Perchloric acid rectification device
By using a jacket structure and water as the heating medium in the perchloric acid distillation unit, combined with a safety valve to control the steam pressure, the problem of unstable temperature during the perchloric acid distillation process was solved, achieving safe, controllable, and efficient production.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SHANDONG HENGHUA NEW MATERIAL CO LTD
- Filing Date
- 2025-04-29
- Publication Date
- 2026-04-28
AI Technical Summary
In the existing technology, the temperature control during the distillation of perchloric acid is unstable, which poses a risk of high temperature or local overheating, especially when distilling high-concentration perchloric acid, leading to unsafe production.
The perchloric acid distillation apparatus with a jacket structure uses water as the heating medium and controls the temperature inside the distillation vessel through heat conduction within the jacket. A safety valve is installed at the gas phase position of the jacket to limit the vapor pressure and ensure that the temperature is always below the explosion temperature of perchloric acid.
This achieves controllable temperature control inside the distillation vessel, avoids localized overheating, reduces the risk of explosion, and ensures safe and efficient temperature control in production.
Smart Images
Figure CN224166923U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of perchloric acid purification technology, and in particular to a perchloric acid distillation apparatus. Background Technology
[0002] Perchloric acid is a strong inorganic oxidizing agent that reacts rapidly with organic matter, and is therefore commonly used as a disinfectant and bleaching agent. Its oxidizing properties promote the synthesis of complex organic compounds, providing crucial support for the development of the chemical industry. The purity of perchloric acid directly affects reaction efficiency, safety, the accuracy of experimental results, and product quality; therefore, purification is essential.
[0003] Because pure perchloric acid is very unstable, its purification is extremely dangerous. When heated to temperatures above 130°C, perchloric acid becomes a strong oxidizing agent and eventually becomes unstable. For continuous purification of perchloric acid, the temperature must be controlled to remain well below its boiling point.
[0004] In the existing technology, the purification of perchloric acid usually adopts conventional vacuum distillation, which takes advantage of the difference in boiling points between perchloric acid and impurities to purify it by distillation under reduced pressure (lowering the boiling point).
[0005] However, this method has certain drawbacks. Regardless of whether the heating medium is direct electric heating or heat transfer oil heating, there is a risk of high temperature or localized overheating leading to decomposition, especially when distilling high-concentration (>72.5%) perchloric acid, which can cause production safety issues. Therefore, it requires high-quality equipment and strict temperature control. Enhancing the stability and controllability of the heating medium is crucial for the perchloric acid distillation process. Utility Model Content
[0006] The technical problem to be solved by this utility model is to provide a perchloric acid distillation device that can produce safely, so as to solve the problems of high temperature control requirements and unstable heating medium in the existing technology of perchloric acid distillation.
[0007] To solve the above-mentioned technical problems, the present invention provides the following technical solution:
[0008] A perchloric acid distillation apparatus includes a distillation vessel and a jacket fitted around the outside of the distillation vessel. The distillation vessel has a feed port and a condensation recovery port at the top and a discharge recovery port at the bottom.
[0009] The jacket contains a heating medium and a heating device for heating the heating medium to make it boil. The heating medium is water. The jacket is provided with a first water inlet. A safety valve is provided at the gas phase position of the jacket. The opening pressure of the safety valve is 0.105MPa-0.12MPa.
[0010] Furthermore, the heating device is a plurality of electric furnaces that are evenly inclined and placed at the bottom of the jacket;
[0011] Alternatively, the heating device may be a spiral heating coil disposed at the bottom of the jacket.
[0012] Furthermore, the heating medium is treated water that meets the requirements for boiler feedwater;
[0013] And / or, the distillation vessel is equipped with a thermometer;
[0014] And / or, the distillation vessel is equipped with a pressure gauge.
[0015] Furthermore, a level gauge is provided on the jacket;
[0016] And / or, the jacket is equipped with a thermometer;
[0017] And / or, the jacket is equipped with a pressure gauge.
[0018] Furthermore, the jacket is equipped with a pressure relay at the gas phase position. When the steam pressure inside the jacket reaches a preset threshold, the pressure relay will interlock and cut off the power supply to the heating device and trigger an alarm. The preset threshold is 0.08 MPa-0.10 MPa.
[0019] Furthermore, the jacket is provided with an L-shaped partition, which includes a vertical plate portion surrounding the outside of the distillation vessel and a horizontal plate portion extending outward from the lower end of the vertical plate portion and connecting to the inside of the jacket. The horizontal plate portion is provided with several through holes. A second water inlet is provided through the jacket, which communicates with the vertical plate portion and the distillation vessel. The first water inlet communicates with the vertical plate portion and the jacket. The lower end of the jacket is provided with a drain outlet.
[0020] Furthermore, the perchloric acid distillation apparatus also includes a three-way valve interlocked and controlled by the pressure relay. The inlet of the three-way valve is connected to a water source, and the two outlets of the three-way valve are respectively connected to the first water inlet and the second water inlet. When the pressure relay is not triggered, the inlet of the three-way valve is connected to the first water inlet. When the pressure relay is triggered, the inlet of the three-way valve is connected to the second water inlet, and the drain outlet is opened at the same time.
[0021] Furthermore, the lower part of the vertical plate is provided with several through holes;
[0022] And / or, the vertical plate portion is fixed to the sleeve by a connecting rod.
[0023] Furthermore, the distillation vessel is equipped with stirring blades;
[0024] And / or, the heat exchange surface of the distillation vessel is provided with fins.
[0025] Furthermore, the distillation vessel is equipped with a mist separator at the condensate recovery port.
[0026] This utility model has the following beneficial effects:
[0027] This utility model relates to a perchloric acid distillation apparatus, comprising a distillation vessel and a jacket surrounding the distillation vessel. Water is used as the heating medium. Through heat conduction between hot water and steam, the temperature inside the distillation vessel is kept consistently below the temperature of the hot water and steam within the jacket. Using water as the heat transfer medium prevents localized overheating, achieving controllable temperature control within the distillation vessel during actual operation and ensuring production safety. A safety valve is installed at the vapor phase position of the jacket. The safety valve's opening (steam) pressure is 0.105MPa-0.12MPa. By controlling the steam pressure of saturated steam, and through continuous heat conduction between steam and hot water within the jacket, the temperature inside the vessel is maintained below 120℃. This controls the distillation temperature within the vessel, ensuring it remains below the explosion temperature of perchloric acid and minimizing the risk of explosion. Attached Figure Description
[0028] Figure 1 This is a schematic diagram of the overall structure of an embodiment of the perchloric acid distillation apparatus of this utility model;
[0029] Figure 2 This is a partial structural schematic diagram of an improved embodiment of the perchloric acid distillation apparatus of this utility model. Detailed Implementation
[0030] To make the technical problems, technical solutions and advantages of this utility model clearer, a detailed description will be given below in conjunction with the accompanying drawings and specific embodiments.
[0031] In the description of this utility model, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.
[0032] This utility model provides a perchloric acid distillation apparatus, such as... Figure 1 As shown, it includes a distillation vessel 2 and a jacket 1 fitted outside the distillation vessel 2. The upper part of the distillation vessel 2 is provided with a feed port 21 and a condensation recovery port 22 (distilled gas is returned to condensation recovery). The lower part of the distillation vessel 2 is provided with a discharge recovery port 23 (discharge is returned to recovery).
[0033] The jacket 1 contains a heating medium 11 and a heating device 12 for heating the heating medium 11 to boiling. The heating medium 11 is water. The jacket 1 is provided with a first water inlet 13. A safety valve 14 (specifically, a double safety valve) is provided at the gas phase position of the jacket 1. The opening pressure of the safety valve 14 is 0.105MPa-0.12MPa (gauge pressure). The opening pressure of the safety valve 14 can be 0.105MPa, 0.11MPa, 0.115MPa, etc., preferably 0.11MPa. This can improve heating efficiency and ensure safe production.
[0034] In operation, crude perchloric acid is first added to the distillation vessel 2 through the feed port 21 using a raw material pump. Then, heating medium 11 (i.e., water) is added to the jacket 1, and the temperature and pressure are increased. The heating medium 11 is then controlled at a constant level and evaporation pressure to maintain a constant temperature between the gas and liquid phases, continuously providing heat to the distillation vessel 2. Because the jacket 1 is a closed structure, the internal steam pressure increases with the increase in heat. When the internal steam pressure reaches the tripping pressure of the safety valve 14, the safety valve 14 trips, releasing the internal steam pressure and ensuring safe production.
[0035] This utility model relates to a perchloric acid distillation apparatus, comprising a distillation vessel and a jacket surrounding the vessel. Water is used as the heating medium. Through heat conduction between the hot water and steam, the temperature inside the distillation vessel is consistently kept below the temperature of the hot water and steam within the jacket. Using water as the heat transfer medium prevents localized overheating, achieving controllable temperature control within the distillation vessel during operation and ensuring production safety. A safety valve is installed at the vapor phase position of the jacket, with a tripping pressure of 0.105 MPa-0.12 MPa (gauge pressure). By controlling the steam pressure of saturated steam, continuous heat conduction between the steam and hot water within the jacket maintains the temperature inside the vessel below 120°C, thereby controlling the distillation temperature and ensuring it remains below the explosion temperature of perchloric acid, thus minimizing the risk of explosion.
[0036] The heating device 2 can take various structural forms that are readily conceived by those skilled in the art. This utility model provides the following two structural forms:
[0037] Structural Form 1
[0038] The heating device 12 can be several electric furnaces (such as those evenly tilted at the bottom of the jacket 1) Figure 1 (As shown). This ensures smooth liquid circulation within the jacket, complete boiling without dead zones, and uniform temperature throughout the vessel.
[0039] Structural Form Two
[0040] The heating device 12 can be a spiral heating coil (not shown) located at the bottom of the jacket 1. The spiral structure of the coil improves the heating efficiency.
[0041] To enhance heat transfer, the heating medium 11 can be treated water that meets the requirements of boiler feedwater, specifically demineralized water. In this way, demineralized water will not produce scale during the heating process, thus not reducing the heat transfer effect.
[0042] The distillation vessel 2 can be equipped with a thermometer 24 and a pressure gauge 25 to facilitate direct observation of the temperature and pressure of the distillation vessel 2.
[0043] To facilitate observation of the remaining water level in jacket 1, a level gauge 15 (specifically, a local and / or remote level gauge) can be installed on jacket 1 to achieve automatic water inlet control of the liquid level in the jacket. An automatic alarm will sound when the liquid level is too high or too low. A thermometer 16 can be installed on jacket 1. The thermometer 16 may include a platinum resistance remote thermometer and a bimetallic local display thermometer. These two thermometers are cross-referenced, and the heating power supply will be interlocked and stopped when the measured temperature exceeds the target value (i.e., 120℃). A pressure gauge 17 can also be installed on jacket 1 for direct observation of the pressure within jacket 1.
[0044] A pressure relay (not shown) can be installed at the gas phase position of jacket 1. When the steam pressure inside jacket 1 reaches a preset threshold, the pressure relay will interlock and cut off the power supply to heating device 12 and trigger an alarm. The preset threshold is 0.08MPa-0.10MPa (gauge pressure), for example, it can be 0.08MPa, 0.09MPa, 0.10MPa, etc., and can be flexibly set according to user needs. In this way, even if the steam pressure inside jacket 1 accidentally reaches the preset threshold due to a malfunction, production safety can still be guaranteed.
[0045] like Figure 2 As shown, in the improved embodiment of this utility model, in order to enable the pressure relay to cool down the distillation vessel 2 quickly and promptly after triggering to ensure safe production, preferably, the jacket 1 is provided with an L-shaped partition 3. The L-shaped partition 3 includes a vertical plate portion 31 surrounding the outside of the distillation vessel 2 and a horizontal plate portion 32 extending outward from the lower end of the vertical plate portion 31 and connecting to the inside of the jacket 1. The horizontal plate portion 32 is provided with several through holes (not shown) to allow the inner and outer sides of the L-shaped partition 3 to communicate. A second water inlet 18 is provided through the jacket 1, connecting the vertical plate portion 31 and the distillation vessel 2. A first water inlet 13 is connected between the vertical plate portion 31 and the jacket 1. The lower end of the jacket 1 is provided with a drain outlet 19.
[0046] During initial water addition, water can be added to the jacket 1 through the first water inlet 13 and / or the second water inlet 18 to improve water addition efficiency. During replenishment, water can be added to the jacket 1 through only the first water inlet 13. Since the first water inlet 13 connects to the vertical plate 31 and the jacket 1, the newly added water enters the space between the vertical plate 31 and the jacket 1 without affecting the temperature of the water between the vertical plate 31 and the distillation vessel 2, thus ensuring production efficiency. If the pressure relay is triggered (i.e., an emergency occurs), water is added to the jacket 1 through the second water inlet 18, and the drain outlet 19 at the lower end of the jacket 1 is opened at the same time. The opening of the drain outlet 19 and the presence of the L-shaped baffle 3 allow the water between the vertical plate 31 and the distillation vessel 2 to be released first, and the newly added water quickly enters the space between the vertical plate 31 and the distillation vessel 2. Compared to directly draining and adding water to the jacket 1 without the L-shaped baffle 3, the newly added water can come into direct contact with the reaction vessel 2 more quickly, achieving rapid cooling and improving the cooling effect.
[0047] For ease of use, the perchloric acid distillation unit may also include a three-way valve 4 interlocked with a pressure relay. The inlet 41 of the three-way valve 4 is connected to a water source (not shown), and the two outlets 42 and 43 of the three-way valve 4 are connected to the first water inlet 13 and the second water inlet 18, respectively. When the pressure relay is not triggered (i.e., the steam pressure in the jacket 1 has not reached the preset threshold), the inlet 41 of the three-way valve 4 is connected to the first water inlet 13. When the pressure relay is triggered (i.e., the steam pressure in the jacket 1 reaches the preset threshold), the inlet 41 of the three-way valve 4 is connected to the second water inlet 18, and the drain outlet 19 is opened simultaneously. In this way, when the steam pressure / temperature in the jacket 1 is too high, causing the pressure relay to be triggered, the distillation kettle 2 can be directly cooled, ensuring production safety.
[0048] The lower part of the vertical plate 31 may be provided with several through holes (not shown), which allows the two sides of the L-shaped partition 3 to be connected without affecting the normal heating of the water in the jacket 1. The vertical plate 31 can be fixed to the jacket 2 by a connecting rod (not shown), which facilitates and securely fixes the L-shaped partition 3.
[0049] To ensure uniform heating of the crude perchloric acid in distillation vessel 2, stirring blades (not shown) may be installed inside distillation vessel 2. Fins (not shown) may be installed on the heat exchange surface of distillation vessel 2, thereby enhancing heat transfer in distillation vessel 2 and improving production efficiency.
[0050] To improve production efficiency, the liquid level in the distillation kettle can be increased to increase the heat transfer area. However, this reduces the gas phase space inside the kettle and the distance between the boiling liquid surface and the recovery port. This makes it easier for the mist and droplets generated during boiling to be carried out to subsequent equipment, affecting the quality of the refined product. Therefore, a mist separator (not shown) is preferably installed inside the distillation kettle 2 at the condensation recovery port 22 to ensure product quality while improving production efficiency.
[0051] In summary, the principle of this utility model is as follows:
[0052] Perchloric acid solution is distilled under reduced pressure (absolute pressure less than 50 mmHg) at approximately 110°C, evaporating and condensing to obtain a perchloric acid solution with a mass concentration of approximately 70%. At 110°C, the vapor pressure is 0.045 MPa (gauge pressure), which is sufficient for distilling the perchloric acid solution.
[0053] Since the vapor pressure of saturated steam is directly proportional to its temperature, when the vapor pressure is controlled at 0.11 MPa (gauge pressure), the saturated vapor pressure inside the jacket is 120°C. At this point, the gas-liquid phase temperature inside the jacket remains constant, which is a safe distance from the explosion temperature of perchloric acid (130°C). Simultaneously, the jacket temperature is higher than the boiling point of the azeotrope of the perchloric acid solution in the reactor under reduced pressure, thus meeting the requirements for heat transfer and providing evaporation heat energy. At this point, the gas-liquid phase temperature inside the jacket remains consistent, not exceeding 120°C, and the gas and liquid phases continuously maintain a boiling state. By controlling the vapor pressure, through continuous heat conduction between the steam and hot water inside the jacket, the temperature inside the reactor is maintained at approximately 110°C and below 120°C. This controls the distillation temperature inside the reactor, ensuring it remains below the explosion temperature of perchloric acid and avoiding the risk of explosion.
[0054] This invention achieves the purpose of controlling the distillation temperature inside the vessel by setting and limiting the saturated vapor pressure within the jacket to a constant value using a safety valve. Compared with existing technologies, it improves upon the phenomenon of localized overheating that occurs with other media (such as direct electric heating or heat transfer oil heating).
[0055] This utility model has the following beneficial effects:
[0056] (1) Limit the starting pressure by using the jacket safety valve to ensure that the temperature inside the jacket is within the target range.
[0057] (2) The heat transfer of hot water and steam in the jacket has a good effect on the heat transfer of different positions in the distillation vessel, ensuring the consistency of the temperature inside the vessel and preventing local overheating. Moreover, the temperature inside the vessel is always lower than the temperature inside the jacket, reducing the risk of explosion.
[0058] (3) Since the steam pressure of saturated steam is related to the temperature, the temperature can be strictly controlled by controlling the steam pressure. This makes it highly operable and controllable.
[0059] The above description is the preferred embodiment of this utility model. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of this utility model, and these improvements and modifications should also be considered within the protection scope of this utility model.
Claims
1. A perchloric acid distillation apparatus, characterized in that, It includes a distillation vessel and a jacket fitted outside the distillation vessel. The distillation vessel is provided with a feed port and a condensation recovery port at the top and a discharge recovery port at the bottom. The jacket contains a heating medium and a heating device for heating the heating medium to make it boil. The heating medium is water. The jacket is provided with a first water inlet. A safety valve is provided at the gas phase position of the jacket. The opening pressure of the safety valve is 0.105MPa-0.12MPa.
2. The perchloric acid distillation apparatus according to claim 1, characterized in that, The heating device consists of several electric furnaces that are evenly tilted and placed at the bottom of the jacket; Alternatively, the heating device may be a spiral heating coil disposed at the bottom of the jacket.
3. The perchloric acid distillation apparatus according to claim 1, characterized in that, The heating medium is treated water that meets the requirements for boiler feedwater; And / or, the distillation vessel is equipped with a thermometer; And / or, the distillation vessel is equipped with a pressure gauge.
4. The perchloric acid distillation apparatus according to claim 1, characterized in that, The jacket is equipped with a level gauge; And / or, the jacket is equipped with a thermometer; And / or, the jacket is equipped with a pressure gauge.
5. The perchloric acid distillation apparatus according to any one of claims 1-4, characterized in that, The jacket is equipped with a pressure relay for the gas phase position. When the steam pressure in the jacket reaches a preset threshold, the pressure relay will interlock and cut off the power supply to the heating device and trigger an alarm. The preset threshold is 0.08 MPa-0.10 MPa.
6. The perchloric acid distillation apparatus according to claim 5, characterized in that, The jacket is provided with an L-shaped partition, which includes a vertical plate portion surrounding the outside of the distillation vessel and a horizontal plate portion extending outward from the lower end of the vertical plate portion and connecting to the inside of the jacket. The horizontal plate portion is provided with several through holes. A second water inlet is provided through the jacket, which connects to the vertical plate portion and the distillation vessel. The first water inlet is connected to the vertical plate portion and the jacket. The lower end of the jacket is provided with a drain outlet.
7. The perchloric acid distillation apparatus according to claim 6, characterized in that, The perchloric acid distillation apparatus also includes a three-way valve controlled by the pressure relay. The inlet of the three-way valve is connected to a water source, and the two outlets of the three-way valve are respectively connected to the first water inlet and the second water inlet. When the pressure relay is not triggered, the inlet of the three-way valve is connected to the first water inlet. When the pressure relay is triggered, the inlet of the three-way valve is connected to the second water inlet, and the drain outlet is opened at the same time.
8. The perchloric acid distillation apparatus according to claim 6, characterized in that, The lower part of the vertical plate is provided with several through holes; And / or, the vertical plate portion is fixed to the sleeve by a connecting rod.
9. The perchloric acid distillation apparatus according to claim 5, characterized in that, The distillation vessel is equipped with stirring blades; And / or, the heat exchange surface of the distillation vessel is provided with fins.
10. The perchloric acid distillation apparatus according to claim 5, characterized in that, The distillation vessel is equipped with a mist separator at the condensate recovery port.