A water vapor distillation apparatus

Abstract

The present application relates to laboratory analysis equipment technical field, disclose a kind of steam distillation apparatus, including steam generator and multiple groups of distillation units in parallel arrangement;Steam generator is provided with control console and steam outlet, steam outlet is connected with main steam pipeline, multiple branch pipes are arranged on main steam pipeline at intervals, electromagnetic valve is arranged on each branch pipe, and electromagnetic valve is electrically connected with control console;Each group of distillation units includes sequentially connected reaction vessel, condenser and collection vessel;Reaction vessel is communicated with main steam pipeline by branch pipe, for steam is introduced into the bottom of reaction vessel;Condenser is communicated with reaction vessel, for after distillation product is condensed into liquid, it is exported to collection vessel.The multiple groups of distillation units of the present application share a steam generator, realize steam independent distribution in each distillation unit, save space and energy consumption, improve efficiency, and automation is realized, greatly reduce the security risk of operation process.

Description

Technical Field

[0001] This invention relates to the field of laboratory analytical equipment technology, and in particular to a steam distillation apparatus. Background Technology

[0002] Steam distillation is an important separation and extraction technique widely used in food testing, such as in standard methods like GB 5009.26-2023 "Determination of N-Dimethylnitrosamine in Food", GB 5009.307-2025 "Determination of Formaldehyde in Beer", and GB 5009.36-2023 "Determination of Cyanide in Drinking Water". Traditional steam distillation apparatuses are typically manually assembled from glass components such as distillation flasks, condensers, and receiving flasks. These apparatuses have several shortcomings in practical applications. For example, traditional single-channel designs cannot process multiple samples in parallel, resulting in low efficiency and high energy consumption. Traditional apparatuses usually require manual monitoring of the distillation process, which increases the risk of bumping or scalding, especially when handling toxic substances (such as cyanide), posing a high operational risk. The volume of the distillate relies mainly on manual observation, making automatic shutdown difficult and affecting recovery rates and experimental reproducibility. Therefore, there is an urgent need to provide a steam distillation apparatus that improves experimental efficiency, accuracy, and safety. Summary of the Invention

[0003] In view of this, the present invention provides a steam distillation apparatus to solve the problems of low efficiency, high operational risk and poor experimental accuracy of traditional apparatuses.

[0004] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: A steam distillation apparatus includes a steam generator and multiple distillation units connected in parallel. The steam generator has a control console and a steam outlet. The steam outlet is connected to a main steam pipe, and multiple branch pipes are spaced apart on the main steam pipe. Each branch pipe is equipped with a solenoid valve, and the solenoid valve is electrically connected to the control console. Each distillation unit includes a reaction vessel, a condenser, and a collection container connected in sequence. The reaction vessel is connected to the main steam pipe through the branch pipes, which are used to introduce steam into the bottom of the reaction vessel. The condenser is connected to the reaction vessel, which is used to condense the distillation product into a liquid and then export it to the collection container.

[0005] Preferably, a liquid level sensor is installed on the outer wall of the collection container to monitor the liquid level in the collection container in real time.

[0006] Preferably, the liquid level sensor is electrically connected to the control console. When the liquid level sensor detects that the liquid level in the collection container has reached a set value, the liquid level sensor sends an electrical signal to the control console so that the control console controls the closing of the solenoid valve.

[0007] Preferably, the liquid level sensor is a photoelectric liquid level sensor.

[0008] Preferably, the steam generator is equipped with a safety valve and a pressure gauge, which are electrically connected to the control console.

[0009] Preferably, the pressure gauge is used to display the system pressure value in real time and send the pressure value to the control console. When the pressure value exceeds the set value, the control console controls the opening or closing of the safety valve.

[0010] Preferably, the main steam pipe and / or branch pipe are equipped with temperature sensors, and the temperature sensors are electrically connected to the control console. When the temperature sensor detects that the steam temperature exceeds the set value, the temperature sensor sends an electrical signal to the control console so that the control console controls the opening or closing of the solenoid valve.

[0011] Preferably, the condenser tube is provided with a water inlet, a water outlet, a sample inlet, and a sample outlet. The water inlet and the sample outlet are located at the bottom end of the condenser tube, and the water outlet and the sample inlet are located at the top end of the condenser tube. The sample inlet is connected to the reaction vessel, and the sample outlet is connected to the collection container.

[0012] Preferably, the condenser is equipped with a temperature sensor, and the temperature sensor is electrically connected to the control console. When the temperature sensor detects that the condensation temperature exceeds the set value, the temperature sensor sends an electrical signal to the control console so that the control console controls the parameters of the water entering at the inlet.

[0013] Preferably, the condenser is a double-vacuum serpentine condenser.

[0014] This invention provides a steam distillation apparatus, which has the following advantages compared with the prior art: The steam distillation apparatus of the present invention includes a steam generator and multiple distillation units arranged in parallel. The multiple distillation units in parallel can process multiple samples independently at the same time, which can effectively reduce energy consumption, improve detection efficiency, and shorten the time for processing the same number of samples by about 50%. The multiple distillation units share a single steam generator, and the distribution of steam in each distillation unit is achieved through the coordinated action of the main steam pipe, branch pipes, and solenoid valves, ensuring the independence of each channel, saving space and energy consumption. Furthermore, the distillation process is automated through the control console, which greatly reduces the safety risks during operation. Attached Figure Description

[0015] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0016] Figure 1 This is a schematic diagram of the steam distillation apparatus of the present invention; Figure 2 This is a schematic diagram of the distillation unit of the present invention.

[0017] In the diagram: 10-Steam generator, 11-Control console, 12-Steam outlet, 13-Safety valve, 14-Pressure gauge, 20-Distillation unit, 21-Reaction vessel, 22-Condenser, 221-Inlet, 222-Outlet, 23-Collection container, 231-Level sensor, 30-Main steam pipe, 40-Branch pipe, 50-Solenoid valve, 60-Connecting pipe. Detailed Implementation

[0018] The present invention will be described below through specific embodiments. Those skilled in the art will understand that the specific embodiments below are merely illustrative and do not limit the scope of the invention in any way. Furthermore, in the following embodiments, unless otherwise specified, the reagents and equipment used are commercially available. If specific processing conditions and methods are not explicitly described in the later embodiments, conditions and methods known in the art can be used for processing.

[0019] This invention provides a steam distillation apparatus, including a steam generator 10 and multiple distillation units 20 arranged in parallel, such as... Figure 1 As shown, six distillation units 20 are arranged in parallel. The number of distillation units 20 can be increased or decreased according to actual needs, and there is no special limitation on this.

[0020] In some embodiments of the present invention, the steam generator 10 is provided with a control console 11 and a steam outlet 12. The steam outlet 12 is connected to a main steam pipe 30. Multiple branch pipes 40 are arranged at intervals on the main steam pipe 30, the number of branch pipes 40 corresponding to the number of distillation units 20. Each branch pipe 40 is equipped with a solenoid valve 50, and the solenoid valve 50 is electrically connected to the control console 11 to achieve balanced steam distribution. Each distillation unit 20 operates independently and includes a reaction vessel 21, a condenser 22, and a collection vessel 23 connected in sequence. The reaction vessel 21 and the main steam pipe 30 are connected through the branch pipes 40 to introduce steam into the distillation unit 20 for distillation operation.

[0021] In some embodiments of the present invention, the reaction vessel 21 is a sealed structure used to hold samples and extracts. The reaction vessel 21 is preferably a reaction flask made of heat-resistant glass, and its specific type and capacity can be selected according to actual conditions; for example, it can be various types of distillation flasks with a capacity of 250-500 mL. The reaction vessel 21 is connected to the main steam pipe 30 via a branch pipe 40, which extends to the bottom of the reaction vessel 21 to introduce steam into the bottom of the reaction vessel 21. Furthermore, since each branch pipe 40 is equipped with a solenoid valve 50, the steam flow rate and on / off state of any distillation unit 20 can be precisely controlled by the solenoid valve 50, enabling independent operation of each distillation unit 20.

[0022] In some embodiments of the present invention, the condenser 22 is connected to the reaction vessel 21 and is used to condense the distillation product into a liquid and then export it to the collection container 23. The condenser 22 is provided with an inlet 221, an outlet 222, a sample inlet, and a sample outlet. The inlet 221 and the sample outlet are located at the bottom end of the condenser 22, and the outlet 222 and the sample inlet are located at the top end of the condenser 22. The sample inlet is connected to the reaction vessel 21, and the sample outlet is connected to the collection container 23. Preferably, the condenser 22 and the reaction vessel 21 are connected by a connecting pipe 60. The connecting pipe 60 can be made of high-temperature resistant silicone material; this is not specifically limited and can be adjusted according to actual conditions.

[0023] In some embodiments of the present invention, the condenser tube 22 is a double-vacuum serpentine condenser tube, which can improve condensation efficiency, reduce heat loss, and lower energy consumption, meeting the requirements for green laboratory construction. For example, the condenser tube 22 has a length of 40cm, an inner tube diameter of 2cm, an outer tube diameter of 3cm, and a vacuum layer thickness of 0.5cm. This double-vacuum structure increases condensation efficiency by 35% and reduces energy consumption by 40% compared to traditional condenser tubes.

[0024] In some embodiments of the present invention, the condensation temperature is set via the control console 11 to accommodate the boiling point requirements of different samples. A temperature sensor is installed on the condenser tube 22 and is electrically connected to the control console 11. When the temperature sensor detects that the condensation temperature exceeds the set value, it sends an electrical signal to the control console 11, causing the control console 11 to control the parameters of the water entering through the inlet 221. The condensation temperature, set via the control console 11, can accommodate the boiling point requirements of different samples. For example, the condensation temperature can be set to 0-15°C via the control console 11. When the temperature sensor detects that the temperature is within the set range, the distillation process operates normally. However, when the detected condensation temperature is higher than 15°C, the temperature sensor sends an electrical signal to the control console 11, causing the control console 11 to control the input of water at a lower temperature through the inlet 221, thus maintaining the condensation temperature at the set value and ensuring sufficient condensation of volatile substances.

[0025] In some embodiments of the present invention, a liquid level sensor 231 is installed on the outer wall of the collection container 23 for real-time monitoring of the liquid level in the collection container 23. The liquid level sensor 231 is electrically connected to the control console 11. When the liquid level sensor 231 detects that the liquid level in the collection container 23 has reached a set value, the liquid level sensor 231 sends an electrical signal to the control console 11, causing the control console 11 to control the closing of the solenoid valve 50 to prevent excessive distillation from causing the decomposition of the target substance. The liquid level in the collection container 23 is set by the control console 11. To avoid the influence of light on the target substance in the collected liquid and to further improve the measurement accuracy, the collection bottle is made of brown glass, and its capacity can be selected as needed, such as 100-500 mL, without special limitation.

[0026] In some embodiments of the present invention, the liquid level sensor 231 is a photoelectric liquid level sensor. The present invention uses a non-contact photoelectric liquid level sensor, which detects the liquid level through the principle of infrared light reflection. This avoids direct contact with the distillate in the collection container 23, avoids contamination of the distillate, achieves precise control of the distillate volume, reduces human error, and enables a sample recovery rate of over 95%.

[0027] In some embodiments of the present invention, the steam generator 10 is equipped with a safety valve 13 and a pressure gauge 14, which are electrically connected to the control console 11. The pressure gauge 14 is used to display the system pressure value in real time and send the pressure value to the control console 11. When the pressure value exceeds the set value, the control console 11 controls the opening or closing of the safety valve 13, which can ensure the normal operation of the distillation process while avoiding over-distillation, reducing operational risks and ensuring operational safety. The steam pressure and output are set and adjusted through the control console 11 to achieve automated operation.

[0028] In some embodiments of the present invention, the steam generator 10 is made of corrosion-resistant material and has a heating element inside, which can quickly generate high-temperature steam.

[0029] In some embodiments of the present invention, the main steam pipe 30 and / or branch pipe 40 are equipped with temperature sensors, which are electrically connected to the control console 11. When the temperature sensor detects that the steam temperature exceeds a set value, it sends an electrical signal to the control console 11, causing the control console 11 to control the opening or closing of the solenoid valve 50. For example, the control console 11 can set the steam temperature to 100-120°C. When the temperature sensor detects that the temperature is within the set range, the distillation process operates normally. When the detected steam temperature is higher than 120°C, the temperature sensor sends an electrical signal to the control console 11, causing the control console 11 to control the solenoid valve 50 to close, temporarily stopping the steam input. When the temperature sensor detects that the temperature has dropped to 100-120°C, the control console 11 controls the solenoid valve 50 to open, continuing the distillation operation. Adjusting the steam temperature through the control console 11 ensures the stability of the distillation process temperature.

[0030] This invention uses the control console 11 to control the steam flow rate, steam temperature, and condensation temperature in a coordinated manner. This not only avoids boiling and splashing during the distillation process, ensuring the accuracy and repeatability of the measurement results, but also allows for adaptation to standard methods such as GB 5009.26-2023, GB 5009.307-2025, and GB 5009.36-2023 through parameter adjustment, thus meeting various testing needs.

[0031] In some embodiments of the present invention, an emergency stop button is provided on the control console 11, which can quickly cut off the steam supply in abnormal situations. It should be noted that the control console 11 integrates a circuit control system to monitor steam temperature, condensation temperature, and liquid level in real time. This circuit control system is a standard industry practice and is not specifically limited thereto. The steam distillation apparatus of the present invention can be used to determine formaldehyde in beer. The steam distillation apparatus used for the determination employs six distillation units 20, and the determination method is as follows: (1) Set the steam temperature to 100-120℃, the condensation temperature to 0-15℃, and the liquid level in the collection container 23 to 200mL via the control console 11. (2) Take 25 mL of beer sample for carbon dioxide removal treatment, then add 20 mL of phosphoric acid solution (200 g / L) and 1 mL of dimethyl silicone oil (dimethyl silicone oil can prevent foam from being generated during distillation) to obtain the sample; (3) Divide the sample into six portions and place them in six reaction containers 21 respectively. Start the steam generator 10. The steam is introduced into the bottom of each reaction container 21 through the main steam pipe 30 and the branch pipe 40 for distillation. The steam carries volatile substances such as formaldehyde into the condenser 22 through the sample inlet. After condensation, it is discharged into the collection container 23 through the sample outlet. When the liquid level sensor 231 detects that the liquid level reaches close to 200mL, the liquid level sensor 231 sends a signal to the control console 11. The control console 11 closes the solenoid valve 50, stops the steam supply, and completes the distillation process to obtain the distillate. (4) Add acetylacetone solution to the distillate according to the standard method, then heat it in a boiling water bath for 5 minutes. After cooling, measure the absorbance at a wavelength of 415 nm and calculate the formaldehyde content in the beer according to the standard curve.

[0032] Furthermore, the steam distillation apparatus of the present invention can also be used for the determination of cyanide in drinking water. In this case, the steam temperature is set to 100-120°C, the condensation temperature is set to 0-15°C, and the liquid level in the collection container 23 is set to 100 mL. When processing a 250 mL water sample, 5 mL of a 100 g / L zinc acetate solution and 1 g of tartaric acid are added to the water sample, mixed, and then placed in the reaction container 21. Additionally, 5.0 mL of a 20 g / L sodium hydroxide solution needs to be pre-added to the collection bottle as an absorption liquid.

[0033] Furthermore, the steam distillation apparatus of the present invention can also be used for the determination of N-dimethylnitrosamine in food. In this case, the steam temperature is set to 100-120°C, the condensation temperature is set to 0-15°C, and the liquid level in the collection container 23 is set to 200-250 mL. When processing a 20g sample of pulverized meat products, 100 mL of water and 50 mL of sodium chloride are added to the sample for thorough mixing and extraction. The mixture is then transferred to the reaction container 21, and the collected liquid can be further extracted with dichloromethane and then analyzed by GC-MS.

[0034] Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of the present invention.

Claims

1. A steam distillation apparatus, characterized in that, It includes a steam generator and multiple distillation units arranged in parallel; the steam generator is equipped with a control console and a steam outlet, the steam outlet is connected to a main steam pipeline, and multiple branch pipelines are arranged at intervals on the main steam pipeline, each of the branch pipelines is equipped with a solenoid valve, and the solenoid valve is electrically connected to the control console. Each distillation unit includes a reaction vessel, a condenser, and a collection vessel connected in sequence; the reaction vessel is connected to the main steam pipe through the branch pipe for introducing steam into the bottom of the reaction vessel; the condenser is connected to the reaction vessel for condensing the distillation product into a liquid and then exporting it to the collection vessel.

2. The steam distillation apparatus according to claim 1, characterized in that, A liquid level sensor is installed on the outer wall of the collection container to monitor the liquid level in the collection container in real time.

3. The steam distillation apparatus according to claim 2, characterized in that, The liquid level sensor is electrically connected to the control console. When the liquid level sensor detects that the liquid level in the collection container has reached a set value, the liquid level sensor sends an electrical signal to the control console so that the control console controls the closing of the solenoid valve.

4. The steam distillation apparatus according to claim 2 or 3, characterized in that, The liquid level sensor is a photoelectric liquid level sensor.

5. The steam distillation apparatus according to claim 1, characterized in that, The steam generator is equipped with a safety valve and a pressure gauge, which are respectively electrically connected to the control console. The pressure gauge is used to display the system pressure value in real time and send the pressure value to the control console. When the pressure value exceeds the set value, the control console controls the opening or closing of the safety valve.

6. The steam distillation apparatus according to claim 1, characterized in that, Temperature sensors are installed in the main steam pipe and / or branch pipes, and the temperature sensors are electrically connected to the control console. When the temperature sensor detects that the steam temperature exceeds the set value, the temperature sensor sends an electrical signal to the control console so that the control console controls the opening or closing of the solenoid valve.

7. The steam distillation apparatus according to claim 1, characterized in that, The condenser tube is provided with a water inlet, a water outlet, a sample inlet, and a sample outlet. The water inlet and the sample outlet are located at the bottom end of the condenser tube, and the water outlet and the sample inlet are located at the top end of the condenser tube. The sample inlet is connected to the reaction vessel, and the sample outlet is connected to the collection container.

8. The steam distillation apparatus according to claim 7, characterized in that, The condenser tube is equipped with a temperature sensor, and the temperature sensor is electrically connected to the control console. When the temperature sensor detects that the condensation temperature exceeds the set value, the temperature sensor sends an electrical signal to the control console so that the control console controls the parameters of the water entering at the inlet.

9. The steam distillation apparatus according to claim 1, 7, or 8, characterized in that, The condenser is a double-vacuum serpentine condenser.

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