High-speed distillation instrument

Abstract

The invention relates to the technical field of chemistry and chemical engineering experimental equipment, in particular to a high-speed distillation instrument which comprises a solvent evaporation system, a solvent condensation system and a controller which are associated with one another. The solvent evaporation system comprises a hot bath pool, an evaporation bottle, a two-way glass shaft, a locking mechanism, a driving motor and a steam guide bottle, and is used for evaporation of a volatile solvent and steam guide; the solvent condensing system comprises a bathing pool, a double-arm condenser, a cold liquid pump, an air pump and a collecting bottle and is used for condensing and recycling solvent steam; the controller is used for controlling the running states of the solvent evaporation system and the solvent condensation system, so that the volatile solvent is efficiently distilled and recycled in a closed environment in the high-speed distillation instrument. The high-speed distillation instrument provided by the invention has the beneficial effects that the bumping phenomenon of a rotary evaporator can be completely eradicated, and the high-speed distillation instrument has the advantages of high working efficiency, environment friendliness, high safety and the like.

Description

Technical Field

[0001] The invention relates to the technical field of chemical experimental equipment, in particular to a high-speed distillation apparatus. Background Art

[0002] The rotary evaporator, a device that effectively distills volatile reagents, is a common instrument in chemical laboratories, especially organic chemistry labs. The rotary evaporator's ability to effectively distill volatile reagents is primarily due to the following: 1. A high-temperature water bath heats the distillation flask, raising the temperature of the solution to be evaporated; 2. The solution to be evaporated forms a thin liquid film on the inner surface of the rotating flask, increasing the effective evaporation area for the volatile reagent; 3. A vacuum pump further reduces the pressure within the evaporation flask, increasing the evaporation rate of the volatile solvent; and 4. The reagent vapor is reliquefied in a low-temperature condenser and flows into a collection flask, enabling rapid distillation of the volatile reagent at a relatively low temperature. However, rotary evaporators generally have two disadvantages: 1. While providing a low-pressure environment for the rotary evaporator, the vacuum pump also releases large amounts of solvent vapor into the atmosphere. If not properly controlled, this can pose a risk to the surrounding environment, particularly the safety of laboratory personnel; 2. When the vacuum level within the evaporation flask and / or the water bath temperature exceed a certain level, the solution within the distillation flask can boil over, contaminating the rotary evaporator cavity and reducing product yield and equipment efficiency.

[0003] In order to reduce the contamination of the solvent in the recovery bottle and the loss of product caused by solvent bumping, National Patent 109759161B discloses a rotary evaporator that uses intersecting partitions to separate the recovery bottle into multiple areas, and accurately guides the distillate into different recovery areas through a diversion device. This setting can not only effectively prevent the solvent in the diversion tube from flowing into two adjacent recovery areas during the reduced pressure distillation of the rotary evaporator, but also prevent the solvents in the recovery areas from contaminating each other when the solvent bumps. In addition, National Patent 110215947B discloses a rotary evaporator that prevents the solution in the rotary bottle from spraying into the condenser and solvent receiving bottle due to bumping under reduced pressure conditions by providing a three-way receiving pipe between the condensation system and the rotary device, and providing a funnel-shaped device and a second circular plate in the receiving pipe. However, these patent designs cannot fundamentally eliminate the bumping phenomenon of the rotary evaporator and the hazards of volatile solvent leakage. Summary of the Invention

[0004] In view of the above-mentioned shortcomings of the prior art, the present invention provides a high-speed distiller to address these issues. The high-speed distiller comprises an interconnected solvent evaporation system, a solvent condensation system, and a controller, enabling high-speed distillation and recovery of volatile solvents in a closed environment. The present invention also offers the advantages of high efficiency, environmental friendliness, and safety, while eliminating the bumping phenomenon associated with rotary evaporators.

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

[0006] A high-speed distillation apparatus is provided, comprising a solvent evaporation system, a solvent condensation system and a controller which are interconnected.

[0007] Furthermore, the solvent evaporation system of the present invention comprises a heat bath, an evaporating flask, a two-way glass shaft, a locking mechanism, a drive motor and a steam guide bottle, and is used for heating and evaporating volatile solvents.

[0008] Furthermore, the hot bath of the solvent evaporation system of the present invention is used to hold high-temperature media and provide a high-temperature environment for the evaporation flask.

[0009] Furthermore, the evaporating bottle of the solvent evaporation system of the present invention has a bottle mouth connected to the steam guide bottle through a two-way glass shaft and is placed in a hot bath for containing the solvent to be evaporated.

[0010] Furthermore, the two-way glass shaft of the solvent evaporation system of the present invention is fixed inside the locking mechanism, and can drive the evaporating flask to rotate around the shaft at a controlled speed under the drive of the drive motor.

[0011] Furthermore, the steam guide bottle of the solvent evaporation system described in the present invention includes a steam guide port, a return air pipe and a main connection port, which is tightly connected to the locking mechanism through the main connection port, and is used for steam diversion and circulation of non-condensable gas between the solvent evaporation system and the solvent condensation system.

[0012] Furthermore, the solvent condensation system of the present invention comprises a cold bath, a double-arm condenser, a cold liquid pump, a collecting bottle and an air pump, which are used for condensing and recovering solvent vapor.

[0013] Furthermore, the cold bath of the solvent condensation system of the present invention is used to hold coolant and provide a low-temperature environment for the double-arm condenser.

[0014] Furthermore, the double-arm condenser of the solvent condensation system described in the present invention includes a "U"-shaped external heat exchange tube, two internal condensation tubes and a liquid collecting pipe, which is immersed in the coolant contained in the cold bath, and is mainly used for heat exchange between solvent vapor and coolant, thereby increasing the liquefaction efficiency of solvent vapor.

[0015] Furthermore, the "U"-shaped external heat exchange tube of the present invention has a steam inlet and an air outlet at both ends respectively; the steam inlet is connected to the steam guide port of the steam bottle and is used to receive the solvent vapor sent from the steam guide port; the air outlet is connected to the steam return pipe of the steam bottle and is used to re-introduce the non-condensable gas in the solvent condensation system into the evaporation flask.

[0016] Furthermore, the inner heat exchange tube of the present invention is located in the straight tubes on both sides of the "U"-shaped outer heat exchange tube; the two ends of the inner heat exchange tube extend out of the side walls of the outer heat exchange tube, respectively serving as the liquid inlet and liquid outlet of the inner heat exchange tube; the liquid inlet and liquid outlet are respectively used for the coolant to flow into and out of the inner heat exchange tube of the double-arm condenser.

[0017] Furthermore, the solvent condensation system cold liquid pump of the present invention is connected to the liquid outlet of an internal heat exchange tube at one end and to the liquid inlet of another internal heat exchange tube at the other end, and is used to drive the circulation of the coolant between the cold bath and the internal heat exchange tube, thereby increasing the heat exchange efficiency of the double-arm condenser.

[0018] Furthermore, the double-arm condenser liquid collecting pipe of the present invention is connected to the collecting bottle and is used to introduce the liquefied solvent in the double-arm condenser into the collecting bottle.

[0019] Furthermore, the air pump of the solvent condensation system of the present invention has an air inlet and an air outlet connected to the air outlet of the double-arm condenser and the air return pipe of the steam guide bottle respectively, and is used to drive the non-condensable gas to circulate between the solvent evaporation system and the solvent condensation system.

[0020] Furthermore, the controller of the present invention is used to control the switches and working states of all power-consuming modules. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] 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.

[0022] Figure 1 This is a schematic structural diagram of a high-speed distillation apparatus provided by the present invention;

[0023] Figure 2 This is a structural schematic diagram of a high-speed distillation solvent evaporation system provided by the present invention;

[0024] Figure 3 This is a schematic structural diagram of a high-speed distillation solvent condensation system provided by the present invention;

[0025] Figures 1 to 3Explanation of the reference numerals: 100: solvent evaporation system; 110: hot bath; 120: evaporating flask; 130: two-way glass shaft; 140: locking mechanism; 150: driving motor; 160: steam guide bottle; 161: main connection port; 162: steam guide port; 163: return air pipe; 200: solvent condensation system; 210: cold bath; 220: double-arm condenser; 221: steam inlet; 222: air outlet; 223a, 223b: internal heat exchange tube; 224: "U"-shaped external heat exchange tube; 225a, 225b: liquid inlet; 226a, 226b: liquid outlet; 227: liquid collecting pipe; 230: cold liquid pump; 240: air pump; 250: liquid collecting bottle; 300: controller. DETAILED DESCRIPTION

[0026] 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 embodiments of the present invention, not all embodiments. All other embodiments obtained by relevant technicians based on the embodiments provided by the present invention without inventive efforts are within the scope of protection of the present invention.

[0027] In the description of the present invention, it should be noted that, unless otherwise clearly stipulated and limited, terms such as "connection" and "communication" 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 a direct connection, an indirect connection through an intermediate medium, or a communication between the two elements; directional words such as "upper", "lower" and "both sides" are based on the drawings in the specification, and relevant technical personnel can understand the actual meaning of the above terms in the present invention according to the specific circumstances. Example 1

[0028] like Figures 1 to 3 As shown, a high-speed distiller comprises a solvent evaporation system 100, a solvent condensation system 200 and a controller 300 which are interconnected and integrated.

[0029] The solvent evaporation system 100 includes a hot bath 110, an evaporating flask 120, a two-way glass shaft 130, a locking mechanism 140, a drive motor 150 and a steam guide bottle 160; the solvent condensation system 200 includes a cold bath 210, a double-arm condenser 220, a cold liquid pump 230, an air pump 240 and a collecting bottle 250.

[0030] The two-way glass shaft 130 is fixed inside the locking mechanism 140 , with its lower end connected to the evaporation flask 120 and its upper end connected to the main connection port 161 of the steam guide bottle 160 , and rotates around the shaft at a controlled speed under the drive motor 150 .

[0031] The steam guide bottle 160 includes a main connection port 161 , a steam guide port 162 and a return air pipe 163 . The steam guide port 162 is connected to the steam inlet 221 of the condenser 220 , and the return air pipe 163 is connected to the air outlet 222 of the condenser 220 through the air pump 240 .

[0032] The double-arm condenser 220 includes a steam inlet 221 , a gas outlet 222 , inner heat exchange tubes 223 a and 223 b , a “U”-shaped outer heat exchange tube 224 , cold liquid inlets 225 a and 225 b , cold liquid outlets 226 a and 226 b , and a liquid collecting pipe 227 .

[0033] The two ends of the cold liquid pump 230 are connected to the liquid outlet 226a and the liquid inlet 225b respectively. When turned on, it can drive the coolant to circulate between the cold bath 210 and the internal heat exchange pipes 223a and 223b, thereby increasing the condensation efficiency of the double-arm condenser 220.

[0034] The two ends of the air pump 240 are connected to the return air pipe 163 and the air outlet 222 respectively. When turned on, the air pump 240 can drive the non-condensable gas to circulate between the solvent evaporation system and the solvent condensation system.

[0035] The collecting bottle 250 is communicated with the liquid collecting tube bottle 227 of the double-arm condenser 220 and is used to collect the liquefied solvent in the double-arm condenser 220 .

[0036] The controller 300 controls the operating temperatures of the hot bath 110 and the cold bath 210 and the start and stop and operating states of the drive motor 150 , the cold liquid pump 230 and the air pump 240 through a preset program.

[0037] The general operation method and working principle of the high-speed distillation apparatus are as follows: The first step is to clean and dry the glass components of the high-speed distiller's solvent evaporation system and solvent evaporation condensation system, and press Figure 1The hot bath 110 and the cold bath 210 are connected to each other in the cold bath. The hot bath 110 and the cold bath 210 are connected to each other in the cold bath. The hot bath 110 and the cold bath 210 are connected to each other in the cold bath. The hot bath 110 and the cold bath 210 are connected to each other in the cold bath. The cold ... The evaporating flask 120 is driven at a set speed, rotating around the axis of the two-way glass shaft 130. In step 7, when the temperatures of the heating bath 110 and the cooling bath 210 reach the set temperature, the cryogenic pump 230 is turned on to circulate the coolant between the cooling bath 210 and the inner heat exchange tubes 223a and 223b of the double-arm condenser 220. In step 8, the air pump 240 is turned on to drive the solvent vapor and non-condensable gas in the evaporating flask 120 through the two-way glass shaft 130, the steam guide tube 162 of the steam guide bottle 160, and the steam inlet 221, into the double-arm condenser 220. The solvent vapor is liquefied through heat exchange between the inner heat exchange tubes 223a and 223b and the outer heat exchange tube 224, and flows through the liquid collecting pipe 227 into the collection bottle 250. Driven by the air pump 240, the non-condensable gas enters the evaporating flask 120 through the gas outlet 222 and the gas return pipe 163 and rejoins the solvent distillation. Application Example 1

[0038] A deionized water distillation experiment was conducted using the high-speed distiller provided in Example 1 as the solvent distillation equipment. The evaporating flask 120 was a 1000 ml ground-jaw eggplant-shaped flask containing 500 g of deionized water. The collecting flask 250 was a 1000 ml round-bottom flask with a ball-milled finish. The temperature of the hot bath 110 was set to 90°C, the temperature of the cold bath 210 was set to 5°C, and the speed of the evaporating flask 120 was set to 60 rpm. When the temperatures of the hot bath 110 and cold bath 210 reached the set values, the cooling liquid pump 230 and the air pump 240 were turned on to distill the deionized water. The experiment was repeated three times. The average distillation rate was approximately 350 g / h, and the average recovery rate was approximately 97%. Application Example 2

[0039] An experiment was conducted distilling anhydrous ethanol using the high-speed distiller provided in Example 1. The evaporating flask 120 was a 1000 ml ground-jaw eggplant-shaped flask containing 500 g of anhydrous ethanol. The collecting flask 250 was a 1000 ml round-bottom flask with a ball-milled finish. The temperature of the hot bath 110 was set to 80 degrees Celsius, the temperature of the cold bath 210 was set to -20 degrees Celsius, and the speed of the evaporating flask 120 was set to 60 rpm. When the temperatures of the hot bath 110 and cold bath 210 reached the set values, the cooling liquid pump 230 and the air pump 240 were turned on to distill the anhydrous ethanol. The experiment was repeated three times. The average distillation rate was approximately 500 g / h, and the average recovery rate was approximately 96%. Application Example 3

[0040] A distillation experiment of dichloromethane was conducted using the high-speed distiller provided in Example 1. The evaporating flask 120 was a 1000 ml ground-jaw eggplant-shaped flask containing 500 g of dichloromethane. The collecting flask 250 was a 1000 ml round-bottom flask with a ball-milled finish. The temperature of the hot bath 110 was set to 50°C, the temperature of the cold bath 210 was set to -20°C, and the speed of the evaporating flask 120 was set to 60 rpm. When the temperatures of the hot bath 110 and cold bath 210 reached the set values, the cooling liquid pump 230 and the air pump 240 were turned on to distill the dichloromethane. The experiment was repeated three times. The average distillation rate was approximately 1000 g / h, and the average recovery rate was approximately 98%. Application Example 4

[0041] Ethyl acetate was distilled using the high-speed distiller provided in Example 1. The evaporating flask 120 was a 1000 ml ground-jaw eggplant-shaped flask containing 500 g of ethyl acetate. The collecting flask 250 was a 1000 ml round-bottom flask with a ball-milled finish. The temperature of the hot bath 110 was set to 70°C, the temperature of the cold bath 210 was set to -15°C, and the speed of the evaporating flask 120 was set to 60 rpm. When the temperatures of the hot bath 110 and cold bath 210 reached the set values, the cooling pump 230 and the air pump 240 were turned on to distill the ethyl acetate. The experiment was repeated three times. The average distillation rate was approximately 900 g / h, and the average recovery rate was approximately 97%. Application Example 5

[0042] A distillation experiment was conducted on petroleum ether (boiling range: 60-90°C) using the high-speed distiller provided in Example 1. The evaporating flask 120 was a 1000 ml ground-jaw eggplant-shaped flask containing 500 g of petroleum ether. The collecting flask 250 was a 1000 ml round-bottom flask with a ball-milled finish. The temperature of the hot bath 110 was set to 80°C, the temperature of the cold bath 210 was set to -15°C, and the speed of the evaporating flask 120 was set to 60 rpm. When the temperatures of the hot bath 110 and cold bath 210 reached the set values, the cooling liquid pump 230 and the air pump 240 were turned on to distill the petroleum ether. The experiment was repeated three times. The average distillation rate was approximately 1500 g / h, and the average recovery rate was approximately 98%.

[0043] Finally, it should be noted that the present invention's description of the structure and composition of the high-speed distiller and the above-mentioned application examples have fully demonstrated that the high-speed distiller provided by the present invention can be widely used for the high-speed distillation of various volatile reagents. Due to space limitations, it is not possible to list the dimensions, connection methods, and applicable solvents of the solvent evaporation system and solvent condensation system involved in the present invention one by one. 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 with equivalents. However, these modifications or equivalent replacements do not deviate the essence of the corresponding technical solution from the spirit and protection scope of the present invention.

Claims

1. A high-speed distillation apparatus, characterized in that: The invention comprises an interrelated integrated design of solvent evaporation system, solvent condensation system and controller.

2. A high-speed distillation apparatus according to claim 1, characterized in that: The solvent evaporation system comprises some or all accessories including a hot bath, an evaporating flask, a two-way glass shaft, a locking mechanism, a driving motor and a steam guide bottle; preferably, all accessories are assembled.

3. A high-speed distillation apparatus according to claim 1, characterized in that: The solvent condensation system comprises some or all accessories including a cold bath, a double-arm condenser, a cold liquid pump, an air pump and a collecting bottle; preferably, all accessories are assembled.

4. A high-speed distillation apparatus according to claim 1, characterized in that: The solvent evaporation system and the solvent condensation system can form a closed solvent distillation system.

5. A high-speed distillation apparatus according to claim 3, characterized in that: The double-arm condenser comprises a U-shaped outer heat exchange tube, two inner heat exchange tubes and a liquid collecting tube.

6. A high-speed distillation apparatus according to claim 3, characterized in that: The solvent condensation system's double-arm condenser is placed within the cold bath. A cooling liquid pump circulates the coolant through the inner heat exchange tubes and the cold bath, utilizing the dual condensation effect of the "U"-shaped outer and inner heat exchange tubes to enhance the liquefaction efficiency of the solvent vapor.

7. A high-speed distillation apparatus according to claim 1, characterized in that: The solvent vapor and non-condensable gas inside the closed distillation system enter the double-arm condenser under the push of the air pump, the solvent vapor is liquefied in the double-arm condenser and flows into the liquid collecting bottle through the liquid collecting pipe, while the non-condensable gas returns to the evaporation bottle through the air outlet of the double-arm condenser, the air pump and the return air pipe to participate in the solvent distillation again, thereby realizing the rapid distillation of the volatile solvent.

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