Environment-friendly continuous distillation instrument

Abstract

The invention relates to the technical field of chemistry and chemical engineering, in particular to an environment-friendly continuous distillation instrument which comprises a distillation assembly and an integrated control assembly which are associated with each other. The decompression filtering assembly comprises a solvent receiving bottle, a decompression funnel, a sealing cover and a pressure balancer; the distillation assembly comprises a stock solution storage bottle, a distillation bottle, a distillation head, a dustproof assembly, a primary condenser, a secondary condenser, a flow divider, a liquid collection bottle and a fraction storage bottle; the integrated control assembly comprises a hot bathing pool, a cold bathing pool, a cooling liquid conveying pump, a circulating air pump, an air pressure sensor, a stock solution adding pump, a fraction conveying pump, a liquid level sensing assembly and a comprehensive controller. Through coordinated operation of the components, the provided environment-friendly continuous distillation instrument can realize lossless, efficient and continuous distillation of a liquid-phase reagent, and has important significance in improving the working environment of a chemistry and chemical engineering laboratory and promoting rapid development of healthy chemistry.

Description

Technical Field

[0001] This invention relates to the field of chemical and chemical engineering experimental technology, specifically to an environmentally friendly continuous distillation apparatus. Background Technology

[0002] Distillation, a commonly used separation and purification method in the chemical industry, is widely applied in chemical synthesis, extraction of active ingredients from traditional Chinese medicine, and petrochemical production. Common distillation methods can be broadly categorized into atmospheric distillation and vacuum distillation. Although the instruments and operating procedures differ slightly between these two methods, they share a similar working principle: converting the component to be distilled into vapor, then condensing it into a liquid and allowing it to flow into a collection flask. To prevent the component from rapidly expanding and damaging the equipment during distillation, the distillation apparatus is usually not completely sealed, resulting in a relatively high vapor leakage rate. To improve distillation efficiency and reduce distillation temperature (reducing energy consumption), vacuum distillation is often used to achieve rapid distillation of high-boiling-point solvents under lower pressure or even high vacuum conditions. Maintaining the vacuum conditions required for vacuum distillation results in more solvent vapor being released from the distillation apparatus. To avoid environmental pollution, tail gas absorption devices can be installed on the distillation equipment to treat harmful gases, or ventilation equipment can be used to remove harmful gases from the experimental site. For example, a Chinese invention patent titled "A Vacuum Distillation Tail Gas Condensation Device" (patent number: CN220238184U) provides a tail gas condensation device including a support and a bottle body. The collection and state of the solvent inside the bottle can be easily observed through a glass window on the bottle body. To address the problem that vacuum distillation equipment is not conducive to continuous distillation experiments, a utility model patent titled "An Automatic Drainage and Receiving Device" (patent number: 217340106U) adds a pressure balancing device to the receiving device. During distillation, air can be directly introduced into the receiving container without stopping the vacuum pump, draining the ethylene glycol in the receiving container to the storage tank, thus achieving continuous distillation. However, these inventions do not completely solve the problem of solvent leakage in distillation equipment. A patent application titled "A High-Speed ​​Distillation Apparatus" (application number: 202510905641X) proposes using a "point-to-point" distillation method, which not only enables high-speed distillation and recovery of volatile solvents in a closed environment but also successfully overcomes the technical problem of solvent leakage. However, the patent application still has three defects: 1) It is not suitable for solvent distillation of solid-liquid mixed systems; 2) The double-effect condenser needs to be embedded in the cold bath, which is not easy to disassemble and clean, and also increases the risk of coolant leakage; 3) It cannot perform continuous distillation, which is not conducive to mass production. Summary of the Invention

[0003] To address the aforementioned technical deficiencies and promote the rapid development of "healthy chemistry," this invention provides an environmentally friendly continuous distillation apparatus. This apparatus comprises interconnected rapid distillation components and integrated control components, enabling continuous distillation and efficient recovery of volatile solvents within a closed system. Furthermore, the external double-effect condenser facilitates regular equipment maintenance and reduces the risk of coolant leakage. More importantly, this environmentally friendly continuous distillation apparatus is equipped with a dustproof component, making it better suited for continuous distillation of solid-liquid mixtures. In summary, the benefits of this invention are: the provided environmentally friendly continuous distillation apparatus offers advantages such as high efficiency, wide applicability, environmental friendliness, and high safety, and is of great significance for improving the working environment of chemical engineering laboratories and enhancing distillation efficiency.

[0004] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0005] An environmentally friendly continuous distillation apparatus is provided, comprising interconnected rapid distillation components and integrated control components.

[0006] Furthermore, the rapid distillation assembly of the present invention includes a stock solution storage bottle, a distillation flask, a distillation head, a dustproof assembly, a primary condenser, a secondary condenser, a distributor, a collection bottle, and a fraction storage bottle.

[0007] Furthermore, the stock solution storage bottle of the present invention is a liquid storage tank or reaction vessel including a stock solution addition port and a discharge port. Its material can be stainless steel, ceramic, glass, or polytetrafluoroethylene (PTFE), preferably glass or PTFE, more preferably glass, with a volume of not less than 1 liter, preferably 1-50 liters, more preferably 10 liters. The stock solution addition port is a connection port with pressure balancing function, with an outer diameter of 6-200 mm, preferably 8-100 mm, more preferably 50 mm; the discharge port is a two-way corrosion-resistant shut-off valve, a straight connecting pipe, or a pagoda-shaped connecting pipe, preferably a two-way corrosion-resistant shut-off valve, with an outer diameter of 6-50 mm, preferably 8-30 mm, more preferably 12 mm.

[0008] Furthermore, the distillation flask of the present invention is a multi-necked glass bottle or reaction vessel comprising a distillation port, a return gas pipe, and a raw material addition port, preferably a multi-necked glass bottle with a volume of not less than 200 ml, preferably 200–1000 ml, and more preferably 500 ml. The distillation port is a flange-type glass connection port with an outer diameter of 30–150 mm, preferably 40–100 mm, and more preferably 50 mm; the return gas pipe and the raw material addition port are straight connecting pipes, pagoda-type connecting pipes, or polytetrafluoroethylene shut-off valves, preferably pagoda-type connecting pipes with an outer diameter of 6–30 mm, preferably 8–20 mm, and more preferably 12 mm.

[0009] Furthermore, the distillation head of the present invention includes a steam inlet and a steam outlet. The included angle between the steam inlet and the steam outlet is 20 to 85 degrees, preferably 30 to 80 degrees, and more preferably 70 degrees; the steam inlet is a flange-type glass connection with an outer diameter of 30 to 150 mm, preferably 40 to 100 mm, and more preferably 50 mm; the steam outlet is a conical ground glass tube with a maximum outer diameter of 12 to 60 mm, preferably 16 to 40 mm, and more preferably 24 mm.

[0010] Furthermore, the dustproof assembly of the present invention includes a dustproof plate and a flange clamp. The dustproof plate is a glass frosted plate, filter paper, PTFE-clad metal filter screen, polymer filter screen, PTFE-clad porous plate, or a combination thereof, preferably a combination of filter paper and PTFE-clad metal filter screen, with an outer diameter of 30-150 mm, preferably 40-100 mm, and more preferably 50 mm; the flange clamp can be a plate flange clamp, a split flange clamp, or a three-piece interlocking flange clamp, preferably a three-piece interlocking flange clamp.

[0011] Furthermore, the primary and secondary condensers of this invention are double-effect heat exchange tubes with tapered ground glass tubes fused at both ends, mainly used for heat exchange between solvent vapor and coolant, increasing the liquefaction efficiency of solvent vapor. The double-effect heat exchange tube consists of four layers of glass tubing, from the outside in: a first layer of glass tube, a second layer of glass tube, a third layer of glass tube, and a fourth layer of glass tube. A pagoda-shaped connecting tube is vertically fused to the lower end of the sidewall of the first layer of glass tube and the upper end of the sidewall of the second layer of glass tube, serving as the coolant inlet and outlet. The upper end of the sidewall of the second layer of glass tube is connected to the top of the fourth layer of glass tube via a thin glass tube. The bottom of the fourth layer of glass tube opens inside the bottom of the third layer of glass tube, the bottom of the third layer of glass tube is closed, and its top vertically passes through the second layer of glass tube. The glass tube sidewall is connected to the coolant outlet; the outer diameter of the first layer of glass tube is 20-180 mm, preferably 20-100 mm, more preferably 50 mm; the outer diameter of the second layer of glass tube is 16-170 mm, preferably 16-90 mm, more preferably 35 mm; the outer diameter of the third layer of glass tube is 12-160 mm, preferably 12-80 mm, more preferably 20 mm; the outer diameter of the fourth layer of glass tube is 8-140 mm, preferably 8-70 mm, more preferably 12 mm; the outer diameter of the pagoda-shaped connecting pipe is 6-30 mm, preferably 8-20 mm, more preferably 12 mm; the maximum diameter of the ground joint of the tapered ground glass tube is 12-60 mm, preferably 16-40 mm.

[0012] Furthermore, the diverter of the present invention comprises two collecting pipes and one drain pipe. The collecting pipes are tapered ground glass tubes with a maximum inner diameter of 12–60 mm, preferably 16–40 mm, and more preferably 34 mm; the included angle between the two collecting pipes is in the range of 0°–90°, preferably in the range of 0°–30°, and more preferably 0°; the drain pipe is a downwardly extending tapered ground glass tube or a glass bulb ground joint, preferably a tapered ground glass tube with a maximum outer diameter of 12–60 mm, preferably 16–40 mm, and more preferably 24 mm; the maximum outer diameter of the glass bulb ground joint is 20–60 mm, preferably 24–40 mm, and more preferably 28 mm.

[0013] Furthermore, the liquid collecting bottle of the present invention is a glass bottle comprising a receiving tube and a draining tube, with a volume of not less than 200 ml, preferably 100-1000 ml, and more preferably 500 ml. The receiving tube is a conical ground glass tube or a glass ball grinding bowl, preferably a conical ground glass tube, with a maximum inner diameter of 12-60 mm, preferably 16-40 mm, and more preferably 24 mm; the glass ball grinding bowl has a maximum inner diameter of 20-60 mm, preferably 24-40 mm, and more preferably 28 mm; the draining tube is a polytetrafluoroethylene shut-off valve or a pagoda-shaped connecting pipe fused to the bottom of the receiving bottle, preferably a polytetrafluoroethylene shut-off valve, with an outer diameter of 6-30 mm, preferably 8-20 mm, and more preferably 12 mm.

[0014] Furthermore, the distillate storage bottle of the present invention is a liquid storage tank with a distillate inlet, and its material can be stainless steel, ceramic, glass or polytetrafluoroethylene, preferably glass or polytetrafluoroethylene, more preferably glass, with a volume of not less than 1 liter, preferably 1 to 50 liters, more preferably 10 liters; the distillate inlet is a connection port with pressure balancing function, and its outer diameter is 6 to 200 mm, preferably 8 to 100 mm, more preferably 50 mm.

[0015] Furthermore, the integrated control component of the present invention includes a hot bath, a cold bath, a coolant delivery pump, a circulating air pump, a pressure sensor, a raw material addition pump, a fraction delivery pump, a liquid level sensing component, and a comprehensive controller.

[0016] Furthermore, the hot bath of the present invention is a barrel-shaped container with magnetic stirring function for holding the hot bath medium, and its volume is not less than 1 liter, preferably 2 to 10 liters, and more preferably 2 liters; the temperature adjustment range of the hot bath medium is room temperature to 200 degrees Celsius, preferably room temperature to 150 degrees Celsius, and more preferably room temperature to 100 degrees Celsius; the magnetic stirring speed adjustment range is 0 to 3000 revolutions per minute, preferably 0 to 1800 revolutions per minute, and more preferably 0 to 1000 revolutions per minute.

[0017] Furthermore, the cold bath of the present invention is a low-temperature container with an outlet and an inlet for holding coolant, and its volume is not less than 1 liter, preferably 2 to 50 liters, and more preferably 5 liters; the temperature adjustment range of the coolant is -25 degrees Celsius to room temperature, preferably -20 to 10 degrees Celsius, and more preferably -10 to 0 degrees Celsius.

[0018] Furthermore, the coolant delivery pump of the present invention can be a centrifugal pump, a plunger pump or a peristaltic pump, preferably a centrifugal pump; its liquid delivery rate is 0 to 8000 ml per minute, preferably 0 to 6000 ml per minute, and more preferably 1000 ml per minute.

[0019] Furthermore, the circulating air pump of the present invention can be a centrifugal pump, a reciprocating pump or a diaphragm pump, preferably a diaphragm pump; its gas delivery rate is 0 to 120 liters per minute, preferably 0 to 60 liters per minute, and more preferably 18 liters per minute.

[0020] Furthermore, the pressure sensor described in this invention is a resistive sensor or a non-resistive sensor, preferably a resistive sensor, with a pressure detection range of -0.1 to 1.0 MPa, more preferably 0 to 0.1 MPa.

[0021] Furthermore, the stock solution addition pump and the fraction transfer pump described in this invention can be centrifugal pumps, plunger pumps or peristaltic pumps, preferably peristaltic pumps, with a liquid delivery rate of 0 to 1500 ml per minute, preferably 0 to 1000 ml per minute, and more preferably 300 ml per minute.

[0022] Furthermore, the liquid level sensing component of the present invention includes three liquid level gauges. The liquid level gauges can be capacitive liquid level gauges, resistive liquid level gauges, or photosensitive liquid level gauges, preferably capacitive liquid level gauges and photosensitive liquid level gauges, more preferably capacitive liquid level gauges. Their sensing method is contact sensing or non-contact sensing, preferably non-contact sensing.

[0023] Furthermore, the integrated controller described in this invention can be an integrated circuit board with display function or a programmable logic controller, preferably a programmable logic controller with display function, used to control the switching and working status of all working modules. Attached Figure Description

[0024] To more clearly illustrate the technical solution of the present invention, the accompanying drawings used in the embodiments and application examples will be briefly introduced below. Obviously, the accompanying drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be derived from the present invention without creative effort.

[0025] Figure 1This is a schematic diagram of the overall structure of an environmentally friendly continuous distillation apparatus provided by the present invention;

[0026] Figure 2 This is an exploded structural diagram of the rapid distillation component of an environmentally friendly continuous distillation apparatus provided by the present invention;

[0027] Figure 3 This is a schematic diagram of the composition structure of an integrated control component for an environmentally friendly continuous distillation apparatus provided by the present invention;

[0028] Figures 1-3 Figure labeling: 100: Rapid distillation assembly; 110: Stock solution storage bottle; 111: Stock solution addition port; 112: Discharge port; 120: Distillation flask; 121: Distillation port; 122: Return gas pipe; 123: Feed inlet; 130: Distillation head; 131: Steam inlet; 132: Steam outlet; 140: Dustproof assembly; 141: Dustproof plate; 142: Flange clamp; 150: Primary condenser; 160: Secondary condenser; 151, 152, 161, 162: Ground glass tubes; 153, 163: First layer glass tubes; 154, 164: Second layer glass tubes; 155, 165: Third layer glass tubes; 156, 166: Fourth layer glass tubes; 1 57, 167: Coolant inlet; 158, 168: Coolant outlet; 170: Diverter; 171, 172: Collector; 173: Drain; 180: Collector bottle; 181: Receiving pipe; 182: Drain; 190: Distillate storage bottle; 191: Distillate inlet; 200: Integrated control unit; 210: Hot bath; 220: Cold bath; 221: Outlet; 222: Return outlet; 230: Coolant transfer pump; 240: Circulating air pump; 250: Pressure sensor; 260: Raw material addition pump; 270: Distillate transfer pump; 280: Level sensing unit; 281, 282, 283: Level gauge; 290: Integrated controller. Detailed Implementation

[0029] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are some, but not all, embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments provided by this invention without creative effort are within the protection scope of this invention.

[0030] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, terms such as "connection" and "connection" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integrated connection; they can refer to a direct connection, an indirect connection through an intermediate medium, or a connection within two components; directional terms such as "upper," "lower," "bottom," "top," "side," and "inner" are based on the accompanying drawings in the specification, and those skilled in the art can understand the actual meaning of the above terms in this invention according to the specific circumstances. Example 1

[0031] like Figures 1-3 As shown, an environmentally friendly continuous distillation apparatus includes an interconnected rapid distillation component 100 and an integrated control component 200.

[0032] The rapid distillation assembly 100 includes a stock solution storage bottle 110, a distillation flask 120, a distillation head 130, a dustproof assembly 140, a primary condenser 150, a secondary condenser 160, a distributor 170, a collection bottle 180, and a fraction storage bottle 190.

[0033] The stock solution storage bottle 110 is a 10-liter glass storage tank containing a stock solution inlet 111 and a discharge outlet 112; the stock solution inlet 111 is a connection port with a pressure balancing function and an outer diameter of 50 mm; the discharge outlet 112 is a two-way corrosion-resistant shut-off valve with an outer diameter of 12 mm.

[0034] The distillation flask 120 is a 500 ml three-necked glass bulb flask containing a distillation port 121, a return gas pipe 122, and a feed port 123. The distillation port 121 is a flanged glass connection port with an outer diameter of 50 mm, and the return gas pipe 122 and the feed port 123 are pagoda-shaped glass tubes with an outer diameter of 12 mm.

[0035] The distillation head 130 includes a steam inlet 131 and a steam outlet 132 with an included angle of 70 degrees. The steam inlet 131 is a flange-type glass connection with an outer diameter of 50 mm. The steam outlet 132 is a conical external ground glass tube with a maximum outer diameter of 24 mm.

[0036] The dustproof assembly 140 includes a dustproof plate 141 and a flange clamp 142. The dustproof plate 141 is composed of a PTFE-clad metal filter screen and filter paper with an outer diameter of 50 mm; the flange clamp 142 is a three-piece interlocking flange clamp.

[0037] The primary condenser 150 comprises a double-effect heat exchange tube consisting of a conical inner ground glass tube 151 with a maximum inner diameter of 24 mm and a conical outer ground glass tube 152 with a maximum outer diameter of 34 mm. The double-effect heat exchange tube is a nested system of four layers of glass tubes, from the outside in: a first layer 153 with an outer diameter of 50 mm, a second layer 154 with an outer diameter of 35 mm, a third layer 155 with an outer diameter of 20 mm, and a fourth layer 156 with an outer diameter of 12 mm. In this system, a pagoda-shaped connecting pipe with an outer diameter of 12 mm is vertically fused to the lower end of the side wall of the first glass tube 153 and the upper end of the side wall of the second glass tube 154, serving as the coolant inlet 157 and the coolant outlet 158, respectively; the upper end of the side wall of the second glass tube 154 is connected to the top of the fourth glass tube 156 through a glass tube with an outer diameter of 10 mm; the bottom of the fourth glass tube 156 is open inside the bottom of the third glass tube 155; the bottom of the third glass tube 155 is closed, and the top passes vertically through the side wall of the second glass tube 154, connecting to the coolant outlet 158.

[0038] The secondary condenser 160 comprises a double-effect heat exchange tube consisting of a conical inner ground glass tube 161 with a maximum inner diameter of 24 mm and a conical outer ground glass tube 162 with a maximum outer diameter of 34 mm. The double-effect heat exchange tube is a nested system of four layers of glass tubes, from the outside in: a first layer of glass tube 163 with an outer diameter of 50 mm, a second layer of glass tube 164 with an outer diameter of 35 mm, a third layer of glass tube 165 with an outer diameter of 20 mm, and a fourth layer of glass tube 166 with an outer diameter of 12 mm. In this system, a pagoda-shaped connecting pipe with an outer diameter of 12 mm is vertically fused to the lower end of the side wall of the first glass tube 163 and the upper end of the side wall of the second glass tube 164, serving as the coolant inlet 167 and the coolant outlet 168, respectively; the upper end of the side wall of the second glass tube 164 is connected to the top of the fourth glass tube 166 through a glass tube with an outer diameter of 10 mm; the bottom of the fourth glass tube 166 is open inside the bottom of the third glass tube 165; the bottom of the third glass tube 165 is closed, and the top passes vertically through the side wall of the second glass tube 164, connecting to the coolant outlet 168.

[0039] The diverter 170 includes collecting pipes 171 and 172 and drain pipe 173. The collecting pipes 171 and 172 are conical ground glass tubes with a maximum inner diameter of 34 mm extending laterally and upward, respectively, with an included angle of 70 degrees; the drain pipe 173 is a conical ground glass tube with a maximum outer diameter of 24 mm extending downward.

[0040] The collection bottle 180 is a 500 ml glass column bottle containing a receiving port 181 and a drain pipe 182. The receiving port 181 is a conical ground glass tube with a maximum inner diameter of 24 mm extending upwards; the drain pipe 182 is a polytetrafluoroethylene shut-off valve with an outer diameter of 12 mm fused to the bottom of the collection bottle 180.

[0041] The distillate storage bottle 190 is a 10-liter glass tank containing a distillate inlet 191; the distillate inlet 191 is a connection port with a pressure balancing function and an outer diameter of 50 mm.

[0042] The integrated control component 200 includes a hot bath 210, a cold bath 220, a coolant delivery pump 230, a circulating air pump 240, a pressure sensor 250, a raw material addition pump 260, a fraction delivery pump 270, a liquid level sensing component 280, and a comprehensive controller 290.

[0043] The hot bath 210 is a cylindrical magnetic stirrer that can hold 2 liters of deionized water. Its hot bath temperature can be adjusted from room temperature to 100 degrees Celsius, and its magnetic stirring speed can be adjusted from 0 to 1000 revolutions per minute.

[0044] The cold bath 220 is a low-temperature container that can hold 5 liters of coolant, including an outlet 221 with an outer diameter of 12 mm and an inlet 222. The coolant temperature can be adjusted within the range of -20 degrees Celsius to room temperature.

[0045] The coolant delivery pump 230 is a centrifugal pump with a liquid delivery rate of approximately 300 ml per minute.

[0046] The circulating air pump 240 is a diaphragm pump with a gas delivery rate of approximately 18 liters per minute.

[0047] The pressure sensor 250 is a resistive sensor with a pressure detection range of 0 to 0.1 MPa.

[0048] The stock solution addition pump 260 and the fraction transfer pump 270 are peristaltic pumps with a liquid transfer rate of approximately 300 ml per minute.

[0049] The liquid level sensing component 280 includes non-contact capacitive liquid level gauges 281, 282 and 283.

[0050] The integrated controller 290 is a programmable logic controller with display function.

[0051] The general method and working principle of the environmentally friendly continuous distillation apparatus are as follows: The first step is to clean and dry the relevant accessories of the rapid distillation component 100 of the environmentally friendly continuous distillation apparatus, and then proceed according to... Figures 1-3 The connection shown is assembled with the integrated control component 200; The second step involves using a cryogenic infusion hose to connect the inlet pipe and outlet 221 of the coolant delivery pump 230, the outlet pipe of the coolant delivery pump 230 and the coolant inlet 157, the coolant outlet 158 ​​and the coolant inlet 167, and the coolant outlet 168 and the return port 222. The third step is to connect the conical ground glass tube 161 and the air inlet of the circulating air pump 240, the air outlet of the circulating air pump 240 and the return air pipe 112 in sequence with the air guide hose, and connect the air pressure sensor 250 between the air outlet of the circulating air pump 240 and the return air pipe 112. The fourth step is to connect the discharge port 131 to the inlet pipe of the raw liquid addition pump 260, the outlet pipe of the raw liquid addition pump 260 to the feed port 123, the discharge pipe 182 to the inlet pipe of the distillation transfer pump 270, and the outlet pipe of the distillation transfer pump 270 to the distillate inlet 191 using corrosion-resistant organic solvent delivery pipes. Fifth step, place level gauges 281, 282 and 283 at the bottom of the original liquid storage bottle 110, the bottom of the collection bottle 180 and the top of the distillation storage bottle 190 respectively; Step 6: Add appropriate amounts of deionized water and coolant to the hot bath 210 and cold bath 220 respectively. At the same time, start the stock solution addition pump 260 to add an appropriate amount of liquid to be distilled into the distillation flask 120. Set the working temperature of the hot bath 210 and cold bath 220 through the integrated controller 290 and start the coolant delivery pump 230. Step 7: The circulating air pump 240 is started via the integrated controller 290, and solvent distillation is carried out in cooperation with the pressure sensor 250. When the trigger signal of the level gauge 281 disappears, the liquid to be distilled is added to the original liquid storage bottle 110 or the distillation is stopped. When the level gauge 282 sends a trigger signal, the fraction transfer pump 270 is started to transfer the distillate collected in the distillate storage bottle 180 to the distillate storage bottle 190, and at the same time, the original liquid addition pump 260 is started to add the liquid to be distilled from the original liquid storage bottle 110 to the distillation bottle 120. When the level gauge 283 sends a trigger signal, the distillate storage bottle 190 is replaced or the distillation is stopped. Step 8: When the experiment is over, shut down the relevant working units in sequence and recover the distillate; Step nine: Clean and recycle the relevant parts. Application Example 1

[0052] Using the environmentally friendly continuous distillation apparatus provided in Example 1 as the distillation device, a continuous distillation experiment was conducted on dichloromethane. The stock solution storage bottle 110 contained 4.0 liters of dichloromethane. The distillation flask 120 and the collection bottle 180 each had a volume of 500 ml. The temperature of the hot bath 110 was set to 50 degrees Celsius, and the temperature of the cold bath 210 was set to -20 degrees Celsius. When the temperatures of the hot bath 110 and the cold bath 210 reached the set values, the coolant delivery pump 230 and the circulating air pump 240 were turned on. With the assistance of the pressure sensor 250, continuous distillation of dichloromethane was performed, and the experiment was repeated three times. The average distillation rate of dichloromethane was approximately 850 ml per hour, the average distillation time was 4.7 hours, and the average recovery rate was approximately 98.2%. Application Example 2

[0053] Using the environmentally friendly continuous distillation apparatus provided in Example 1 as the distillation equipment, a continuous distillation experiment was conducted on ethyl acetate. The stock solution storage bottle 110 contained 4.0 liters of ethyl acetate. The distillation flask 120 and the collection bottle 180 each had a volume of 500 ml. The temperature of the hot bath 110 was set to 80 degrees Celsius, and the temperature of the cold bath 210 was set to -20 degrees Celsius. When the temperatures of the hot bath 110 and the cold bath 210 reached the set values, the coolant delivery pump 230 and the circulating air pump 240 were turned on. With the assistance of the pressure sensor 250, ethyl acetate was continuously distilled. The experiment was repeated three times. The average distillation rate of ethyl acetate was approximately 710 ml per hour, the average distillation time was 5.6 hours, and the average recovery rate was approximately 99.1%.

[0054] Finally, it should be noted that the description of the structure and application examples of the environmentally friendly continuous distillation apparatus provided by this invention has fully demonstrated that it can be widely used in continuous distillation experiments. Due to space limitations, the dimensions, models, connection methods, and applicable experimental processes of the rapid distillation components and integrated control components involved in this invention cannot be listed one by one. Therefore, the above embodiments and application examples are only used to illustrate the technical solutions of this invention, and not to limit it. Although this invention has been described in detail with reference to the foregoing embodiments and application examples, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or equivalent substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of protection of this invention.

Claims

1. An environmentally friendly continuous distillation apparatus, characterized in that, It includes interconnected rapid distillation components and integrated control components.

2. The environmentally friendly continuous distillation apparatus according to claim 1, characterized in that, The rapid distillation assembly includes a stock solution storage bottle, a distillation flask, a distillation head, a dustproof assembly, a primary condenser, a secondary condenser, a distributor, a collection bottle, and a fraction storage bottle.

3. The environmentally friendly continuous distillation apparatus according to claim 2, characterized in that: The stock solution storage bottle is a liquid storage tank or reaction vessel containing a stock solution inlet and a discharge outlet. Its material can be stainless steel, ceramic, glass, or polytetrafluoroethylene (PTFE), preferably glass or PTFE, more preferably glass, with a volume of not less than 1 liter, preferably 1–50 liters, more preferably 10 liters. The stock solution inlet is a connection port with pressure balancing function, with an outer diameter of 6–200 mm, preferably 8–100 mm, more preferably 50 mm. The discharge outlet is a two-way corrosion-resistant shut-off valve, a straight connecting pipe, or a pagoda-shaped connecting pipe, preferably a two-way corrosion-resistant shut-off valve, with an outer diameter of 6–50 mm, preferably 8–30 mm, more preferably 12 mm. The distillation flask is a multi-necked glass bottle or reaction vessel containing a distillation port, a return gas pipe, and a raw material addition port, preferably a multi-necked glass bottle with a volume of not less than 200 ml, preferably 200-1000 ml, and more preferably 500 ml; the distillation port is a flange-type glass connection port with an outer diameter of 30-150 mm, preferably 40-100 mm, and more preferably 50 mm; the return gas pipe and the raw material addition port are straight connecting pipes, pagoda-type connecting pipes, or polytetrafluoroethylene shut-off valves, preferably pagoda-type connecting pipes with an outer diameter of 6-30 mm, preferably 8-20 mm, and more preferably 12 mm; The distillation head includes a steam inlet and a steam outlet; the included angle between the steam inlet and the steam outlet is 20–85 degrees, preferably 30–80 degrees, and more preferably 70 degrees; the steam inlet is a flange-type glass connection with an outer diameter of 30–150 mm, preferably 40–100 mm, and more preferably 50 mm; the steam outlet is a conical ground glass tube with a maximum outer diameter of 12–60 mm, preferably 16–40 mm, and more preferably 24 mm. The dustproof assembly includes a dustproof plate and a flange clamp; the dustproof plate is a glass frosted plate, filter paper, PTFE-coated metal filter screen, polymer filter screen, PTFE-coated porous plate, or a combination thereof, preferably a combination of filter paper and PTFE-coated metal filter screen, with an outer diameter of 30-150 mm, preferably 40-100 mm, and more preferably 50 mm; the flange clamp can be a plate flange clamp, a split flange clamp, or a three-piece interlocking flange clamp, preferably a three-piece interlocking flange clamp; The primary and secondary condensers are double-effect heat exchange tubes with tapered ground glass tubes fused at both ends. They are mainly used for heat exchange between solvent vapor and coolant, increasing the liquefaction efficiency of solvent vapor. The double-effect heat exchange tube consists of four layers of glass tubing, from the outside in: a first layer, a second layer, a third layer, and a fourth layer. A pagoda-shaped connecting tube is vertically fused to the lower end of the sidewall of the first layer glass tube and the upper end of the sidewall of the second layer glass tube, serving as the coolant inlet and outlet. The upper end of the sidewall of the second layer glass tube is connected to the top of the fourth layer glass tube via a thin glass tube. The bottom of the fourth layer glass tube opens inside the bottom of the third layer glass tube, and the bottom of the third layer glass tube is closed, with its top vertically passing through the sidewall of the second layer glass tube. The first glass tube has an outer diameter of 20–180 mm, preferably 20–100 mm, more preferably 50 mm; the second glass tube has an outer diameter of 16–170 mm, preferably 16–90 mm, more preferably 35 mm; the third glass tube has an outer diameter of 12–160 mm, preferably 12–80 mm, more preferably 20 mm; the fourth glass tube has an outer diameter of 8–140 mm, preferably 8–70 mm, more preferably 12 mm; the pagoda-shaped connecting pipe has an outer diameter of 6–30 mm, preferably 8–20 mm, more preferably 12 mm; the conical ground glass tube has a maximum ground joint diameter of 12–60 mm, preferably 16–40 mm. The diverter comprises two collecting pipes and one drain pipe; the collecting pipes are tapered ground glass tubes with a maximum inner diameter of 12–60 mm, preferably 16–40 mm, and more preferably 34 mm; the included angle between the two collecting pipes is in the range of 0°–90°, preferably in the range of 0°–30°, and more preferably 0°; the drain pipe is a downward-extending tapered ground glass tube or a glass ball ground joint, preferably a tapered ground glass tube with a maximum outer diameter of 12–60 mm, preferably 16–40 mm, and more preferably 24 mm; the maximum outer diameter of the glass ball ground joint is 20–60 mm, preferably 24–40 mm, and more preferably 28 mm; The collection bottle is a glass bottle comprising a receiving tube and a draining tube, with a volume of not less than 200 ml, preferably 100-1000 ml, and more preferably 500 ml; the receiving tube is a conical ground glass tube or a glass ball grinding bowl, preferably a conical ground glass tube, with a maximum inner diameter of 12-60 mm, preferably 16-40 mm, and more preferably 24 mm; the glass ball grinding bowl has a maximum inner diameter of 20-60 mm, preferably 24-40 mm, and more preferably 28 mm; the draining tube is a polytetrafluoroethylene shut-off valve or a pagoda-shaped connecting tube fused to the bottom of the collection bottle, preferably a polytetrafluoroethylene shut-off valve, with an outer diameter of 6-30 mm, preferably 8-20 mm, and more preferably 12 mm. The distillate storage bottle is a liquid storage tank with a distillate inlet. Its material can be stainless steel, ceramic, glass, or polytetrafluoroethylene, preferably glass or polytetrafluoroethylene, more preferably glass, with a volume of not less than 1 liter, preferably 1 to 50 liters, more preferably 10 liters; the distillate inlet is a connection port with pressure balancing function, with an outer diameter of 6 to 200 mm, preferably 8 to 100 mm, more preferably 50 mm.

4. The environmentally friendly continuous distillation apparatus according to claim 1, characterized in that, The integrated control component includes a hot bath, a cold bath, a coolant delivery pump, a circulating air pump, a pressure sensor, a raw material addition pump, a fraction delivery pump, a liquid level sensing component, and a comprehensive controller.

5. The environmentally friendly continuous distillation apparatus according to claim 4, characterized in that: The hot bath is a barrel-shaped container with magnetic stirring function for holding the hot bath medium, with a volume of not less than 1 liter, preferably 2 to 10 liters, and more preferably 2 liters; the temperature adjustment range of the hot bath medium is room temperature to 200 degrees Celsius, preferably room temperature to 150 degrees Celsius, and more preferably room temperature to 100 degrees Celsius; the magnetic stirring speed adjustment range is 0 to 3000 revolutions per minute, preferably 0 to 1800 revolutions per minute, and more preferably 0 to 1000 revolutions per minute; The cold bath is a low-temperature container with an outlet and an inlet for holding coolant, and its volume is not less than 1 liter, preferably 2 to 50 liters, and more preferably 5 liters; the temperature adjustment range of the coolant is -25 degrees Celsius to room temperature, preferably -20 to 10 degrees Celsius, and more preferably -10 to 0 degrees Celsius. The coolant delivery pump can be a centrifugal pump, a plunger pump, or a peristaltic pump, preferably a centrifugal pump; its liquid delivery rate is 0 to 8000 ml per minute, preferably 0 to 6000 ml per minute, and more preferably 1000 ml per minute; The circulating air pump can be a centrifugal pump, a reciprocating pump, or a diaphragm pump, preferably a diaphragm pump; its gas delivery rate is 0 to 120 liters per minute, preferably 0 to 60 liters per minute, and more preferably 18 liters per minute; The pressure sensor is a resistive sensor or a non-resistive sensor, preferably a resistive sensor, and its pressure detection range is -0.1 to 1.0 MPa, preferably 0 to 0.1 MPa; The original liquid addition pump and the fraction transfer pump can be centrifugal pumps, plunger pumps or peristaltic pumps, preferably peristaltic pumps, with a liquid delivery rate of 0 to 1500 ml per minute, preferably 0 to 1000 ml per minute, and more preferably 300 ml per minute. The liquid level sensing component includes three liquid level gauges; the liquid level gauges can be capacitive liquid level gauges, resistive liquid level gauges or photosensitive liquid level gauges, preferably capacitive liquid level gauges and photosensitive liquid level gauges, more preferably capacitive liquid level gauges, and their sensing method is contact sensing or non-contact sensing, preferably non-contact sensing. The integrated controller can be an integrated circuit board with display function or a programmable logic controller, preferably a programmable logic controller with display function, used to control the switching and working status of all working modules.

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