Molecular distillation instrument capable of automatically and accurately feeding sample

Abstract

The utility model relates to a molecular distillation instrument capable of automatically and accurately feeding samples, which comprises a storage tank, a molecular distillation chamber and a three-way pipe, two of three ports of the three-way pipe are respectively communicated with a discharge port of the storage tank and a feed port of the molecular distillation chamber, and the other port is communicated with a flow pump through a guide pipe. A one-way valve flowing into the molecular distillation chamber from the flow pump is fixed in a port communicated with the guide pipe in the three-way pipe, a manual flow regulating valve is arranged on a discharge port of the storage tank, and an air outlet in the side end of the molecular distillation chamber is connected with a vacuum pump through a glass guide pipe. The device has the beneficial effects that the three-way pipe with the built-in one-way valve and the flow pump are additionally arranged at the feeding hole of the molecular distillation chamber to replace a manual flow regulating valve for manual sampling, so that automatic and accurate sampling of materials is realized, process parameters can be more systematically optimized, the utilization rate of the materials is improved, and the purposes of reducing cost, improving efficiency and stabilizing production are achieved.

Description

Technical Field

[0001] The utility model relates to the technical field of separation and purification of tobacco flavor and fragrance, and particularly relates to a molecular distillation instrument with automatic and precise sample injection. Background Art

[0002] In the development and preparation technology of natural tobacco flavors, molecular distillation technology plays an important role in the further separation and purification of flavor products. The structure of a traditional manually-injected molecular distillation instrument is as Figure 1 shown. It includes a storage tank 1, a molecular distillation chamber 2, and a two-way pipe 9. The two ports of the two-way pipe 9 are respectively communicated with the discharge port of the storage tank 1 and the feed port of the molecular distillation chamber 2. A manual flow regulating valve 7 is provided at the discharge port of the storage tank 1. The gas outlet at the side end of the molecular distillation chamber 2 is connected to a vacuum pump 8 through a glass conduit 210. Along the gas flow direction on the glass conduit 210, a piston 290, a liquid nitrogen cold trap 220, and a pressure gauge 230 are successively arranged. A condensation column 240 is provided inside the molecular distillation chamber 2. The heavy component outlet and the light component outlet at the bottom of the molecular distillation chamber 2 are respectively connected to a heavy component receiving tank 250 and a light component receiving tank 260. A melted water receiving tank 270 communicating with the liquid nitrogen cold trap 220 is fixed below the liquid nitrogen cold trap 220 on the glass conduit 210. A stirrer 280 is fixed on the molecular distillation chamber 2, and the scraper 281 of the stirrer 280 is located inside the molecular distillation chamber 2.

[0003] The factors affecting the experimental results in molecular distillation technology include evaporation temperature, scraper rotation speed, vacuum degree, and the sample injection volume of the material. The thin film evaporation temperature can be controlled by a constant temperature water bath through circulating water. The scraper rotation speed can be accurately set through the stirrer. The vacuum degree can be stably controlled by the vacuum pump to achieve air pressure stability, that is, the thin film evaporation temperature, scraper rotation speed, and vacuum degree can all be accurately controlled through auxiliary equipment. However, the sample injection volume of the material can only be manually adjusted through a valve, and the material flow rate adjustment is unstable, resulting in highly likely inconsistent results before and after, and affecting the significant level difference expression among the changes of the other three parameters (evaporation temperature, scraper rotation speed, and vacuum degree), ultimately causing batch fluctuations in the quality of natural tobacco flavor products. Summary of the Utility Model

[0004] The technical problem to be solved by the utility model is to provide a molecular distillation instrument with automatic and precise sample injection to overcome the deficiencies in the above-mentioned prior art.

[0005] The technical solution of the present utility model to solve the above technical problems is as follows: A molecular distillation instrument with automatic and precise sample injection, comprising: a storage tank, a molecular distillation chamber, and a three-way pipe. Two of the three ports of the three-way pipe are respectively connected to the discharge port of the storage tank and the feed port of the molecular distillation chamber, and the other port is connected to a flow pump through a conduit. A one-way valve with a flow direction from the flow pump into the molecular distillation chamber is fixed in the port of the three-way pipe connected to the conduit. A manual flow regulating valve is provided at the discharge port of the storage tank, and the gas outlet at the side end of the molecular distillation chamber is connected to a vacuum pump through a glass conduit.

[0006] Based on the above technical solution, the present utility model can be further improved as follows.

[0007] Further, the flow pump is a valveless pump.

[0008] Further, the material flow rate regulated by the manual flow regulating valve is 2 mL / min to 50 mL / min.

[0009] Further, the volume of the storage tank is 1000 mL to 1200 mL.

[0010] Further, a piston, a liquid nitrogen cold trap, and a pressure gauge are sequentially provided on the glass conduit along the gas flow direction. A condensation column is provided in the molecular distillation chamber. The heavy component outlet and the light component outlet at the bottom of the molecular distillation chamber are respectively connected to a heavy component receiving tank and a light component receiving tank. A melted water receiving tank communicating with the liquid nitrogen cold trap is fixed below the liquid nitrogen cold trap on the glass conduit.

[0011] Further, the operating temperature range of the condensation column is -1 °C to -30 °C, the operating pressure range generated by the vacuum pump is 1 Pa to 1000 Pa, and the operating temperature range of the thin film evaporation on the surface of the molecular distillation chamber is 20 °C to 80 °C.

[0012] Further, a stirrer is fixed on the molecular distillation chamber, and the scraper of the stirrer is inside the molecular distillation chamber.

[0013] Further, the operating speed range of the stirrer is 1 r / min to 600 r / min.

[0014] Further, the pressure gauge is an electronic pressure gauge.

[0015] The beneficial effects of the present utility model are as follows: A tee pipe with an internal one-way valve and a flow pump are added at the feed inlet of the molecular distillation chamber to replace the manual injection of samples with a manual flow regulating valve, so as to achieve automatic and precise injection of materials. When optimizing the preliminary test conditions, the injection volume of the materials can be precisely controlled to carry out gradient tests, and orthogonal tests of four factors can be jointly carried out together with the three factors of evaporation temperature, scraper speed, and vacuum degree to obtain the best molecular distillation process. When the molecular distillation process is established after condition optimization, materials can also be manually injected through the storage tank to carry out the separation and purification of tobacco flavorings, obtaining molecular distillation light components and heavy components. The molecular distillation instrument equipped with a flow pump can more systematically optimize process parameters, improve the utilization rate of materials, achieve the purpose of cost reduction, efficiency increase, and stable production, and is convenient to use. Under the same molecular distillation process conditions, the average error of the three-time yield of the light component product of the molecular distillation instrument with automatic and precise injection described in the present utility model is less than 0.8%, while the average error of the three-time yield of the light component product of the molecular distillation instrument in the prior art is greater than 3%. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 is a structural diagram of a manual injection molecular distillation instrument in the prior art;

[0017] Figure 2 is a structural diagram of the molecular distillation instrument with automatic and precise injection in the present utility model;

[0018] Figure 3 is a matching diagram of the tee pipe and the one-way valve in the present utility model. In the figure, A is connected to the discharge port of the storage tank, B is connected to the feed inlet of the molecular distillation chamber, and C is connected to the flow pump through a conduit.

[0019] In the drawings, the list of components represented by each reference numeral is as follows:

[0020] 1. Storage tank, 2. Molecular distillation chamber, 210. Glass conduit, 220. Liquid nitrogen cold trap, 230. Pressure gauge, 240. Condensing column, 250. Heavy component receiving tank, 260. Light component receiving tank, 270. Melting water receiving tank, 280. Stirrer, 281. Scraper, 290. Piston, 3. Tee pipe, 4. Conduit, 5. Flow pump, 6. One-way valve, 7. Manual flow regulating valve, 8. Vacuum pump, 9. Two-way pipe. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0021] The principles and features of the present utility model are described below with reference to the accompanying drawings. The examples given are only used to explain the present utility model and are not intended to limit the scope of the present utility model.

[0022] As Figure 2 、 Figure 3As shown in the figure, a molecular distillation apparatus with automatic and precise sample injection includes: a storage tank 1, a molecular distillation chamber 2, and a three-way pipe 3. Two of the three ports of the three-way pipe 3 are respectively connected to the discharge port of the storage tank 1 and the feed port of the molecular distillation chamber 2, and the other port of the three-way pipe 3 is connected to a flow pump 5 through a conduit 4. In addition, a one-way valve 6 is fixed in the port of the three-way pipe 3 that is connected to the conduit 4, and the flow direction of the one-way valve 6 is from the flow pump 5 into the molecular distillation chamber 2. The material of the three-way pipe 3 can be steel, and the conduit 4 can be a PVC transparent hose, which is soft and does not harden, can be bent, is cold-resistant and freeze-resistant, and is corrosion-resistant. The material of the one-way valve 6 can be SUS316, which is corrosion-resistant and not easy to rust, and the passage can only be opened under a certain negative pressure condition. When the vacuum degree is small, the external pressure is not enough to open this valve. When the vacuum degree is large, the pressure difference between the external pressure and the vacuum degree can open this valve; a manual flow regulating valve 7 is provided at the discharge port of the storage tank 1, and the gas outlet at the side end of the molecular distillation chamber 2 is connected to a vacuum pump 8 through a glass conduit 210.

[0023] Furthermore: The flow pump 5 is preferably a valveless pump, with a working voltage of 12 - 24V. The sample injection volume can be set by the rotation speed (R / s) and the injection volume (mL / R), and the sample injection flow rate is stable and consistent.

[0024] Specifically, the material flow rate regulated by the manual flow regulating valve 7 is 2 mL / min to 50 mL / min, and the sample injection flow rate will decrease as the height of the material liquid level drops.

[0025] Specifically, the volume of the storage tank 1 is 1000 mL to 1200 mL.

[0026] Specifically, the main body of the molecular distillation chamber 2 is made of special glass material and is a hollow structure. The evaporation temperature can be controlled to be constant by circulating water at a certain temperature; the working range of the film evaporation temperature on the surface of the molecular distillation chamber 2 is 20°C to 80°C. Along the gas flow direction on the glass conduit 210, a piston 290, a liquid nitrogen cold trap 220, and a pressure gauge 230 are successively provided. There is a condensation column 240 in the molecular distillation chamber 2, and the working range of the temperature of the condensation column 240 is -1°C to -30°C; the heavy component outlet and the light component outlet at the bottom of the molecular distillation chamber 2 are respectively connected to a heavy component receiving tank 250 and a light component receiving tank 260; a melted water receiving tank 270 connected to it is fixed below the liquid nitrogen cold trap 220 on the glass conduit 210, and the pressure generated by the vacuum pump 8 has a working range of 1 Pa to 1000 Pa.

[0027] Specifically, a stirrer 280 is fixed on the molecular distillation chamber 2. The scraper 281 of the stirrer 280 is inside the molecular distillation chamber 2, and the working range of the rotation speed of the stirrer 280 is 1 r / min to 600 r / min.

[0028] Specifically, the barometer 230 is an electronic barometer, and can measure in three atmospheric pressure measurement units: Bar, Pa, and Torr.

[0029] A three-way pipe 3 with a built-in one-way valve 6 and a flow pump 5 are added to the feed inlet of the molecular distillation chamber 2 to replace the manual injection with a manual flow regulating valve 7, so as to achieve automatic and precise injection of materials. When optimizing the preliminary test conditions, the injection volume of the materials can be precisely controlled to carry out gradient tests, and together with the three factors of evaporation temperature, scraper speed, and vacuum degree, an orthogonal test of four factors can be carried out to obtain the best molecular distillation process; when the molecular distillation process is established after condition optimization, materials can also be manually injected through the storage tank 1 to carry out the separation and purification of tobacco flavorings, obtaining molecular distillation light components and heavy components. The molecular distillation apparatus equipped with a flow pump 5 can more systematically optimize process parameters, improve the utilization rate of materials, achieve the purpose of cost reduction, efficiency increase, and stable production, and is convenient to use. Under the same molecular distillation process conditions, the average error of the three-time yield of the light component product of the molecular distillation apparatus with automatic and precise injection described in the present utility model is less than 0.8%, while the average error of the three-time yield of the light component product of the molecular distillation apparatus in the prior art is greater than 3%.

[0030] Although the embodiments of the present utility model have been shown and described above, it can be understood that the above embodiments are exemplary and should not be construed as limiting the present utility model. Those of ordinary skill in the art can make changes, modifications, substitutions, and variations to the above embodiments within the scope of the present utility model.

Claims

1. A molecular distillation apparatus with automatic and precise sampling, characterized in that: include: A material storage tank (1), a molecular distillation chamber (2) and a three-way pipe (3); two of the three ports of the three-way pipe (3) are respectively connected to the material discharge port of the material storage tank (1) and the material feed port of the molecular distillation chamber (2); the other port is connected to a flow pump (5) via a conduit (4); a one-way valve (6) is fixed in the port connected to the conduit (4) in the three-way pipe (3) so that the flow direction is from the flow pump (5) to the molecular distillation chamber (2); a manual flow regulating valve (7) is provided on the material discharge port of the material storage tank (1); and the gas outlet at the side end of the molecular distillation chamber (2) is connected to a vacuum pump (8) via a glass conduit (210).

2. The molecular distillation apparatus with automatic and precise sampling according to claim 1, characterized in that: The flow pump (5) is a valveless pump.

3. The molecular distillation apparatus with automatic and precise sampling according to claim 1, characterized in that: The material flow rate regulated by the manual flow regulating valve (7) is 2 mL / min to 50 mL / min.

4. The molecular distillation apparatus with automatic and precise sampling according to claim 1, characterized in that: The volume of the storage tank (1) is 1000 mL to 1200 mL.

5. A molecular distillation apparatus with automatic and precise sampling according to any one of claims 1 to 4, characterized in that: The glass conduit (210) is provided with a piston (290), a liquid nitrogen cold trap (220) and a barometer (230) in sequence along the airflow direction; the molecular distillation chamber (2) is provided with a condensation column (240); a heavy component outlet and a light component outlet at the bottom of the molecular distillation chamber (2) are connected to a heavy component receiving tank (250) and a light component receiving tank (260) respectively; and a melted water receiving tank (270) connected to the liquid nitrogen cold trap (220) is fixed on the glass conduit (210) below the liquid nitrogen cold trap (220).

6. The molecular distillation apparatus with automatic and precise sampling according to claim 5, characterized in that: The temperature operating range of the condensation column (240) is -1°C to -30°C, the pressure operating range generated by the vacuum pump (8) is 1Pa to 1000Pa, and the thin film evaporation temperature operating range on the surface of the molecular distillation chamber (2) is 20°C to 80°C.

7. The molecular distillation apparatus with automatic and precise sampling according to claim 5, characterized in that: A stirrer (280) is fixed on the molecular distillation chamber (2), and a scraper (281) of the stirrer (280) is located inside the molecular distillation chamber (2).

8. The molecular distillation apparatus with automatic and precise sampling according to claim 7, characterized in that: The operating range of the rotation speed of the stirrer (280) is 1 r / min to 600 r / min.

9. The molecular distillation apparatus with automatic and precise sampling according to claim 5, characterized in that: The barometer (230) is an electronic barometer.

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