Micro-negative pressure distillation device

Abstract

The invention relates to the technical field of chemical experiments, in particular to a micro-negative pressure distillation device which comprises a multi-port distiller, a condenser, a liquid outlet device, an air pump, an air supply pipe and a refrigeration pump which are connected with one another. The multi-port distiller comprises a distillation chamber, a vapor-liquid separation plate, a gas guide port, a distillation port, a gas return port and a liquid collection port; the condenser comprises an air inlet, an air outlet, a refrigerant fluid inlet and a refrigerant fluid outlet; the liquid collector comprises a liquid receiving opening and a liquid collecting cavity; the air supply pipe comprises an upper port, an expansion pipe and a lower port. When the micro-negative-pressure distillation device operates, a micro-negative-pressure environment is formed in a closed system, and solvent steam is driven by non-condensable gas to realize efficient distillation and recovery of a solvent through the liquefaction effect of the condenser. The micro-negative pressure distillation device has the beneficial effects that the bumping phenomenon of reduced pressure distillation can be completely eradicated, and the micro-negative pressure distillation device has the advantages of high distillation efficiency, environment friendliness, high safety and the like.

Description

Technical Field

[0001] The invention relates to the technical field of chemical experiments, and in particular to a micro-negative pressure distillation device. Background Art

[0002] Distillation is a common experimental method in chemical laboratories, primarily used for liquid-liquid separation, solid-liquid separation, and reagent purification. Because the boiling point of reagents drops significantly under vacuum conditions, high-boiling-point reagents are typically separated and recovered using vacuum distillation. However, when the vacuum level is too high or the operation is improper, vacuum distillation can be prone to explosive boiling, contaminating the distillation equipment and fractions, reducing product yield and distillation efficiency. Furthermore, the vacuum system used in vacuum distillation emits a small amount of solvent vapor into the surrounding environment during operation. Improper control can endanger the surrounding environment and the health of the experimenters.

[0003] To effectively mitigate the hazards of bumping during vacuum distillation, relevant technical personnel have invented distillation equipment such as rotary evaporators. For example, a Chinese patent application discloses a rotary evaporator (CN 109759161B) that uses intersecting partitions to divide a recovery flask into multiple zones, and uses a diversion device to accurately direct the distillate into different recovery zones. This configuration not only effectively prevents the solvent in the diversion tube from flowing into two adjacent recovery zones during vacuum distillation, but also prevents cross-contamination of solvents within the recovery zones during solvent bumping. Furthermore, a rotary evaporator (CN 110215947B) published by the Chinese Patent Office prevents the solution in the rotary flask from being sprayed into the receiving flask due to bumping under reduced pressure conditions by providing a three-way connecting pipe between the condensing system and the rotating device, and installing a funnel-shaped device and a second circular plate in the connecting pipe. While the above work can alleviate the adverse effects of bumping on experiments in rotary evaporators to a certain extent, it does not fundamentally eliminate the bumping phenomenon during vacuum distillation and the solvent leakage problem of the vacuum system. Summary of the Invention

[0004] In view of the above-mentioned shortcomings of the prior art, the present invention provides a micro-negative pressure distillation device for solving the problems of the prior art. The provided micro-negative pressure distillation device mainly comprises a multi-port distiller, a condenser, a liquid collector, an air pump, an air supply pipe and a refrigeration pump connected to each other, so that volatile solvents can be efficiently distilled in the micro-negative pressure environment of the sealed distillation system, and can effectively eliminate the boiling phenomenon and solvent leakage problems of reduced pressure distillation. The effective benefits of the present invention are: the provided micro-negative pressure distillation device has the advantages of high working efficiency, simple operation and environmental friendliness.

[0005] To achieve the above object, the technical solution adopted by the present invention is:

[0006] Provided is a micro-negative pressure distillation device, comprising a multi-port distiller, a condenser, a liquid collector, an air pump, an air supply pipe and a refrigeration pump which are connected to each other.

[0007] Furthermore, the multi-port distiller of the present invention includes a distillation chamber, a vapor-liquid separation plate, an air guide port, a distillation port, a return air port and a liquid outlet; the condenser includes an air inlet, an air outlet, a refrigerant liquid inlet and a refrigerant liquid outlet; the air supply pipe includes an upper port, an expansion tube and a lower port; the liquid collector includes a liquid receiving port and a liquid collecting cavity.

[0008] Furthermore, the air supply pipe of the present invention has an outer wall of the expansion pipe sealedly connected to the inner wall of the return air port of the multi-port distiller, and the lower end of the air supply pipe extends into the distillation chamber of the multi-port distiller.

[0009] Furthermore, the vapor-liquid separation plate of the multi-port distiller of the present invention has air guide holes for allowing the solvent vapor in the distillation chamber of the multi-port distiller to pass through the vapor-liquid separation plate, while also guiding the liquefied solvent to the liquid outlet of the multi-port distiller.

[0010] Furthermore, the distillation ports of the multi-port distiller of the present invention are sealed and connected to the air inlet of the condenser, so as to introduce the steam passing through the vapor-liquid separation plate into the condenser.

[0011] Furthermore, in the condenser described in the present invention, the refrigerant liquid inlet and the refrigerant liquid outlet form a refrigeration circuit through a refrigeration pump, which is used to liquefy the solvent vapor in the condenser through heat exchange; the air outlet is sealed and connected to the air supply pipe through an air pump, which is used to perform heat exchange with the steam introduced from the distillation port, so that the solvent vapor is liquefied and refluxes to the upper surface of the vapor-liquid separation plate. At the same time, the non-condensable gas is driven by the air pump and returns to the distillation chamber of the multi-mouth distillation flask through the air supply pipe to re-participate in the micro-negative pressure distillation.

[0012] Furthermore, the liquid receiving port of the liquid collector of the present invention is sealed and connected to the liquid outlet of the multi-port distiller, and is used to receive the solvent that flows back through the upper surface of the vapor-liquid separation plate after being liquefied in the condenser, and transfer it to the liquid collecting cavity of the liquid collector.

[0013] Furthermore, the micro-negative pressure distillation device is a closed distillation system, and no solvent vapor is discharged outside the system during operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] In order to more clearly illustrate the technical solution of the present invention, the following briefly introduces the drawings required for use in the embodiments and application examples. Obviously, the drawings described below are some embodiments of the present invention. For relevant technical personnel, other drawings can be derived based on the present invention without paying any creative work.

[0015] Figure 1This is a schematic diagram of the overall structure of a micro-negative pressure distillation device provided by the present invention;

[0016] Figure 2 This is a structural schematic diagram of a multi-port distiller of a micro-negative pressure distillation device provided by the present invention;

[0017] Figure 3 This is a structural schematic diagram of an air supply pipe of a micro-negative pressure distillation device provided by the present invention;

[0018] Figures 1 to 3 Explanation of the reference numerals: 100: multi-port distiller; 101: distillation chamber; 102: vapor-liquid separation plate; 103: air guide hole; 104: distillation port; 105: air return port; 106: liquid outlet; 200: condenser; 201: air inlet; 202: air outlet; 203: refrigerant liquid inlet; 204: refrigerant liquid outlet; 300: liquid collector; 301: liquid receiving port; 302: liquid collecting chamber; 400: air pump; 500: air supply pipe; 501: upper port; 502: expansion pipe; 503: lower port; 600: refrigeration pump. DETAILED DESCRIPTION

[0019] To make the objectives, technical solutions, and advantages of the present invention more clear, the technical solutions of the present invention are described clearly and completely below with reference to the accompanying drawings. Obviously, the embodiments described are only some of the embodiments of the present invention, not all of them. All other embodiments derived by relevant technicians based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0020] In the description of the present invention, it should be noted that the terms "connected", "connected" and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integrated connection; it can be directly connected, indirectly connected through an intermediate medium, or connected internally between two components. Relevant technical personnel can understand the actual meaning of the above terms in the present invention based on the specific circumstances. Example 1

[0021] like Figures 1 to 3 The micro-negative pressure distillation device shown includes a multi-port distiller 100, a condenser 200, a liquid collector 300, an air pump 400, an air supply pipe 500 and a refrigeration pump 600 that are interconnected.

[0022] The multi-port distiller 100 includes a distillation chamber 101 , a vapor-liquid separation plate 102 , air guide holes 103 , a distillation port 104 , a gas return port 105 and a liquid outlet 106 .

[0023] The condenser 200 includes an air inlet 201 , an air outlet 202 , a refrigerant inlet 203 , and a refrigerant outlet 204 .

[0024] The air supply pipe 500 includes an upper port 501 , an expansion pipe 502 and a lower port 503 .

[0025] The liquid outlet 106 of the multi-port distiller 100 is sealed and communicated with the liquid receiving port 301 of the liquid collector 300 .

[0026] The air inlet 201 of the condenser 200 is sealed and connected to the distillation port 104 of the multi-port distiller 100, and the air outlet 202 is sealed and connected to the upper end 501 of the air supply pipe 500 through the air pump 400.

[0027] The condenser 200 , the refrigerant liquid inlet 203 and the refrigerant liquid outlet 204 form a refrigeration circuit through the refrigeration pump 600 .

[0028] The outer walls of the air supply pipe 500 and the expansion pipe 502 are sealedly connected to the inner wall of the air return port 105 of the multi-port distiller 100 , and the lower port 503 extends into the distillation chamber 101 of the multi-port distiller 100 .

[0029] The general operating method of the micro-negative pressure distillation device is as follows: The first step is to press Figure 1 Assemble the micro-negative pressure distillation device according to the connection relationship shown; second, place the distillation chamber 101 of the multi-port distiller 100 into a constant temperature stirrer and set the hot bath temperature and stirring speed; third, use a conduit to connect the refrigeration pump 600 with the refrigerant inlet 203 and the refrigerant outlet 204 of the condenser 200 and start the refrigeration pump 600; fourth, add an appropriate amount of the solution to be evaporated into the distillation chamber 101 through the return air port 105 of the multi-port distiller 100; fourth, when the temperature of the solution to be evaporated in the distillation chamber 101 and the temperature of the coolant in the condenser 200 reach the set value, turn on the air pump 400 to perform micro-negative pressure distillation in the closed distillation system of the micro-negative pressure distillation device.

[0030] The working principle of the micro-negative pressure distillation device is as follows: Driven by the air pump 400, the solvent vapor and non-condensable gas in the distillation chamber 101 enter the condenser 200 through the air guide hole 103 on the vapor-liquid separation plate 102; the solvent vapor is liquefied through heat exchange in the condenser 100 and flows back to the upper surface of the vapor-liquid separation plate 102, and then collected into the liquid collecting cavity 302 of the liquid collector 300 through the liquid outlet 106; the non-condensable gas is returned to the distillation chamber 101 through the air supply pipe 500 under the drive of the air pump 400 to participate in the micro-negative pressure distillation again. Since the liquefaction of the solvent vapor can generate a micro-negative pressure inside the closed evaporation system, the micro-negative pressure distillation device provided by the present invention can not only achieve efficient distillation of the solvent, but also effectively eliminate the risk of boiling in the reduced pressure distillation experiment. In addition, the closed evaporation system gives the micro-negative pressure distillation device provided by this patent the characteristics of environmental friendliness and high safety. Application Example 1

[0031] Deionized water was subjected to micro-negative pressure distillation using the micro-negative pressure distillation apparatus provided in Example 1. The volume of the distillation chamber 101 of the multi-port distiller 100 was 500 ml, the mass of the deionized water in the distillation chamber 101 was 200 g, the hot bath temperature was set to 60 degrees Celsius, and the coolant temperature was set to 5 degrees Celsius. When the micro-negative pressure distillation apparatus met the operating requirements, the air pump 400 and the refrigeration pump 600 were turned on to perform micro-negative pressure distillation of the deionized water. The experiment was repeated three times, and the average distillation rate was approximately 180 g / h, with an average recovery rate of approximately 95%. Application Example 2

[0032] Anhydrous ethanol was subjected to micro-negative pressure distillation using the micro-negative pressure distillation apparatus provided in Example 1. The volume of the distillation chamber 101 of the multi-port distiller 100 was 500 ml, the mass of the anhydrous ethanol in the distillation chamber 101 was 200 g, the hot bath temperature was set to 40 degrees Celsius, and the cold bath temperature was set to -5 degrees Celsius. When the micro-negative pressure distillation apparatus met the operating requirements, the air pump 400 and the refrigeration pump 600 were turned on to perform micro-negative pressure distillation of the anhydrous ethanol. The experiment was repeated three times, and the average distillation rate was approximately 260 g / h, with an average recovery rate of approximately 97%. Application Example 3

[0033] Using the micro-negative pressure distillation apparatus provided in Example 1 as the distillation equipment, dichloromethane was subjected to micro-negative pressure distillation. The volume of the distillation chamber 101 of the multi-port distiller 100 was 500 ml, the mass of dichloromethane in the distillation chamber 101 was 200 g, the hot bath temperature was set to 25 degrees Celsius, and the cold bath temperature was set to -20 degrees Celsius. When the micro-negative pressure distillation apparatus met the operating requirements, the air pump 400 and the refrigeration pump 600 were turned on to perform micro-negative pressure distillation of the dichloromethane. The experiment was repeated three times, with an average distillation rate of approximately 400 g / h and an average recovery rate of approximately 95%. Application Example 4

[0034] Ethyl acetate was subjected to micro-negative pressure distillation using the micro-negative pressure distillation apparatus provided in Example 1. The distillation chamber 101 of the multi-port distiller 100 had a capacity of 500 ml and contained 200 g of ethyl acetate. The hot bath temperature was set to 30°C, and the cold bath temperature was set to -15°C. When the micro-negative pressure distillation apparatus met operating requirements, the air pump 400 and the refrigeration pump 600 were turned on to continue micro-negative pressure distillation of the ethyl acetate. The experiment was repeated three times, resulting in an average distillation rate of approximately 380 g / h and an average recovery rate of approximately 97%. Application Example 5

[0035] Using the micro-negative pressure distillation apparatus provided in Example 1 as the distillation equipment, petroleum ether (boiling range: 60-90 degrees Celsius) was subjected to micro-negative pressure distillation. The volume of the still chamber 101 of the multi-port distiller 100 was 500 ml, the mass of the petroleum ether in the still chamber 101 was 200 grams, the hot bath temperature was set to 30 degrees Celsius, and the coolant temperature was set to -20 degrees Celsius. When the micro-negative pressure distillation apparatus met the operating requirements, the air pump 400 and the refrigeration pump 600 were turned on to perform micro-negative pressure distillation of the petroleum ether. The experiment was repeated three times, and the average distillation rate was approximately 350 grams per hour, and the average recovery rate was approximately 98%.

[0036] Finally, it should be noted that the present invention's description of the composition of the micro-negative pressure distillation device and the above-mentioned application examples have fully demonstrated that the micro-negative pressure distillation device provided by the present invention can be widely used in distillation experiments of various reagents. Due to space limitations, it is not possible to list the dimensions, connection methods, and micro-negative pressure experiments to which the micro-negative pressure distillation device provided by the present invention is applicable. Therefore, the above-mentioned embodiments and application examples are only used to illustrate the technical solution of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the above-mentioned embodiments and application examples, relevant technical personnel should understand that it is still possible to modify the technical solutions described in the above-mentioned embodiments, or to replace some of the technical features therein by equivalents. However, these modifications or equivalent replacements cannot cause the essence of the corresponding technical solution to deviate from the spirit and protection scope of the present invention.

Claims

1. A micro-negative pressure distillation device, characterized in that: The utility model comprises a multi-port distiller, a condenser, a liquid receiver, an air pump, an air supply pipe and a refrigeration pump which are interconnected.

2. A micro-negative pressure distillation device according to claim 1, characterized in that: The multi-port distiller comprises a distillation chamber, a vapor-liquid separation plate, a distillation port, a gas return port and a liquid outlet; the condenser comprises an air inlet, an air outlet, a refrigerant liquid inlet and a refrigerant liquid outlet; the air supply pipe comprises an upper port, an expansion pipe and a lower port; the liquid collector comprises a liquid receiving port and a liquid collecting cavity.

3. A micro-negative pressure distillation device according to claim 2, characterized in that: The multi-port distiller vapor-liquid separation plate has air guide holes for guiding the solvent liquefied in the condenser to the liquid collector through the liquid outlet, while allowing the solvent vapor to flow to the distillation port through the air guide holes.

4. A micro-negative pressure distillation device according to claim 2, characterized in that: The liquid collector has a liquid receiving port that is sealedly connected to the liquid outlet of the multi-port distiller; the condenser has an air inlet that is sealedly connected to the distillation port of the multi-port distiller, and an air outlet that is sealedly connected to the upper port of the air delivery pipe via an air pump; the refrigerant liquid inlet and the refrigerant liquid outlet form a refrigeration circuit via a cooling pump.

5. A micro-negative pressure distillation device according to claim 2, characterized in that: The lower end of the air delivery pipe extends into the distillation chamber through the return air port of the multi-port distiller, and the outer wall of the expansion pipe of the air delivery pipe is sealed and connected with the inner wall of the return air port of the multi-port distiller.

6. A slight negative pressure distillation device according to claim 2, characterized in that: The distillation system forms a closed system and no solvent vapor is discharged into the surrounding environment during operation.

7. A slight negative pressure distillation device according to claim 6, characterized in that: Its working principle is: when the distillation chamber temperature and coolant temperature of the multi-mouth distiller reach the set values, the solvent vapor and the circulating non-condensable gas inside the closed distillation system enter the condenser together under the push of the air pump, and the solvent vapor is liquefied inside the condenser and flows into the liquid collecting cavity of the liquid collector through the upper surface of the vapor-liquid distributor. The non-condensable gas is driven by the air pump to return to the multi-mouth distillation bottle through the air delivery pipe to participate in the micro-negative pressure distillation again.

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