A reciprocating distillation apparatus and method of use thereof

Abstract

The present application relates to chemical analysis instrument technical field, specifically to a kind of reciprocating distillation equipment and its using method.It includes that heating furnace is arranged on automatic distillation instrument and is placed in distillation flask on heating furnace, still includes sample adding tube, is set on the outer wall of distillation flask, sample adding tube is inclined to extend to the bottom of distillation flask, and the bottom end of sample adding tube is in contact with the bottom of distillation flask;Composite mechanism is used to add sample or extract distillate into distillation flask and clean distillation flask, including with the liquid pump of sample adding tube interface, liquid pump is connected with composite pipeline distillation operation and instrument measurement, can realize all automation, from water sample, reagent, start distillation to distillation end, distillation distillate is directly exported, all realize automatic completion.The whole operation process is automated, realizes unattended operation.Working time is greatly shortened, and work efficiency is significantly improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical analysis instrument, in particular to a reciprocating distillation device and a using method thereof. BACKGROUND

[0002] The distillation instrument is generally manually operated, the water sample to be distilled is poured into a distillation flask, a reagent is manually added, the distillation flask is placed on a heating furnace, a condensing device is installed, cooling water is connected, and the distillation is heated. After the distillate reaches the required volume, the heating is turned off, and the distillate is taken to an analysis instrument for measurement.

[0003] At present, the full-automatic distillation instrument on the market can realize automatic addition of water samples or reagents by connecting an automatic liquid adding device to the top liquid inlet of the distillation flask, can realize automatic temperature control of the distillation flask by using a temperature control device, and can also realize functions such as automatic measurement of the liquid amount by weighing the distillate in the receiving bottle with a weighing device. However, such a distillation instrument is only semi-automatic in actual use, on the one hand, the distillate after distillation of such a distillation instrument still needs to be manually sent to an analysis instrument for subsequent analysis, and on the other hand, such a distillation instrument can only distill a single reagent, and manual cleaning of the distillation flask, condenser and receiving bottle is still required when the distillation reagent is replaced.

[0004] It can be seen that such a full-automatic distillation instrument still needs manual assistance to complete multiple operation steps in the distillation process in actual use, and it is difficult to realize a full-automatic distillation process. In particular, in some laboratories, there is a high frequency of distillate analysis, distillation reagent replacement and high cleanliness requirements, so the current distillation instrument cannot meet the user's use requirements, and the use effect is reduced. SUMMARY

[0005] In view of the above shortcomings of the prior art, the present application provides a reciprocating distillation device and a using method thereof, which can effectively solve the problem of low automation degree of the prior art.

[0006] To achieve the above purpose, the present application realizes the following technical scheme:

[0007] The present application provides a reciprocating distillation device, which comprises an automatic distillation instrument, a heating furnace provided on the automatic distillation instrument, and a distillation flask placed on the heating furnace, and further comprises:

[0008] A sample adding pipe is provided on the outer wall of the distillation flask, the sample adding pipe extends to the bottom of the distillation flask in an inclined manner, and the bottom end of the sample adding pipe is in contact with the bottom of the distillation flask.

[0009] The composite mechanism is used for adding sample, reagent or distillate into the distillation flask and cleaning the distillation flask, comprising a liquid delivery pump connected with a sample adding tube, and a composite pipeline connected with the liquid delivery pump, through which the sample, reagent or distillate is added into the distillation flask, and through which the cleaning liquid is added into the distillation flask to clean the distillation flask.

[0010] The receiving assembly comprises a plurality of receiving flasks placed on the automatic distillation instrument and corresponding to the number of the distillation flasks, the top of each of the distillation flasks is provided with a condenser tube, and each of the receiving flasks is used for receiving the distillate condensed by the condenser tube, after the distillation flasks are cleaned, the distillation flasks are vacuumized, the distillate in the receiving flasks is sucked into the distillation flasks through negative pressure, and the sample adding tube is used for sucking away the distillate for detection.

[0011] Further, the distillation flask is provided with an anti-backflow connecting pipe, the automatic distillation instrument is provided with an anti-backflow port in communication with the anti-backflow connecting pipe, and the anti-backflow port is provided with an anti-backflow valve.

[0012] Further, the condenser tube is provided with a condenser water outlet and a condenser water inlet, respectively.

[0013] Further, the condenser tube of the automatic distillation instrument is provided with a distillation outlet pipeline, the distillation outlet pipeline is provided with an outlet valve, the receiving flask is provided with a distillation outlet pipeline clamp for clamping the outlet end of the distillation outlet pipeline, and the condenser tube is provided with a distillation outlet port in communication with the distillation outlet pipeline.

[0014] Further, the receiving flask of the automatic distillation instrument is provided with a weighing tray below, the receiving flask is placed on the weighing tray, and the weighing tray is provided with a weighing sensor.

[0015] Further, the composite pipeline comprises a single multi-way valve or a plurality of single-way valves.

[0016] Further, the automatic distillation instrument is provided with a condenser water inlet and a condenser water outlet, or the automatic distillation instrument is provided with a water chiller water tank and a water chiller cooling fan.

[0017] Further, the condenser tube is connected with a distillation outlet pipeline, and the lower end of the distillation outlet pipeline is located at the bottom of the receiving flask.

[0018] A method for using a reciprocating distillation device, comprising the following steps:

[0019] S1: water sample is introduced into the distillation flask;

[0020] S2: reagent is introduced into the distillation flask;

[0021] S3: heating distillation, the anti-backflow port is closed, the outlet valve is opened, and the distillation flask is heated;

[0022] S4: Automatic Distillation Stop: When the weighing tray detects that the weight has reached the preset value, the distillation heating and liquid outlet valves are turned off, the anti-backflow valve is opened, and cooling is allowed;

[0023] S5: Cleaning the distillation flask: Drain the remaining solution from the distillation flask, then add cleaning water to the distillation flask, and finally drain the cleaning water.

[0024] S6: Collect the solution in the condenser: Blow air into the distillation flask to push the remaining distillate in the condenser into the receiving flask and weigh it accurately;

[0025] S7: Transfer distillate: Vacuum the distillation flask. After the distillation flask is evacuated, the distillate is drawn from the sample addition tube into the container through the distillation flask for analysis and measurement.

[0026] S8: Measurement: Use various automated analytical instruments to perform automatic quantitative measurement of distillate.

[0027] The technical solution provided by this invention has the following advantages compared with the known prior art:

[0028] 1. A tilted sample addition tube is installed on the distillation flask of a traditional distillation instrument. Based on this sample addition tube and in conjunction with composite tubing and analytical instruments, automated functions such as controlling water sample intake, adding reagents, exporting distillate, and adding cleaning solution to clean the distillation flask are realized. This can meet the requirements of high-frequency distillate analysis, distillation reagent replacement, and high cleanliness, thus improving the performance of the automatic distillation instrument.

[0029] 2. Based on this sample addition tube, the distillation flask can be evacuated by the infusion pump, so that the distilled liquid can be drawn out from the receiving bottle through the distillation flask and then sent through the tube to the original container that held the water sample for analysis and measurement by the analytical instrument. During this process, the negative pressure environment formed in the distillation flask can be used to remove all the distilled liquid in the receiving bottle, ensuring the delivery effect of the distilled liquid.

[0030] 3. The method of using the reciprocating distillation equipment provided by the present invention is different from the method of using existing automatic distillation instruments. It does not require manual assistance, optimizes the operation steps, and realizes the complete automation of the automatic distillation instrument. Attached Figure Description

[0031] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the accompanying drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are merely some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without any creative effort.

[0032] Figure 1 This is an overall schematic diagram of the present invention;

[0033] Figure 2 This is a front view of the present invention;

[0034] Figure 3 This is a right view of the present invention;

[0035] Figure 4 This is the left view of the present invention;

[0036] Figure 5 This is a rear view of the present invention;

[0037] Figure 6 This is a schematic diagram of the working state of a distillation flask.

[0038] The labels in the diagram represent: 1. Heating furnace; 101. Ceramic heater; 2. Distillation flask; 201. Anti-backflow connector; 202. Sample addition tube; 3. Condenser; 301. Condensate outlet; 302. Condensate inlet; 303. Distillate outlet; 304. Condenser clamp; 4. Receiving bottle; 5. Weighing tray; 501. Weighing sensor; 6. Distillate tubing clamp; 7. Anti-backflow interface; 701. Anti-backflow valve; 8. Touch screen; 9. Power switch; 10. Main and auxiliary power sockets; 11. Communication port; 13. Discharge valve; 14. Air-cooled cooling fan; 15. Chiller water tank; 16. Chiller cooling fan; 17. Backflush pump. Detailed Implementation

[0039] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0040] The present invention will be further described below with reference to embodiments.

[0041] Example 1:

[0042] refer to Figures 1-6A reciprocating distillation apparatus includes an automatic distiller, a heating furnace 1, and a distillation flask 2 placed on the heating furnace. The heating furnace 1 uses a ceramic heater 101. A condenser tube 3 is provided on the top of the distillation flask 2. A condenser tube clamp 304 is provided on the automatic distiller, and the condenser tube 3 is clamped in the condenser tube clamp 304. A condensate water outlet 301 and a condensate water inlet 302 are respectively provided on the outside of the condenser tube 3. The automatic distiller has the same number of receiving bottles 4 as the distillation flask 2. The automatic distiller has a distillation outlet pipeline, and the distillation outlet pipeline is equipped with an outlet valve 13. The receiving bottles 4 are equipped with distillation outlet pipeline clamps 6 for clamping the water outlet end of the distillation outlet pipeline. The tube 3 is provided with a distillate outlet 303 connected to the distillate outlet pipeline. The automatic distillation apparatus is provided with multiple weighing trays 5. The receiving bottle 4 is placed on the weighing tray 5. The weighing tray 5 is provided with a weighing sensor 501. A receiving component is also provided, including receiving bottles placed on the automatic distillation apparatus in the same number as the distillation flasks. The top of the distillation flask is provided with a condenser tube, and the receiving bottle is used to receive the distillate condensed from the condenser tube. After the distillation flask is cleaned, the distillate in the receiving bottle is drawn into the distillation flask by a liquid pump in conjunction with a negative pressure environment, and then drawn away through the sample addition tube. One end of the distillate outlet pipeline extends to the bottom of the receiving bottle, and the liquid in the receiving bottle is drawn into the distillation flask through the distillate outlet pipeline. In traditional methods, the distillate, i.e., the distillate in the receiving flask, requires an additional cleaning line and pump. In this invention, it can be directly drawn back. The process involves using the distillate outlet line to draw the distillate from the receiving flask into the condenser, and then drawing the distillate from the condenser back into the distillation flask 2, achieving the goal of returning it along the same path. Note that the pump is a reversible pump; also, the distillate outlet line in the receiving flask 4 is located at the bottom of the receiving flask 4. After distillation, the outlet valve 13 is closed to facilitate weighing by the weighing tray 5. When cleaning or testing is required, the outlet valve 13 is reopened. At this time, the heating device below the distillation flask 2 stops heating, the external air pressure remains constant, and the temperature inside the distillation flask drops, creating a negative pressure environment. This ensures that all the distillate is drawn away, thus achieving the goal of drawing the distillate from the receiving flask into the distillation flask through negative pressure, and then, under the action of the pump, drawing it away through the sample addition tube for subsequent steps. The distilled liquid is returned via the original path to achieve fully automated distillation cleaning and testing. The actual path is: receiving bottle → condenser → distillation flask → sample addition tube → composite pipeline → analytical instrument. That is, the automatic distillation apparatus is connected to a forward and reverse pump. Through a multi-port valve or multiple single-port valves, the water sample, reagents, etc. to be tested can be added to the distillation flask through the sample addition tube, or the distillate in the receiving bottle can be reversed and introduced into the measuring instrument for measurement.

[0043] The condenser tube 3 is externally equipped with a condensate outlet 301 and a condensate inlet 302 to facilitate the inflow and outflow of cooling water. Furthermore, the automatic distillation apparatus may be equipped with a condensate inlet and a condensate drain, which are connected to the condensate inlet 302 and the condensate outlet 301 respectively via water pipes to facilitate the connection to external cooling water; alternatively, the automatic distillation apparatus may be equipped with a chiller tank 15 and a chiller cooling fan 16, with the chiller tank's inlet and outlet connected to the condensate outlet 301 and the condensate inlet 302 respectively via water pipes to facilitate the recycling of cooling water within the automatic distillation apparatus.

[0044] refer to Figure 3 or Figure 4 A sample addition tube 202 is provided on the outer wall of the distillation flask 2. The sample addition tube 202 extends at an angle of 25 degrees to the bottom of the distillation flask 2, and the bottom end of the sample addition tube 202 contacts the bottom of the distillation flask 2. The automatic distillation apparatus is also equipped with a composite mechanism for adding samples or extracting distillate into the distillation flask 2 and cleaning the distillation flask 2. This mechanism includes a pump 12 connected to the sample addition tube 202 and a composite pipeline. The distillation flask 2 is equipped with an anti-backflow tube 201. The automatic distillation apparatus is equipped with an anti-backflow interface 7 connected to the anti-backflow tube 201 and an anti-backflow valve 701. The automatic distillation apparatus is equipped with a backflush pump 17, which adds samples or extracts distillate into the distillation flask 2 through the composite pipeline, and simultaneously adds cleaning solution and blowing air into the distillation flask 2.

[0045] The composite pipeline is equipped with a single multi-way valve or multiple single-way valves. The single multi-way valve or multiple single-way valves are connected to the infusion pump 12. The number of single-way valves and the number of branches of the multi-way valve depend on the type of solution to be transferred.

[0046] The automatic distillation apparatus is equipped with a processor and a controller. The controller controls the heating furnace 1, various valves, and pumps, and completes the entire distillation and analysis process according to a pre-set program. Externally, the automatic distillation apparatus is equipped with an operation touch screen 8, a power switch 9, main and auxiliary power sockets 10, and a communication port 11.

[0047] The distillation process described above is not significantly different from traditional distillation techniques. The difference lies in the installation of a sample addition tube 202 on the distillation flask 2 of a traditional automatic distillation apparatus. The tube reaches the bottom of the distillation flask, and the other end of the tube is connected to an infusion pump, which is connected to a single multi-port valve or multiple single-port valves.

[0048] The distillate delivery tube of the distillation flask exits through the condenser and reaches the bottom of the receiving flask, which is then placed on a weighing device for accurate weighing of the distillate.

[0049] Connect the water sample, distillation reagent, cleaning water, waste liquid, and container holding the water sample to one end of the solenoid valve or multi-way valve. Switch the valve to allow each solution to flow into or out of the distillation flask.

[0050] In this way, multiple distillation flasks can be connected, and multiple channels can perform automatic distillation operations simultaneously.

[0051] For detailed usage instructions, please refer to [link / reference]. Figure 6 :

[0052] 1. Water sample inlet: The water sample to be distilled is introduced into the distillation flask by the forward operation of the pump.

[0053] 2. Add reagents: The pump is running in the forward direction to introduce the distillation reagents into the distillation flask.

[0054] 3. Heating and distillation: The program automatically turns on V1 and turns off V2, automatically controlling the heating and distillation.

[0055] 4. Automatic Distillation Stop: When the weight of the distillate measured on the balance reaches the set value, the distillation heater and valve V1 will be automatically shut off, and valve V2 will be opened to allow cooling.

[0056] 5. Cleaning the distillation flask: Open the waste liquid discharge valve V5, the pump will run in reverse to discharge the remaining solution in the distillation flask, close V5, open V6, the pump will run in the forward direction to inject cleaning water into the distillation flask, close V6 and open V5, the pump will run in reverse to discharge the cleaning water.

[0057] 6. Collect the solution in the condenser: Turn V1 on, turn V2 off, turn V5 or V4 on, run the pump in the forward direction, blow air into the distillation flask, push the remaining distillate in the condenser into the receiving flask and weigh it accurately.

[0058] 7. Transfer distillate: V5 is closed, V4 is opened, the pump runs in reverse, and after the distillation flask is evacuated, the distillate is pumped through the distillation flask into the original container that held the water sample for analysis and measurement.

[0059] 8. Measurement: Various automated analytical instruments are used to automatically and quantitatively measure the distillate.

[0060] like Figure 6 As shown, it is worth noting that by adjusting different valves and pumps, cleaning water can be delivered to each pipeline to achieve the purpose of cleaning each pipeline, achieving the goal of no manual intervention throughout the process, and further improving its automation level.

[0061] It is worth noting that, such as Figure 6 As shown, V3, V4, V5 and V6 can each be a single-way valve; or, V3, V4, V5 and V6 can be different branches of the same multi-way valve, thereby completing functions such as adding cleaning water and draining waste liquid.

[0062] The aforementioned multi-port valve can also be equipped with other tubing to expand its functionality, such as facilitating the addition of different reagents to the distillation flask. Its main functions include distillation, drainage, cleaning, and the removal and detection of the distillate via the sample addition tube 202.

[0063] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit them. Although the present invention has been described in detail with reference to the preceding embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the preceding embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions will not cause the essence of the corresponding technical solutions to deviate from the protection scope of the technical solutions of the embodiments of the present invention.

Claims

1. A reciprocating distillation apparatus, comprising an automatic distillation apparatus, wherein a heating furnace and a distillation flask placed on the heating furnace are provided on the automatic distillation apparatus, characterized in that, Also includes: The sample addition tube is located on the outer wall of the distillation flask, with the bottom end of the sample addition tube in contact with the bottom of the distillation flask. A composite mechanism for adding samples, reagents, or extracting distillate into a distillation flask and cleaning the distillation flask, including an infusion pump connected to a sample addition tube, the infusion pump being connected to a composite pipeline for adding samples, reagents, or extracting distillate into the distillation flask, and for adding cleaning solution to the distillation flask to clean it. The receiving component includes receiving bottles placed on an automatic distillation apparatus in the same number as the distillation flasks. Each distillation flask is equipped with a condenser tube at the top, and the receiving bottle is used to receive the distillate condensed from the condenser tube. After the distillation flask is cleaned, a vacuum is drawn into the distillation flask, and the distillate in the receiving bottle is drawn into the distillation flask by negative pressure and then drawn away through a sample addition tube for testing.

2. The reciprocating distillation apparatus according to claim 1, characterized in that, The distillation flask is equipped with an anti-backflow tube, and the automatic distillation apparatus is equipped with an anti-backflow interface connected to the anti-backflow tube. An anti-backflow valve is provided at the anti-backflow interface.

3. The reciprocating distillation apparatus according to claim 2, characterized in that, The condenser tube is provided with a condensate outlet and a condensate inlet on the outside.

4. The reciprocating distillation apparatus according to claim 3, characterized in that, The automatic distillation apparatus has a distillation outlet pipe on its condenser tube, and an outlet valve on the distillation outlet pipe. The receiving bottle is equipped with a distillation outlet pipe clamp for holding the water outlet end of the distillation outlet pipe.

5. The reciprocating distillation apparatus according to claim 4, characterized in that, The automatic distillation apparatus has a weighing tray under the receiving bottle, the receiving bottle is placed on the weighing tray, and a weighing sensor is installed in the weighing tray.

6. The reciprocating distillation apparatus according to claim 1, characterized in that, The composite pipeline includes a single multi-way valve or multiple single-way valves.

7. The reciprocating distillation apparatus according to claim 3, characterized in that, The automatic distillation apparatus is equipped with a condensate inlet and a condensate outlet.

8. A reciprocating distillation apparatus according to claim 3, characterized in that, The automatic distillation apparatus is equipped with a chiller water tank and a chiller cooling fan.

9. A reciprocating distillation apparatus according to claim 1, characterized in that, The condenser is connected to a distillation outlet pipe, the lower end of which is located at the bottom of the receiving bottle.

10. A method of using a reciprocating distillation apparatus applicable to any one of claims 1-9, characterized in that, Includes the following steps: S1: Water sample inlet: Introduce the water sample to be distilled into the distillation flask; S2: Add reagent: Pour the distillation reagent into the distillation flask; S3: Heating distillation: Close the anti-backflow port, open the liquid outlet valve, and heat the distillation flask; S4: Automatic Distillation Stop: When the weighing tray detects that the weight has reached the preset value, the distillation heating and liquid outlet valves are turned off, the anti-backflow valve is opened, and cooling is allowed; S5: Cleaning the distillation flask: Drain the remaining solution from the distillation flask, then add cleaning water to the distillation flask, and finally drain the cleaning water. S6: Collect the solution in the distillation line: Blow air into the distillation flask to push the remaining distillate in the distillation line into the receiving flask and weigh it accurately; S7: Transfer distillate: Vacuum the distillation flask. After the distillation flask is evacuated, the distillate is drawn from the sample addition tube into the container through the distillation flask for analysis and measurement. S8: Measurement: Use various automated analytical instruments to perform automatic quantitative measurement of distillate.

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