liquor is distilled, the residual waste liquid is inconvenient to flocculate.

[0007] In order to solve the above technical problems, the present invention provides a treatment device for a mixed mother liquor of ethanol and water, comprising a flocculation box, a flocculation frame and a driving mechanism;

[0008] The top of the flocculation frame is mounted with a mounting plate by bolts, and the driving mechanism includes a mounting bracket mounted on the upper surface of the mounting plate, the inner walls of the mounting bracket are respectively fixed with a top plate and a bottom plate, a double-headed motor is mounted inside the mounting bracket and between the top plate and the bottom plate by bolts, the top output shaft keyway of the double-headed motor is connected to a first ratchet, the outer wall of the first ratchet is meshed with a first ratchet ring, and the outer wall keyway of the first ratchet ring is connected to a cam;

[0009] The bottom output shaft keyway of the double-headed motor is connected to a second ratchet wheel, the outer wall of the second ratchet wheel is meshedly connected to a second ratchet ring, and the bottom of the second ratchet ring is integrally provided with a first pulley;

[0010] The inner wall of the flocculation box is fixedly provided with a partition on one side of the flocculation frame, the inner wall of the flocculation box is located on the right side of the partition and is rotatably connected with an equidistantly arranged inclined plate, the inner wall of the flocculation box is located above the inclined plate and is fixed with a limit plate, the inner side of the limit plate is slidably connected with a plurality of linkage plates, the top of the plurality of linkage plates is fixed with a connecting plate, the outer wall of the flocculation box is fixed with a groove plate, the side wall of the connecting plate is fixed with a slider, the top of the connecting plate is fixed with a vertical rod, the top of the vertical rod is fixed with a push rod, the middle position of the push rod is installed with a guide wheel, the front and rear ends above the plurality of inclined plates are fixed with limiting rods, and the side wall of the flocculation box is installed with a liquid outlet pipe.

[0011] Preferably, the outer wall of the first ratchet ring is rotatably connected to the top plate via a bearing, and the outer wall of the second ratchet ring is rotatably connected to the bottom plate via a bearing.

[0012] Preferably, the outer wall of the guide wheel fits with the outer wall of the cam, the slider is horizontally slidably connected to the slot plate through a spring, and the outer walls on both sides of the limiting rod fit with the inner walls on both sides of the linkage plate.

[0013] Preferably, a flocculation mechanism is installed inside the flocculation frame, and the flocculation mechanism includes a rotating rod fixed at the axis of the first pulley, the outer wall of the rotating rod is fixed with equidistant annular support rods, the inner wall of the flocculation frame is installed with a toothed ring, the upper part of the toothed ring is meshed with two gears, the bottom end of the rotating rod is fixed with a mounting block, and both sides of the mounting block are rotatably connected to flocculation plates.

[0014] Preferably, the axes of the two flocculation plates are fixedly connected to the axes of the two gears, and the outer wall of the rotating rod is rotatably connected to the mounting plate via a bearing.

[0015] Preferably, the invention further comprises a base, a distillation mechanism and a dosing mechanism, wherein the distillation mechanism comprises a water bath placed on the upper surface of the base, an electric heating tube is installed inside the water bath, a sealing plate is installed on the top of the water bath by bolts, a distillation barrel is integrally provided at the axis of the sealing plate, an end cover is installed on the top of the distillation barrel by bolts, an injection pipe, a discharge pipe and a distillation pipe are installed through the inside of the end cover, a condenser is installed on the outer wall of the distillation pipe, and an exhaust mechanism is installed inside the water bath;

[0016] The exhaust mechanism includes an exhaust pipe fixed on the inner wall of the water bath tub, a fixed pipe is fixed inside the water bath tub and at the air outlet end of the exhaust pipe, the inner wall of the fixed pipe is provided with two sliding grooves, the interior of the two sliding grooves is slidably connected with a sliding pipe, and the outer wall of the sliding pipe is provided with a through hole.

[0017] Preferably, a positioning frame is fixedly provided on the upper surface of the base and located on one side of the water bath, a condensation box is installed inside the positioning frame, a clamping plate is fixedly provided on the outer wall of the positioning frame, the dosing mechanism includes a side plate fixedly provided on the side wall of the flocculation box and located 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 provided on the inner wall of the clamping plate, a spiral rod is connected to the keyway at the axis of the second pulley, a dosing tube is installed on the top of the mixing cylinder, and an inclined drug discharge tube is installed below the mixing cylinder.

[0018] Preferably, the two sides of the sliding tube are slidingly connected to the two sliding grooves through blocks, the upper and lower ends of the spiral rod are rotatably connected to the mixing barrel through bearings, the exhaust pipe and the top of the condensation box are sealed, and the bottom of the condensation box is sealed to the side wall of the mixing barrel.

[0019] The method for purifying sodium nitrate and potassium nitrate comprises the following steps:

[0020] S1: preparing to mix sodium nitrate and potassium nitrate, and mechanically stirring 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 from S2 to a thermostatic water bath reactor, control the temperature at 25°C, and slowly add ethanol dropwise at a ratio of 1:0.5-1 of solution mass to anhydrous ethanol mass, while continuously stirring at 200 rpm. Continue stirring for ten minutes after the addition of ethanol, then let it stand at 5°C-50°C for 30 minutes to precipitate a white flocculent potassium nitrate precipitate;

[0023] S4: vacuum filtration is performed on the mixed system after standing in S3 to separate the crude potassium nitrate solid (filter cake) and the filtrate containing sodium nitrate;

[0024] S5: The filtrate obtained in S4 was transferred to a rotary evaporator and concentrated under reduced pressure at 80°C and -0.09 MPa to evaporate 70%-90% of the original volume. The remaining concentrated solution was cooled to 10°C to precipitate sodium nitrate crystals, which were filtered to obtain crude sodium nitrate solid;

[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 for 20 minutes, filtering and drying to obtain high-purity potassium nitrate crystals; adding the crude sodium nitrate obtained in S5 to a saturated aqueous solution of sodium nitrate at 40° C. at a solid-liquid mass ratio of 1:0.5-2, stirring at 200 rpm 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 it in conjunction with the treatment equipment of the ethanol and water mixed mother liquor.

[0027] Compared with the related art, the processing equipment for the mixed mother liquor of ethanol and water and the purification method of sodium nitrate and potassium nitrate provided by the present invention have the following beneficial effects:

[0028] Inclined plates are arranged at equal intervals to ensure that large flocs can settle inside the flocculation box. During the overflow and drainage process, the internal water body of the flocculation box will change, and small flocs will surge upward. Initially, the inclined plates with a large slope can block and capture the flocs surging upward, preventing the flocs from overflowing through the inclined plates with the water flow. 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 flocs captured on the inclined plates can be shaken and precipitated downward to avoid congestion of the flocs, ensuring 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 and reuse. 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 following briefly introduces the drawings required for use in the embodiments or the description of the prior art. 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 any 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 is shown;

[0032] Figure 3 for Figure 1 Schematic diagram of the driving mechanism structure shown;

[0033] Figure 4 for Figure 3 The schematic diagram of the bottom structure of the driving mechanism shown;

[0034] Figure 5 for Figure 3 The top structure diagram of the driving mechanism shown;

[0035] Figure 6 A schematic diagram of the cross-sectional structure of a flocculation box provided by the present invention;

[0036] Figure 7 for Figure 6 The enlarged structural diagram of point B is shown;

[0037] Figure 8 for Figure 6 The enlarged structural diagram of position C is shown;

[0038] Figure 9 for Figure 6 Schematic diagram of the initial state of the inclined plate shown;

[0039] Figure 10 for Figure 9 The schematic diagram of the working state of the cam controlling the tilting plate when the cam rotates is shown;

[0040] Figure 11 for Figure 1 The schematic diagram of the distillation mechanism shown;

[0041] Figure 12 for Figure 11 The schematic diagram of the split structure of the distillation mechanism shown;

[0042] Figure 13 Schematic diagram of the exhaust mechanism, wherein (a) is a schematic diagram of the exhaust mechanism in its initial working state when the water bath is not heated, and (b) is a schematic diagram of the exhaust mechanism in its exhaust working state when steam is ejected;

[0043] Figure 14 A schematic diagram of the flocculation mechanism structure provided by the present invention;

[0044] Figure 15 This is a schematic structural diagram of the dosing mechanism provided by the present invention.

[0045] Description of Figure Numbers:

[0046] 1. Flocculation box, 2. Mounting plate;

[0047] 3. Driving mechanism, 31. Mounting frame, 32. Top plate, 33. Bottom plate, 34. Double-headed motor, 35. First ratchet, 36. First ratchet ring, 37. Cam, 38. Second ratchet, 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, 62. Sealing plate, 63. Distillation barrel, 64. End cover, 65. Injection pipe, 66. Discharge pipe, 67. Distillation pipe, 68. Condenser, 69. Electric heating pipe;

[0051] 7. Dosing mechanism, 71. Side plate, 72. Second pulley, 73. Mixing cylinder, 74. Screw rod, 75. Dosing pipe, 76. Dropping pipe;

[0052] 8. Exhaust mechanism, 81. Fixed pipe, 82. Exhaust pipe, 83. Slide groove, 84. Sliding pipe, 85. Through hole;

[0053] 9. Flocculation frame, 10. Liquid outlet pipe, 11. Limit plate, 12. Inclined plate, 13. Linkage plate, 14. Connecting plate, 15. Groove plate, 16. Slider, 17. Vertical pole, 18. Top rod, 19. Guide wheel, 20. Partition, 21. Limit rod, 22. Positioning frame, 23. Card plate, 24. Condensation box.

[0054] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings and in conjunction with the embodiments. DETAILED DESCRIPTION

[0055] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0056] The invention provides equipment for processing a mixed mother liquor of ethanol and water and a method for purifying sodium nitrate and potassium nitrate.

[0057] First embodiment:

[0058] The method for purifying sodium nitrate and potassium nitrate comprises the following steps:

[0059] S1: preparing to mix sodium nitrate and potassium nitrate, and mechanically stirring 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 from S2 to a thermostatic water bath reactor, control the temperature at 25°C, and slowly add ethanol dropwise at a ratio of 1:0.5-1 of solution mass to anhydrous ethanol mass, while continuously stirring at 200 rpm. Continue stirring for ten minutes after the addition of ethanol, then let it stand at 5°C-50°C for 30 minutes to precipitate a white flocculent potassium nitrate precipitate;

[0062] S4: vacuum filtration is performed on the mixed system after standing in S3 to separate the crude potassium nitrate solid (filter cake) and the filtrate containing sodium nitrate;

[0063] S5: The filtrate obtained in S4 was transferred to a rotary evaporator and concentrated under reduced pressure at 80°C and -0.09 MPa to evaporate 70%-90% of the original volume. The remaining concentrated solution was cooled to 10°C to precipitate sodium nitrate crystals, which were filtered to obtain crude sodium nitrate solid;

[0064] 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 for 20 minutes, filtering and drying to obtain high-purity potassium nitrate crystals; adding the crude sodium nitrate obtained in S5 to a saturated aqueous solution of sodium nitrate at 40° C. at a solid-liquid mass ratio of 1:0.5-2, stirring at 200 rpm for 15 minutes, filtering, and drying to obtain high-purity sodium nitrate crystals;

[0065] 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 it in conjunction with the treatment equipment of the ethanol and water mixed mother liquor.

[0066] Implementation method:

[0067] (1): Weigh sodium nitrate and potassium nitrate, add deionized water to completely dissolve, and 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 1:0.5-1 of solution mass to anhydrous ethanol mass, and mechanically stir at 200 rpm. Continue stirring for 10 minutes after addition. After standing at 25°C for 30 minutes, a white flocculent precipitate is observed. Separate the precipitate (crude potassium nitrate) and the filtrate (containing sodium nitrate) by vacuum filtration. Transfer the filtrate to a rotary evaporator, concentrate under reduced pressure to 80% of the original volume, cool to 10°C, precipitate crystals, and filter to obtain crude sodium nitrate. Add the crude potassium nitrate to a pre-prepared saturated potassium nitrate aqueous solution at a solid-liquid ratio of (1:0.5-2), stir at 250 rpm for 20 minutes, filter, and dry to obtain high-purity potassium nitrate. Crude sodium nitrate is added to a saturated sodium nitrate ethanol solution at a solid-to-liquid ratio of 1:0.5-2. Stir at 200 rpm for 15 minutes, filter, and dry to obtain high-purity sodium nitrate. The final product, potassium nitrate, and sodium nitrate, have a recovery rate exceeding 50%, and after washing with a saturated nitrate solution, the purity can reach over 99%.

[0068] calcium% sodium% Potassium % Sulfate % Crude sodium nitrate 0.07 28.02 0.89 0.037 Crude potassium nitrate 0.09 0.91 35.923 0.0548 High-purity sodium nitrate 0.002 24.86 0.3 0.0248 High-purity potassium nitrate 0.002 0.22 37.33 0.0159

[0069] (2): This method changes the standing temperature. Weigh sodium nitrate and potassium nitrate, add deionized water to completely dissolve, and 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 solution mass to anhydrous ethanol mass of 1: (0.5-1), and mechanically stir at a rate of 200 rpm. Continue stirring for 10 minutes after addition. After standing at 5°C for 30 minutes, a white flocculent precipitate is observed. Separate the precipitate (crude potassium nitrate) and the filtrate (containing sodium nitrate) by vacuum filtration. Transfer the filtrate to a rotary evaporator, concentrate under reduced pressure to 80% of the original volume, cool to 10°C, precipitate crystals, and filter to obtain crude sodium nitrate. Add the crude potassium nitrate to a pre-prepared saturated potassium nitrate aqueous solution at a solid-liquid ratio of (1:0.5-2), stir at 250 rpm for 20 minutes, filter, and dry to obtain high-purity potassium nitrate. Crude sodium nitrate is added to a saturated sodium nitrate ethanol solution at a solid-to-liquid ratio of 1:0.5-2. Stir at 200 rpm for 15 minutes, filter, and dry to obtain high-purity sodium nitrate. The final product, potassium nitrate, and sodium nitrate, have a recovery rate exceeding 50%, and after washing with a saturated nitrate solution, the purity can reach over 99%.

[0070] calcium% sodium% Potassium % Sulfate % Crude sodium nitrate 0.06 23.598 1.66 0.065 Crude potassium nitrate 0.07 0.855 35.659 0.0589 High-purity sodium nitrate 0.003 27.382 0.164 0.0125 High-purity potassium nitrate 0.002 0.282 35.386 0.0256

[0071] (3): This method changes the degree of concentration. Weigh sodium nitrate and potassium nitrate, add deionized water to completely dissolve, and 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 1: (0.5-1) of solution mass to anhydrous ethanol mass, while mechanically stirring at a speed of 200 rpm. Continue stirring for 10 minutes after addition. After standing at 25°C for 30 minutes, a white flocculent precipitate is observed. Separate the precipitate (crude potassium nitrate) and the filtrate (containing sodium nitrate) by vacuum filtration. Transfer the filtrate to a rotary evaporator, concentrate under reduced pressure to 90% of the original volume, cool to 10°C, precipitate crystals, and filter to obtain crude sodium nitrate. Add the crude potassium nitrate to a pre-prepared saturated potassium nitrate aqueous solution at a solid-liquid ratio of (1:0.5-2), stir at 250 rpm for 20 minutes, filter, and dry to obtain high-purity potassium nitrate. Crude sodium nitrate is added to a saturated sodium nitrate ethanol solution at a solid-to-liquid ratio of 1:0.5-2. Stir at 200 rpm for 15 minutes, filter, and dry to obtain high-purity sodium nitrate. The final product, potassium nitrate, and sodium nitrate, have a recovery rate exceeding 50%, and after washing with a saturated nitrate solution, the purity can reach over 99%.

[0072] calcium% sodium% Potassium % Sulfate % Crude sodium nitrate 0.05 28.02 0.86 0.038 Crude potassium nitrate 0.08 0.91 35.923 0.0654 High-purity sodium nitrate 0.001 26.708 0.391 0.0241 High-purity potassium nitrate 0.002 0.294 36.547 0.0152

[0073] This embodiment:

[0074] Traditional methods for separating potassium nitrate (KNO3) and sodium nitrate (NaNO3) rely on the temperature-dependent differences in their solubility (e.g., evaporation, concentration, crystallization, or cooling crystallization). However, when the solubility difference between the two salts is small (e.g., potassium nitrate and sodium nitrate have similar solubilities at room temperature), traditional methods have low separation efficiency, high energy consumption, and questionable purity. The alcohol precipitation method, on the other hand, reduces the polarity of the aqueous solution by introducing alcohol solvents (e.g., ethanol, methanol, etc.), and utilizes the significant difference in solubility of the two nitrates in the alcohol-water mixture to achieve efficient separation. Solvent alcohols can be recovered and reused through distillation.

[0075] Evaporation and concentration crystallization: By heating and concentrating the solution, salts with lower solubility (such as sodium nitrate) are preferentially precipitated. However, the solubility of potassium nitrate and sodium nitrate varies slightly with temperature (especially in the medium and low temperature range), resulting in incomplete separation and the need for multiple recrystallizations, high energy consumption, and low yield.

[0076] Cooling crystallization: Suitable for substances such as potassium nitrate whose solubility changes significantly with temperature, but it has poor separation effect on sodium nitrate and requires long-term temperature control, resulting in low efficiency;

[0077] The basic scheme of the present invention is an alcohol precipitation method + saturated nitrate solution washing. This method can filter out most of the potassium nitrate after the alcohol precipitation method. Secondly, from the perspective of energy consumption, it avoids the high energy consumption conditions brought about by high-temperature concentration + cooling crystallization to separate potassium nitrate. The filtrate obtained after the alcohol precipitation method is evaporated and concentrated to obtain sodium nitrate. The sodium nitrate and potassium nitrate can reach more than 95%, and then they are washed with corresponding saturated solutions to achieve a purity of more than 99%.

[0078] Second embodiment:

[0079] See also Figure 1 、 Figure 2 、 Figure 11 and Figure 12 , the processing equipment for the mixed mother liquor of ethanol and water also includes a base 5, a distillation mechanism 6 and a dosing mechanism 7, the distillation mechanism 6 includes a water bath 61 placed on the upper surface of the base 5, the interior of the water bath 61 is installed with an electric heating tube 69, the top of the water bath 61 is installed with a sealing plate 62 by bolts, the axis of the sealing plate 62 is integrated with a distillation barrel 63, the top of the distillation barrel 63 is installed with an end cover 64 by bolts, the interior of the end cover 64 is penetrated by an injection pipe 65, a discharge pipe 66 and a distillation pipe 67, the outer wall of the distillation pipe 67 is installed with a condenser 68, and the interior of the water bath 61 is installed with an exhaust mechanism 8.

[0080] See also Figure 11 and Figure 12 In step S7 of the first embodiment, the end cap 64 and the distillation barrel 63 need to be sealed and installed before distillation. After installation, clean water needs to be added to the water bath 61 (the water level cannot be higher than the exhaust mechanism 8). Then, the entire distillation barrel 63 needs to be placed inside the water bath 61 and the electric heating tube 69 needs to be passed through.

[0081] In step S7 of the first embodiment, the generated ethanol-water mother liquor mixture is injected into the distillation barrel 63 through the injection pipe 65 (the amount of the ethanol-water mother liquor mixture does not exceed 2 / 3 of the capacity of the distillation barrel 63). The user then controls the temperature inside the water bath 61 by heating the electric heating pipe 69 to heat the distillation barrel 63 (slowly raising the temperature to 78.3°C, the boiling point of ethanol, and controlling the temperature to avoid violent boiling. Zeolite may be added).

[0082] The ethanol produced by distillation will enter the curved distillation tube 67, and the outer wall of the distillation tube 67 will be cooled by the condenser 68, so that the distilled ethanol will be condensed into liquid for recovery. Finally, the inside of the distillation barrel 63 is the residual waste liquid without ethanol. The residual waste liquid inside the distillation barrel 63 can be extracted through the discharge pipe 66 and stored centrally for subsequent treatment.

[0083] The exhaust mechanism 8 includes an exhaust pipe 82 fixed on the inner wall of the water bath tub 61. A fixed pipe 81 is fixed inside the water bath tub 61 and at the air outlet end of the exhaust pipe 82. The inner wall of the fixed pipe 81 is provided with two slide grooves 83. The inside of the two slide grooves 83 is slidably connected with a sliding pipe 84. The outer wall of the sliding pipe 84 is provided with a through hole 85.

[0084] See also Figure 12 and Figure 13 In order to ensure a stable pressure inside the distillation barrel 63, an exhaust mechanism 8 is usually provided. Since a large amount of steam is generated inside the water bath 61 when it is heated, the internal pressure will be too high, and the steam generated will push the sliding tube 84 upward;

[0085] See also Figure 13 (a): In the initial state, the through hole 85 and the exhaust pipe 82 are separated, so the interior of the entire water bath 61 is sealed and the internal and external pressures are balanced;

[0086] 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. 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. During the sliding, the through hole 85 will intersect with the inner hole of the exhaust pipe 82. 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.

[0087] It is understandable that since the chute 83 is not a through-groove design, when the temperature inside the water bath 61 drops and the pressure remains constant, the sliding tube 84 will automatically return to its initial state.

[0088] In this embodiment, a water bath heating method is used to distill the ethanol-water mixed mother liquor. The heating is stable and the ethanol can be well distilled and precipitated, which can fully realize the recovery and reuse of ethanol. 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 internal and external pressure balance 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.

[0089] Third embodiment:

[0090] See also Figures 1 to 10 and Figure 14 , including a flocculation box 1, a flocculation frame 9 and a driving mechanism 3;

[0091] The top of the flocculation frame 9 is fixed with a mounting plate 2 by bolts. The driving mechanism 3 includes a mounting frame 31 mounted 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 inside the mounting frame 31 and between the top plate 32 and the bottom plate 33 by bolts. The top output shaft keyway of the double-headed motor 34 is connected to a first ratchet 35. The outer wall of the first ratchet 35 is meshed with a first ratchet ring 36. The outer wall keyway of the first ratchet ring 36 is connected to a cam 37.

[0092] The bottom output shaft keyway of the double-headed motor 34 is connected to a second ratchet 38 , the outer wall of the second ratchet 38 is meshed with a second ratchet ring 39 , and the bottom of the second ratchet ring 39 is integrally provided with a first pulley 310 ;

[0093] Please refer to Figure 1 and Figure 2 : Through the process of the second embodiment, residual waste liquid without ethanol will be generated. When the waste liquid collected meets the carrying capacity of the flocculation box 1, the user needs to add waste liquid into the flocculation box 1 through the flocculation frame 9 for flocculation treatment;

[0094] See also Figures 3 to 5 Starting the double-headed motor 34 can control the upper and lower ends of the double-headed motor 34 to rotate freely clockwise or counterclockwise. Since the helical teeth of the first ratchet 35 and the second ratchet 38 are set in different directions, when the double-headed motor 34 rotates clockwise, the second ratchet 38 will rotate clockwise inside the second ratchet ring 39, thereby forming an avoidance to ensure that the second ratchet 38 does not affect the rotation of the second ratchet ring 39. The clockwise rotating first ratchet 35 will affect the control of the first ratchet ring 36 to drive the outer cam 37 to rotate synchronously clockwise;

[0095] If it rotates counterclockwise, the cam 37 will not rotate, and the second ratchet wheel 38 at the bottom of the double-headed motor 34 will drive the second ratchet ring 39 and the first pulley 310 to rotate counterclockwise.

[0096] A flocculation mechanism 4 is installed inside the flocculation frame 9, and the flocculation mechanism 4 includes a rotating rod 41 fixedly provided at the axis of the first pulley 310 and connected by a keyway. The outer wall of the rotating rod 41 is fixedly provided with support rods 42 distributed equidistantly in an annular shape. A toothed ring 43 is installed on the inner wall of the flocculation frame 9, and two gears 45 are meshed and connected to the upper part of the toothed ring 43. A mounting block 44 is fixedly provided at the bottom end of the rotating rod 41, and flocculation plates 46 are rotatably connected on both sides of the mounting block 44.

[0097] See also Figure 4 and Figure 14: When 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 outside 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.

[0098] 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. An inner wall of the flocculation box 1 and located on the right side of the partition 20 is rotatably connected with an equidistantly arranged inclined plate 12. 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. 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. A slider 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. 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. Limiting rods 21 are fixedly provided on the front and rear ends above the plurality of inclined plates 12. A liquid outlet pipe 10 is installed on the side wall of the flocculation box 1.

[0099] 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.

[0100] 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 .

[0101] 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. Due to the different densities of the flocs and the liquid, 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;

[0102] 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 before it can be discharged;

[0103] The small floccules at the bottom will surge upwards, and the multiple inclined plates 12 can block and capture the small floccules that surge upwards;

[0104] Please refer again Figure 10 When the cam 37 rotates clockwise, the long end of the cam 37 will resist the guide wheel 19 and move to the right. The guide wheel 19 can control the top rod 18 and the vertical rod 17 to control the connecting plate 14 to realize that multiple linkage plates 13 drive the corresponding limiting rods 21 to control the corresponding inclined plates 12 to flip clockwise inside the flocculation box 1 to change the inclination of the inclined plates 12.

[0105] See also Figure 7 and Figure 8 : Each limiting rod 21 and the linkage plate 13 are fitted with a restriction, so that when the linkage plate 13 moves left and right, the limiting rod 21 can be controlled to slide along the vertical direction of the linkage plate 13, so that when the linkage plate 13 moves, the inclined plate 12 can be smoothly flipped to avoid interference.

[0106] At the same time, elastic sliding is adopted between the connecting plate 14 and the flocculation box 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 after being turned over.

[0107] In this embodiment, the upper and lower output shafts of the double-headed motor 34 can rotate in a zoned manner. When the double-headed motor 34 rotates clockwise, the cam 37 rotates. When the double-headed motor 34 rotates counterclockwise, the first pulley 310 rotates.

[0108] When the first pulley 310 rotates, the rotating rod 41 can be controlled to realize the coordinated rotation of the support rod 42 and the flocculation plate 46. Since the rotation direction of the support rod 42 is horizontal, and the rotation direction of the flocculation plate 46 is vertical, the flocculant and the waste liquid can be pre-mixed by the support rod 42 first, and then when the mixed liquid enters the flocculation plate 46, the mixed liquid falling on the flocculation plate 46 will be mixed for the second time 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 mixed in an irregular rotation, thereby ensuring sufficient mixing, improving the flocculation effect, and avoiding uneven distribution of the flocculant.

[0109] At the same time, during the flocculation process, equidistantly arranged inclined plates 12 are provided to ensure that large flocculants can be settled inside the flocculation box 1. During the overflow and drainage process, the internal water body of the flocculation box 1 will change, and the small flocculants will surge upward. Initially, the inclined plates 12 with a large slope can block and capture the flocculants surging upward, preventing the flocculants from overflowing with the water flow through the inclined plates 12. At the same time, the linkage plates 13 can be used to control the linkage and synchronous flipping of multiple inclined plates 12 to change the slope to make it smaller. In this way, the flocculants captured on the inclined plates 12 can be shaken and precipitated downward to avoid congestion of the flocculants, ensuring 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 and reuse.

[0110] Fourth embodiment:

[0111] A positioning frame 22 is fixedly provided on the upper surface of the base 5 and located on one side of the water bath 61, a condensation box 24 is installed inside the positioning frame 22, a card plate 23 is fixedly provided on the outer wall of the positioning frame 22, and the dosing mechanism 7 includes a side plate 71 fixedly provided on the side wall of the flocculation box 1 and located below the card plate 23, the top of the side plate 71 is rotatably connected to the second pulley 72, the outer walls of the first pulley 310 and the second pulley 72 are sleeved with a belt 311, a mixing cylinder 73 is fixedly provided on the inner wall of the card plate 23, a screw rod 74 is connected to the keyway at the axis of the second pulley 72, a dosing tube 75 is installed on the top of the mixing cylinder 73, and an oblique drug discharge tube 76 is installed below the mixing cylinder 73.

[0112] The two sides of the sliding tube 84 are slidingly connected to the two sliding grooves 83 through blocks, and the upper and lower ends of the spiral rod 74 are rotatably connected to the mixing cylinder 73 through bearings. The exhaust pipe 82 and the top of the condensation box 24 are sealed and installed, and the bottom of the condensation box 24 is sealed and installed with the side wall of the mixing cylinder 73.

[0113] Please refer to 3. Figure 4 、 Figure 11 and Figure 15 During the operation of the second embodiment, the steam generated when the water bath 61 is heated is discharged into the condensation box 24 through the exhaust mechanism 8, and the steam is condensed in the condensation box 24 to form distilled water which is stored in the condensation box 24;

[0114] 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 drum 73. At this time, PAM type flocculation powder (other powder type flocculants can be used) can be added to the mixing drum 73 through the dosing tube 75. The distilled water inside the condensation box 24 will enter the mixing drum 73. When the screw rod 74 rotates, the distilled water and 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.

[0115] In this embodiment, the distillation process and the water treatment process are linked and combined. 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. It can not only be used for experimental water, but also can be connected with the mixing barrel 73. When the flocculation mechanism 4 is rotating, 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 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 and is derived from recycled water, which can be more environmentally friendly.

[0116] 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 transformations made by using the contents of the present invention description and drawings under the concept of the present invention, or direct / indirect application in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. A treatment device for a mixed mother liquor of ethanol and water, characterized in that: It includes a flocculation box, a flocculation frame and a driving mechanism; The top of the flocculation frame is mounted with a mounting plate by bolts, and the driving mechanism includes a mounting bracket mounted on the upper surface of the mounting plate, the inner walls of the mounting bracket are respectively fixed with a top plate and a bottom plate, a double-headed motor is mounted inside the mounting bracket and between the top plate and the bottom plate by bolts, the top output shaft keyway of the double-headed motor is connected to a first ratchet, the outer wall of the first ratchet is meshed with a first ratchet ring, and the outer wall keyway of the first ratchet ring is connected to a cam; The bottom output shaft keyway of the double-headed motor is connected to a second ratchet wheel, the outer wall of the second ratchet wheel is meshedly connected to a second ratchet ring, and the bottom of the second ratchet ring is integrally provided with a first pulley; The inner wall of the flocculation box is fixedly provided with a partition on one side of the flocculation frame, the inner wall of the flocculation box is located on the right side of the partition and is rotatably connected to an equidistantly arranged inclined plate, the inner wall of the flocculation box is located above the inclined plate and is fixedly provided with a limit plate, the inner side of the limit plate is slidably connected to a plurality of linkage plates, the tops of the plurality of linkage plates are fixedly provided with a connecting plate, the outer wall of the flocculation box is fixedly provided with a groove plate, the side walls of the connecting plate are fixedly provided with a sliding block, the top of the connecting plate is fixedly provided with a vertical rod, the top of the vertical rod is fixedly provided with a push rod, the middle position of the push rod is installed with a guide wheel, the front and rear ends above the plurality of inclined plates are fixedly provided with limiting rods, and the side walls of the flocculation box are installed with a liquid outlet pipe; The outer wall of the guide wheel is in contact with the outer wall of the cam, the slider is horizontally slidably connected to the slot plate through a spring, and the outer walls on both sides of the limiting rod are in contact with the inner walls on both sides of the linkage plate; It also includes a base, a distillation mechanism and a dosing mechanism, the distillation mechanism includes a water bath placed on the upper surface of the base, an electric heating tube is installed inside the water bath, a sealing plate is installed on the top of the water bath by bolts, a distillation barrel is integrally provided at the axis of the sealing plate, an end cover is installed on the top of the distillation barrel by bolts, an injection pipe, a discharge pipe and a distillation pipe are installed inside the end cover, a condenser is installed on the outer wall of the distillation pipe, and an exhaust mechanism is installed inside the water bath; The exhaust mechanism includes an exhaust pipe fixed on the inner wall of the water bath tub, a fixed pipe is fixed inside the water bath tub and at the air outlet end of the exhaust pipe, the inner wall of the fixed pipe is provided with two sliding grooves, the interior of the two sliding grooves is slidably connected with a sliding pipe, and the outer wall of the sliding pipe is provided with a through hole.

2. The processing equipment for the mixed mother liquor of ethanol and water 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, and the outer wall of the second ratchet ring is rotatably connected to the bottom plate through a bearing.

3. The processing equipment for the mixed mother liquor of ethanol and water according to claim 1, characterized in that: A flocculation mechanism is installed inside the flocculation frame, and the flocculation mechanism includes a rotating rod fixed at the axis of the first pulley connected by a keyway, and the outer wall of the rotating rod is fixed with support rods distributed equidistantly in an annular shape. A toothed ring is installed on the inner wall of the flocculation frame, and two gears are meshed and connected to the upper part of the toothed ring. A mounting block is fixed at the bottom end of the rotating rod, and flocculation plates are rotatably connected on both sides of the mounting block.

4. The processing equipment for the mixed mother liquor of ethanol and water according to claim 3, characterized in that: The axes of the two flocculation plates are fixedly connected to the axes of the two gears, and the outer wall of the rotating rod is rotatably connected to the mounting plate through a bearing.

5. The processing equipment for the mixed mother liquor of ethanol and water according to claim 1, characterized in that: A positioning frame is fixedly provided on the upper surface of the base and located on one side of the water bath, a condensation box is installed inside the positioning frame, a card plate is fixedly provided on the outer wall of the positioning frame, the dosing mechanism includes a side plate fixedly provided on the side wall of the flocculation box and located below the card 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 provided on the inner wall of the card plate, a spiral rod is connected to the keyway at the axis of the second pulley, a dosing tube is installed on the top of the mixing cylinder, and an oblique medicine discharge tube is installed below the mixing cylinder.

6. The processing equipment for the mixed mother liquor of ethanol and water according to claim 5, characterized in that: The two sides of the sliding tube are slidably connected to the two sliding grooves through blocks, the upper and lower ends of the spiral rod are rotatably connected to the mixing cylinder through bearings, the exhaust pipe and the top of the condensation box are sealed, and the bottom of the condensation box is sealed to the side wall of the mixing cylinder.

7. A method for purifying sodium nitrate and potassium nitrate, characterized in that: The method for purifying sodium nitrate and potassium nitrate comprises the processing equipment for the mixed mother liquor of ethanol and water according to any one of claims 1 to 6, comprising the following steps: S1: preparing to mix sodium nitrate and potassium nitrate, and mechanically stirring 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 from S2 to a thermostatic water bath reactor, control the temperature at 25°C, and slowly add ethanol dropwise at a ratio of 1:0.5-1 of solution mass to anhydrous ethanol mass, while continuously stirring at 200 rpm. Continue stirring for ten minutes after the addition of ethanol, then let it stand at 5°C-50°C for 30 minutes to precipitate a white flocculent potassium nitrate precipitate; S4: vacuum filtration is performed on the mixed system after standing in S3 to separate the crude potassium nitrate solid and the filtrate containing sodium nitrate; S5: The filtrate obtained in S4 was transferred to a rotary evaporator and concentrated under reduced pressure at 80°C and -0.09 MPa to evaporate 70%-90% of the original volume. The remaining concentrated solution was cooled to 10°C to precipitate sodium nitrate crystals, which were filtered to obtain crude sodium nitrate solid; 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 for 20 minutes, filtering and drying to obtain high-purity potassium nitrate crystals; adding the crude sodium nitrate obtained in S5 to a saturated aqueous solution of sodium nitrate at 40° C. at a solid-liquid mass ratio of 1:0.5-2, stirring at 200 rpm for 15 minutes, filtering, and drying to obtain high-purity sodium nitrate crystals; 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 it in conjunction with the treatment equipment of the ethanol and water mixed mother liquor.

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