A three-layer jacketed vacuumized visual cold trap suitable for supercritical extract collection

Abstract

The application discloses a three-layer jacketed vacuumized visual cold trap suitable for supercritical extract collection. The three-layer jacketed vacuumized visual cold trap comprises a cold trap body; the cold trap body comprises a refrigeration chamber and a refrigeration room sleeved outside the refrigeration chamber, the refrigeration chamber is used for placing refrigerant; a ring cavity is sleeved outside the refrigeration room as a vacuum chamber; an air inlet and an air outlet are arranged on the outer wall of the refrigeration room, a collecting port is arranged at the bottom of the refrigeration room; and a vacuum air outlet is arranged on the outer wall of the vacuum chamber. The three-layer jacketed vacuumized visual cold trap can be used in cooperation with a supercritical extraction instrument, and specifically, the visual cold trap of the application can be used after a separation kettle, so that the extract in tail gas and the residual extract in the system can be effectively collected.

Description

TECHNICAL FIELD

[0001] The present application relates to a three-layer jacketed vacuumized visual cold trap suitable for supercritical extract collection, belonging to the technical field of supercritical extraction. BACKGROUND

[0002] Natural plant volatile is a kind of organic compounds with molecular weight between 50-500 Da, which plays an important role in plant growth and is an important quality index of aromatic plants. It is also an important factor affecting the quality of flowers, fruits and wine. Traditional extraction methods of plant volatile include steam distillation, pressing and solvent extraction. Emerging extraction techniques include microwave-assisted extraction, ultrasonic-assisted extraction and supercritical extraction. Due to the advantages of low temperature and no pollution, supercritical extraction is increasingly used in the preparation of plant volatile.

[0003] The state point at which the liquid-gas two-phase interface disappears is called the supercritical point. The temperature and pressure at the critical point are called the critical temperature and the critical pressure, respectively. The critical point pressure and temperature of different substances are different. A supercritical fluid (SCF) is a fluid with a temperature and pressure higher than its critical point. When CO2 is in a state with a temperature higher than the critical temperature Tc = 31.26℃ and a pressure higher than the critical pressure Pc = 72.9atm, it becomes a supercritical fluid. Its density is close to that of a liquid, its viscosity is close to that of a gas, and its diffusion coefficient is 100 times that of a liquid, so it has strong solubility. The supercritical extraction and separation process takes advantage of the special increased solubility of CO2 fluid in the supercritical state for organic matter, and the basic insolubility of organic matter in the non-critical state. CO2 fluid is continuously circulated between the extraction kettle, so that the components to be extracted are extracted from the raw materials, and then enter the separation kettle. The CO2 in the non-supercritical state releases the extracted components.

[0004] Currently, there are problems with supercritical extraction instruments. Some volatile substances cannot be released in the separation kettle in time and are carried out of the separation kettle by CO2 gas. Therefore, the tail gas contains a large amount of volatile substances. Although some supercritical extraction instruments are equipped with a cold trap that can collect some compounds in the tail gas, the cold trap structure is relatively simple, with only one gas channel and is not transparent, making it inconvenient to observe and affecting the use efficiency. Some supercritical extraction instruments do not have a cold trap, and a large amount of substances is lost in the tail gas. Moreover, after the extraction is completed, some volatile substances remain in the entire system, especially in the separation kettle and the pipeline after it, resulting in a low extraction rate.

[0005] Therefore, it is necessary to provide a cold trap that can collect the extracted substances in the tail gas, extract the remaining extracted substances in the system through negative pressure, and be visualized for easy operation, thereby improving the extraction efficiency. SUMMARY

[0006] The application aims to provide a three-layer jacketed vacuumized visual cold trap suitable for supercritical extract collection to enhance the collection of volatile substance supercritical extract.

[0007] The three-layer jacketed vacuumized visual cold trap comprises a cold trap body, wherein the cold trap body comprises a refrigeration chamber and a freezing chamber sleeved outside the refrigeration chamber, and the refrigeration chamber is used for placing refrigerant.

[0008] The freezing chamber is sleeved with a ring cavity as a vacuum chamber.

[0009] The outer wall of the freezing chamber is provided with an air inlet and an air outlet, and the air inlet is preferably arranged at the upper part of the freezing chamber, and the air outlet is preferably arranged at the lower part of the freezing chamber.

[0010] The bottom of the freezing chamber is provided with a collection port.

[0011] The outer wall of the vacuum chamber is provided with a vacuum air outlet.

[0012] The three-layer jacketed vacuumized visual cold trap is visual and can be made of glass; the visual design can ensure sufficient refrigerant such as liquid nitrogen, thereby improving the efficiency of the cold trap.

[0013] The three-layer jacketed vacuumized visual cold trap can use liquid nitrogen as refrigerant.

[0014] The application sets a vacuum chamber outside the freezing chamber, and a vacuum layer is formed by vacuumizing to play a heat insulation role.

[0015] Specifically, the vacuum chamber and the freezing chamber are communicated through a bypass.

[0016] The two ends of the bypass are connected with the vacuum chamber and the air outlet respectively, and the communication between the vacuum chamber and the freezing chamber is controlled through the bypass.

[0017] Specifically, an adjusting valve can be arranged on the bypass, and the two are threadedly connected.

[0018] The communication and closure of the bypass are controlled through the adjusting valve, that is, when the bypass is closed, the vacuum chamber serves as a heat insulation layer, and when the bypass is communicated, the air outlet is closed, the residual extract in the pipeline is extracted through vacuumizing, and more compounds are released.

[0019] The three-layer jacketed vacuumized visual cold trap can be used with a supercritical extractor, and specifically, the visual cold trap can be used after a separation kettle to effectively collect the extract in tail gas, and the residual extract in the system can be collected through vacuumizing to improve the extraction rate.

[0020] The three-layer jacket vacuumized visualized cold trap has the following beneficial effects:

[0021] 1. Visualized setting, thereby ensuring sufficient refrigerant and improving the efficiency of the cold trap.

[0022] 2. Vacuumization can manufacture a vacuum chamber, which functions as a heat insulation layer.

[0023] 3. The flow path is changed by adjusting the valve: when the valve is closed, the exhaust gas passes through the refrigeration chamber, and the liquid nitrogen refrigeration collects; when the valve is opened, the refrigeration chamber and the vacuum chamber are connected, and the residual extract in the system is extracted and collected by the liquid nitrogen refrigeration through the refrigeration chamber.

[0024] 4. By means of vacuumization, negative pressure is provided to the entire system of the extraction instrument, so that more compounds in the material are released. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 The structure diagram of the three-layer jacket vacuumized visualized cold trap is provided.

[0026] Figure 2 The schematic diagram of the three-layer jacket vacuumized visualized cold trap when the bypass is closed is provided.

[0027] Figure 3 The schematic diagram of the three-layer jacket vacuumized visualized cold trap when the bypass is connected is provided.

[0028] Figure 4 The schematic diagram of the three-layer jacket vacuumized visualized cold trap cooperating with the supercritical extraction instrument is provided.

[0029] The various marks in the figure are as follows:

[0030] 1 refrigeration chamber, 2 refrigeration chamber, 3 vacuum chamber, 4 air inlet, 5 air outlet, 6 collection port, 7 vacuum air outlet, 8 bypass, 9 adjusting valve. DETAILED DESCRIPTION

[0031] The present application will be further described below in conjunction with the drawings, but the present application is not limited to the following embodiments.

[0032] For example, Figure 1As shown in the structure diagram of the three-layer jacket vacuumized visual cold trap provided by the application, the cold trap body includes a refrigeration chamber 1 (liquid nitrogen) and a freezing chamber 2 sleeved outside the refrigeration chamber 1, and a ring cavity outside the freezing chamber 2 is sleeved as a vacuum chamber 3. The upper part of the outer wall of the freezing chamber 2 is provided with an air inlet 4, the lower part of the outer wall is provided with an air outlet 5, and the bottom is provided with a collection port 6. The outer wall of the vacuum chamber 3 is provided with a vacuum air outlet 7. A bypass 8 is connected between the vacuum chamber 3 and the freezing chamber 2, the two ends of the bypass 8 are connected with the vacuum chamber 3 and the air outlet 5 respectively, and a regulating valve 9 is threadedly connected on the bypass 8. The communication and closure of the bypass 8 are controlled through the regulating valve 9, that is, when the regulating valve 9 is closed, the bypass 8 is closed, and the vacuum chamber 3 and the freezing chamber 2 are not communicated, at this time, the vacuum chamber 3 serves as a heat insulation layer; when the regulating valve 9 is opened, the bypass 8 is communicated, the vacuum chamber 3 and the freezing chamber 2 are communicated, and the air outlet 5 is closed, at this time, the residual extract in the pipeline is extracted through vacuumization, and more compounds can be released under negative pressure. Figure 2 Figure 3

[0033] The three-layer jacket vacuumized visual cold trap is visual and is made of low-temperature-resistant glass; the visual design can ensure sufficient liquid nitrogen, thereby improving the efficiency of the cold trap.

[0034] The three-layer jacket vacuumized visual cold trap can be used in cooperation with a supercritical extraction instrument, and the system schematic diagram after cooperation is as shown in the drawing. Figure 4 The inlet of the extraction kettle is connected with a pressure gauge, a booster pump and an extraction kettle back pressure system, a valve A is arranged between the back pressure system and the separation kettle. The outlet of the extraction kettle is connected with the separation kettle, and a valve B is arranged between the extraction kettle and the separation kettle. The upper outlet of the separation kettle is sequentially connected with a separation kettle back pressure system and the three-layer jacket vacuumized visual cold trap provided by the application, wherein the back pressure system is connected with the air inlet 4, and the air outlet 5 is communicated with the outside. The lower outlet of the separation kettle is connected with a collection bottle, and a valve C is arranged between the separation kettle and the collection bottle.

[0035] When the above system performs extraction, in the extraction stage, the regulating valve 9 is closed, as shown in the drawing, vacuumization is performed through the vacuum air outlet 7, at this time, the vacuum chamber 3 plays a role of heat insulation. The tail gas in the separation kettle enters the freezing chamber 2, the extract is collected by freezing, and CO2 flows out from the air outlet 5. Figure 2

[0036] After the extraction is completed, low-pressure extraction is performed, the valve A is closed, the regulating valve 9 is opened, and the air outlet 5 is closed, as shown in the drawing, at this time, the vacuum chamber 3 is communicated with the freezing chamber 2, the air inlet 4 is communicated with the separation kettle, the residual extract in the system is extracted into the freezing chamber 2 by the vacuum pump, and the extract is collected by freezing. Figure 3

[0037] Through cooperation of the visual cold trap provided by the application after the separation kettle, the extract in the tail gas and the residual extract in the system can be effectively collected.​​​​

Claims

1. A three-layer jacketed evacuated visualized cold trap suitable for supercritical extract collection comprising a cold trap body; characterized in that: The cold trap body comprises a refrigeration chamber for placing refrigerant and a freezing chamber sleeved outside the refrigeration chamber; The freezing chamber is sleeved with a ring cavity as a vacuum chamber; The outer wall of the freezing chamber is provided with an air inlet and an air outlet, and the bottom of the freezing chamber is provided with a collection port; The outer wall of the vacuum chamber is provided with a vacuum air outlet; The three-layer jacket vacuum visual cold trap is visual; The vacuum chamber and the freezing chamber are communicated through a bypass; The two ends of the bypass are connected with the vacuum chamber and the air outlet respectively, and the communication between the vacuum chamber and the freezing chamber is controlled through the bypass; An adjusting valve is arranged on the bypass to control the communication and closure of the bypass; The air inlet is arranged at the upper part of the freezing chamber, and the air outlet is arranged at the lower part of the freezing chamber.

2. The three-layer jacketed vacuum-pumpable visualizing cold trap according to claim 1, characterized in that: The three-layer jacket vacuum visual cold trap is made of glass.

3. The three-layer jacketed vacuum-pumpable visualization cold trap according to claim 1 or 2, characterized in that: The adjusting valve and the bypass are threadedly connected.

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