CN111603795A - Efficient rotary evaporation device and working method thereof - Google Patents
Efficient rotary evaporation device and working method thereof Download PDFInfo
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- CN111603795A CN111603795A CN202010654541.1A CN202010654541A CN111603795A CN 111603795 A CN111603795 A CN 111603795A CN 202010654541 A CN202010654541 A CN 202010654541A CN 111603795 A CN111603795 A CN 111603795A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/08—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs
- B01D3/085—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs using a rotary evaporator
Abstract
The utility model provides an efficient rotary evaporation device, includes support, first condensing equipment, second condensing equipment, four-way pipe, evaporimeter, control by temperature change water bath, rotating device, pipeline, functional device, the first condensing equipment of support fixed connection and second condensing equipment, the four-way pipe left end is equipped with feed inlet and evacuation mouth, and the right-hand member passes rotating device and is connected with the evaporimeter, the four-way pipe middle part is equipped with first mouth of pipe and second mouth of pipe, first mouth of pipe passes through the pipeline and is connected with first condensing equipment, the second mouth of pipe passes through functional device and is connected with second condensing equipment, the evaporimeter is established in control by temperature change water bath top, control by temperature change water bath lower extreme is equipped with the regulation pole. Different functions of the device are realized through the design of the four-way pipe, different functions of rectification, distillation, extraction and the like can be realized through the use of different instruments of the functional device, and efficient and safe rotary evaporation operation is realized through the pressure in the control and regulation device of the control valve of the vacuumizing port.
Description
Technical Field
The invention relates to the technical field of chemical or medical rotary evaporation, in particular to a high-efficiency rotary evaporation device and a working method thereof.
Background
The rotary evaporator is an indispensable conventional device in chemical, pharmaceutical laboratories and factories, and is widely used in the concentration of liquid medicines and chemical synthesis. The rotary evaporator is mainly used for continuously distilling a large amount of volatile solvents under the reduced pressure condition, and mainly drives the distillation flask to continuously rotate through the rotator to form a rotary film to increase the evaporation area and accelerate the evaporation speed. Meanwhile, the vacuum pumping pump device can provide negative pressure, the boiling point of the solvent is reduced by the negative pressure, the heating temperature is reduced, and the heat-sensitive components of the concentrated solution are well protected.
At present, the rotary evaporator has a single function, only distillation concentration can be used, the operation of integration of rectification, Soxhlet extraction distillation and reflux cannot be realized, in the test, the rectification, the extraction and the separation are coherent actions, and if the operation is separated, the operation is complex, the efficiency is low, the test is not thorough, the cost is higher, and the traditional vacuum rotary evaporator is easy to explode in the negative pressure distillation process, so that materials are easily flushed out of the evaporator, the material loss is caused, and the rotary evaporation cannot be completed timely and efficiently.
Disclosure of Invention
The purpose of the invention is as follows: the invention discloses an efficient rotary evaporation device, which can realize multifunctional use and realize efficient and safe multifunctional rotary evaporation by controlling the pressure in the device.
The technical scheme is as follows: in order to achieve the purpose, the invention discloses an efficient rotary evaporation device which comprises a support, a first condensation device, a second condensation device, a four-way pipe, an evaporator, a temperature control water bath kettle, a rotating device, a pipeline and a function device, wherein the support is fixedly connected with the first condensation device and the second condensation device, the left end of the four-way pipe is provided with a feed inlet and a vacuum pumping port, the right end of the four-way pipe penetrates through the rotating device to be connected with the evaporator, the middle part of the four-way pipe is provided with a first pipe orifice and a second pipe orifice, the first pipe orifice is connected with the first condensation device through the pipeline, the second pipe orifice is connected with the second condensation device through the function device, the evaporator is connected with the rotating device, the evaporator is arranged above the temperature control water bath kettle, the lower end of the temperature control water bath kettle is provided with an adjusting rod, and. The efficient rotary evaporation device can be connected with instruments matched with the radial ports through the design of a four-way pipe to realize different functions of the device, can realize different functions of rectification, distillation, extraction and the like through the use of different instruments as the functional device, can realize efficient and safe rotary evaporation operation through controlling and adjusting the pressure in the device through a control valve of the vacuumizing port, realizes rotary evaporation of different liquids, and avoids safety accidents caused by evaporation of water in a constant-temperature water bath through the design of a water depth measuring probe.
Furthermore, foretell rotatory evaporation plant of efficient is equipped with first control valve and second control valve on first mouth of pipe and the second mouth of pipe, first mouth of pipe and second mouth of pipe port are the mill mouth, the evacuation mouth is equipped with control valve.
Further, foretell rotatory evaporation plant of efficient, first mouth of pipe is the T style of calligraphy, including violently managing and standpipe, the standpipe communicates with each other from top to bottom, the evacuation mouth is equipped with control valve.
Further, in the above efficient rotary evaporation apparatus, the functional apparatus is a rectification apparatus or an extraction apparatus.
Furthermore, in the efficient rotary evaporation device, the temperature control water bath is internally provided with the water depth measuring probe, and the height of the water depth measuring probe can be adjusted.
Further, the rotating device comprises a fixing clamp, a shaft sleeve and a rotating shaft, wherein the fixing clamp fixes the shaft sleeve, and the rotating shaft is arranged in the shaft sleeve.
Furthermore, in the above efficient rotary evaporation apparatus, the first condensing unit and the second condensing unit are provided with a first exhaust port and a second exhaust port.
Further, the working method of the high-efficiency rotary evaporation device comprises the following steps:
a1, firstly, mounting the whole device on a bracket, adding a reaction solution into the device, and mounting an evaporator on a rotating device;
a2, adjusting the adjusting rod to lift the temperature control water bath kettle, and placing the evaporator in the temperature control water bath kettle;
a3, closing the first control valve, and pumping the device into negative pressure through the vacuum pumping port;
a4, opening a temperature control water bath kettle for heating, wherein the reaction in the device can be rectified or extracted;
and A5, feeding the rectified and extracted gas into a collecting bottle through a condensing device to finish the functional operations of rectification, extraction and the like.
Further, in the above operating method of the high efficiency rotary evaporation apparatus, the rectification includes the following steps:
s1, firstly, mounting the whole device on a bracket, adding reaction liquid into an evaporator, and mounting the evaporator on a rotating device;
s2, adjusting the adjusting rod to lift the temperature control water bath kettle and place the evaporator in the temperature control water bath kettle;
s3, closing the first control valve, pumping the device into negative pressure through the vacuumizing port, and introducing condensed water into the first condensing device;
s4, opening the temperature control water bath kettle for heating, and separating different components of the reaction liquid through the functional device;
s5, the first exhaust port and the second exhaust port are connected through a hose, different components of the reaction liquid enter the first condensing device through the second condensing device and the hose to be condensed into liquid, and then enter a collecting bottle below the pipeline to finish separation.
Further, the working method of the efficient rotary evaporation device comprises the following steps:
b1, firstly, mounting the whole device on a bracket, and mounting the evaporator on a rotating device;
b2, adjusting the adjusting rod to lift the temperature control water bath kettle, and placing the evaporator in the temperature control water bath kettle;
b3, closing the first control valve, adding the reaction liquid into the functional device, and connecting and installing a second condensing device on the functional device;
b4, pumping the device into negative pressure through a vacuum pumping port, and introducing condensed water into the second condensing device;
b5, opening a temperature control water bath pot for heating, heating the reaction liquid in the functional device, and feeding the reaction liquid into a four-way pipe so as to enter an evaporator;
b6, opening a temperature control water bath pot for heating, heating the reaction liquid in the functional device, and feeding the reaction liquid into a four-way pipe so as to enter an evaporator;
b7, closing the second control valve, opening the temperature control water bath to heat, condensing the reaction liquid through the pipeline, and then feeding the solution into a collecting bottle below the pipeline to finish the separation.
The technical scheme shows that the invention has the following beneficial effects:
according to the efficient rotary evaporation device, through the design of the four-way pipe, the four-way pipe can play a role of a buffer bottle in the device, meanwhile, the pipe orifice can be connected with instruments matched with the various calibers, flexible assembly and disassembly of the instruments are facilitated, different functions of the device are achieved, meanwhile, different instruments can be used through the functional device, different functions such as rectification, distillation and extraction can be achieved, the pressure in the device can be controlled and adjusted through the control valve of the vacuumizing port, liquid in the evaporator is prevented from being exploded and boiled due to overlarge pressure, the working efficiency of the rotary evaporation device is improved, the design of the feeding port can enable the amount of solution to be large, continuous material continuation can be achieved, the evaporator does not need to be detached, high-efficiency work is achieved, and meanwhile, safety accidents caused by evaporation of water in a constant temperature water bath are avoided through the design of the water depth measuring probe.
Drawings
FIG. 1 is a schematic view of the overall structure of a high-efficiency rotary evaporation apparatus according to embodiment 1 of the present invention;
FIG. 2 is a schematic view of the overall structure of a high-efficiency rotary evaporation apparatus according to embodiment 2 of the present invention;
FIG. 3 is a schematic view of the overall structure of a high-efficiency rotary evaporation apparatus according to embodiment 3 of the present invention;
FIG. 4 is a schematic structural view of the four-way pipe according to the present invention;
FIG. 5 is a top view of the cross-piece of the present invention;
in the figure: 1 support, 2 first condensing equipment, 3 second condensing equipment, 4 four-way pipes, 5 functional devices of 6 evaporators, 7 temperature control water baths, 8 rotating devices, 9 pipelines, 41 feed inlets, 42 vacuumizing ports, 43 first pipe orifices, 44 second pipe orifices, 71 adjusting rods, 72 adjusting handles, 45 first control valves, 46 second control valves, 47 transverse pipes, 48 vertical pipes, 11 rectifying devices, 10 extracting devices, 72 water depth measuring probes, 81 fixing clamps, 82 shaft sleeves, 83 rotating shafts, 49 control valves, 21 first exhaust ports and 31 second exhaust ports.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Example 1
The invention discloses a high-efficiency rotary evaporation device, which comprises a bracket 1, a first condensing device 2, a second condensing device 3, a four-way pipe 4, an evaporator 5, a temperature control water bath 7, a rotating device 8, a pipeline 9 and a rectifying device 11 as shown in figure 1, the bracket 1 is fixedly connected with the first condensing device 2 and the second condensing device 3, the left end of the four-way pipe 4 is provided with a feeding hole 41 and a vacuum pumping hole 42, wherein, the vacuum-pumping port 42 is provided with a control valve 49, the right end passes through the rotating device 8 to be connected with the evaporator 5, a first pipe orifice 43 and a second pipe orifice 44 are arranged in the middle of the four-way pipe 4, the first pipe orifice 43 is connected with the first condensing device 2 through a pipeline 9, the second pipe orifice 44 is connected with the second condensing device 3 through a rectifying device 11, the first condensing device 2 and the second condensing device 3 are provided with a first exhaust port 21 and a second exhaust port 31; the evaporator 5 is connected with the rotating device 8, the evaporator 5 is arranged above the temperature control water bath pot 7, the lower end of the temperature control water bath pot 7 is provided with an adjusting rod 71, and the adjusting rod is provided with an adjusting handle 72.
In addition, a first control valve 45 and a second control valve 46 are arranged on the first pipe orifice 43 and the second pipe orifice 44, and the ports of the first pipe orifice 43 and the second pipe orifice 44 are grinding ports. The first pipe opening 43 is T-shaped, and includes a horizontal pipe 47 and a vertical pipe 48, and the vertical pipe 48 is communicated with each other up and down, as shown in fig. 4 and 5.
Further, the rectifying device 11 includes a distillation head 111 and a rectifying column 112.
A water depth measuring probe 72 is arranged in the temperature control water bath 7, and the height of the water depth measuring probe 72 is adjustable.
In addition, the rotating device 8 comprises a fixing clamp 81, a shaft sleeve 82 and a rotating shaft 83, wherein the fixing clamp 81 is used for fixing the shaft sleeve 82, and the rotating shaft 83 is arranged in the shaft sleeve 82.
During the use, at first install whole device on support 1, evaporimeter 5 adds the reaction liquid, install on rotating device 8, adjust regulation pole 71 and make control by temperature change water bath 7 rise, make evaporimeter 5 put in control by temperature change water bath 7, close first control valve 45, draw into the negative pressure through evacuation mouth 42 with the device, first condensing equipment 2 lets in the comdenstion water, open control by temperature change water bath 7 and heat, the reaction liquid passes through rectifier unit 11 and accomplishes the separation of the different components of reaction liquid, first gas vent 21 and second gas vent 31 pass through the hose connection, the different components of reaction liquid pass through second condensing equipment 3 and hose and enter into first condensing equipment 2 and condense into liquid, get into the collection bottle below pipeline 9 again, accomplish the separation.
Example 2
The invention discloses a high-efficiency rotary evaporation device, which comprises a bracket 1, a first condensing device 2, a second condensing device 3, a four-way pipe 4, an evaporator 5, a temperature control water bath 7, a rotating device 8, a pipeline 9 and an extraction device 10 as shown in figure 2, the bracket 1 is fixedly connected with the first condensing device 2 and the second condensing device 3, the left end of the four-way pipe 4 is provided with a feeding hole 41 and a vacuum pumping hole 42, wherein, the vacuum-pumping port 42 is provided with a control valve 49, the right end passes through the rotating device 8 to be connected with the evaporator 5, a first pipe orifice 43 and a second pipe orifice 44 are arranged in the middle of the four-way pipe 4, the first pipe orifice 43 is connected with the first condensing device 2 through a pipeline 9, the second pipe orifice 44 is connected with the second condensing device 3 through an extraction device 10, the first condensing device 2 and the second condensing device 3 are provided with a first exhaust port 21 and a second exhaust port 31; the evaporator 5 is connected with the rotating device 8, the evaporator 5 is arranged above the temperature control water bath pot 7, the lower end of the temperature control water bath pot 7 is provided with an adjusting rod 71, and the adjusting rod is provided with an adjusting handle 72.
In addition, a first control valve 45 and a second control valve 46 are arranged on the first pipe orifice 43 and the second pipe orifice 44, and the ports of the first pipe orifice 43 and the second pipe orifice 44 are grinding ports. The first pipe opening 43 is T-shaped, and includes a horizontal pipe 47 and a vertical pipe 48, and the vertical pipe 48 is communicated with each other up and down, as shown in fig. 4 and 5.
Further, the extraction device 10 is a siphon 121.
A water depth measuring probe 72 is arranged in the temperature control water bath 7, and the height of the water depth measuring probe 72 is adjustable.
In addition, the rotating device 8 comprises a fixing clamp 81, a shaft sleeve 82 and a rotating shaft 83, wherein the fixing clamp 81 is used for fixing the shaft sleeve 82, and the rotating shaft 83 is arranged in the shaft sleeve 82.
When in use, firstly, the whole device is arranged on a bracket 1, an evaporator 5 is arranged on a rotating device 8, a regulating rod 71 is regulated to enable a temperature control water bath pot 7 to rise, the evaporator 5 is placed in the temperature control water bath pot 7, a first control valve 45 is closed, reaction liquid is added into a siphon 121 of an extraction device 10, a second condensing device 3 is connected and arranged on the upper surface of the temperature control water bath pot, the device is pumped into negative pressure through a vacuumizing port 42, condensed water is introduced into the second condensing device 3, the temperature control water bath pot 7 is opened for heating, the reaction liquid in a functional device 6 enters a four-way pipe 4 through heating, then enters the evaporator 5, the temperature control water bath pot 7 is opened for heating, the reaction liquid enters a four-way pipe 4 through heating, then enters the evaporator 5, the second control valve 46 is closed, the temperature control water bath pot 7 is opened for heating, the reaction liquid is condensed through a pipeline 9, and then enters a collecting bottle below a pipeline 9, the separation is completed.
Example 3
The invention discloses a high-efficiency rotary evaporation device, which comprises a bracket 1, a first condensing device 2, a second condensing device 3, a four-way pipe 4, an evaporator 5, a temperature control water bath 7, a rotating device 8, a pipeline 9 and a rectifying device 11 as shown in figure 3, the bracket 1 is fixedly connected with the first condensing device 2 and the second condensing device 3, the left end of the four-way pipe 4 is provided with a feeding hole 41 and a vacuum pumping hole 42, wherein, the vacuum-pumping port 42 is provided with a control valve 49, the right end passes through the rotating device 8 to be connected with the evaporator 5, a first pipe orifice 43 and a second pipe orifice 44 are arranged in the middle of the four-way pipe 4, the first pipe orifice 43 is connected with the first condensing device 2 through a pipeline 9, the second pipe orifice 44 is connected with the second condensing device 3 through a rectifying device 11, the first condensing device 2 and the second condensing device 3 are provided with a first exhaust port 21 and a second exhaust port 31; the evaporator 5 is connected with the rotating device 8, the evaporator 5 is arranged above the temperature control water bath pot 7, the lower end of the temperature control water bath pot 7 is provided with an adjusting rod 71, and the adjusting rod is provided with an adjusting handle 72.
In addition, as shown in fig. 4 and 5, a first control valve 45 and a second control valve 46 are arranged on the first nozzle 43 and the second nozzle 44, and the ports of the first nozzle 43 and the second nozzle 44 are grinding ports. The first pipe opening 43 is T-shaped and comprises a horizontal pipe 47 and a vertical pipe 48, the vertical pipe 48 is vertically communicated, and the lower end of the vertical pipe 48 is provided with the receiving bottle 12.
Further, the rectifying device 11 includes a distillation head 111 and a rectifying column 112.
A water depth measuring probe 72 is arranged in the temperature control water bath 7, and the height of the water depth measuring probe 72 is adjustable.
In addition, the rotating device 8 comprises a fixing clamp 81, a shaft sleeve 82 and a rotating shaft 83, wherein the fixing clamp 81 is used for fixing the shaft sleeve 82, and the rotating shaft 83 is arranged in the shaft sleeve 82.
When the device is used, firstly, the whole device is installed on the support 1, the evaporator 5 is added with reaction liquid and installed on the rotating device 8, the temperature control water bath pot 7 is lifted by adjusting the adjusting rod 71, the evaporator 5 is placed in the temperature control water bath pot 7, the second control valve 46 is closed, the device is pumped into negative pressure through the vacuumizing port 42, condensed water is introduced into the first condensing device 2, the temperature control water bath pot 7 is opened for heating, a solvent in the reaction liquid is rotationally evaporated and falls into the receiving bottle 12 through the pipeline 9, when the reaction liquid in the evaporator 5 is concentrated to a certain volume, the reaction liquid is supplemented with materials into the evaporator 5 through the feeding port 41 until the concentration of the reaction liquid is completed.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. An efficient rotary evaporation device, characterized in that: comprises a bracket (1), a first condensing device (2), a second condensing device (3), a four-way pipe (4), an evaporator (5), a temperature control water bath (7), a rotating device (8), a pipeline (9) and a functional device (6), wherein the bracket (1) is fixedly connected with the first condensing device (2) and the second condensing device (3), the left end of the four-way pipe (4) is provided with a feed inlet (41) and a vacuum pumping port (42), the right end of the four-way pipe (4) passes through the rotating device (8) to be connected with the evaporator (5), the middle part of the four-way pipe (4) is provided with a first pipe orifice (43) and a second pipe orifice (44), the first pipe orifice (43) is connected with the first condensing device (2) through the pipeline (9), the second pipe orifice (44) is connected with the second condensing device (3) through the functional device (6), the evaporator (5) is arranged above the temperature control water bath (7), the lower end of the temperature control water bath kettle (7) is provided with an adjusting rod (71), and the adjusting rod is provided with an adjusting handle (72).
2. A high efficiency rotary evaporator apparatus as set forth in claim 1 wherein: the vacuum pump is characterized in that a first control valve (45) and a second control valve (46) are arranged on the first pipe orifice (43) and the second pipe orifice (44), the ports of the first pipe orifice (43) and the second pipe orifice (44) are grinding ports, and a control valve (49) is arranged on the vacuumizing port (42).
3. A high efficiency rotary evaporator apparatus as set forth in claim 2 wherein: the first pipe orifice (43) is T-shaped and comprises a transverse pipe (47) and a vertical pipe (48), and the vertical pipe (48) is communicated up and down.
4. A high efficiency rotary evaporator apparatus as set forth in claim 3 wherein: the functional device (6) is a rectifying device (11) or an extracting device (10).
5. A high efficiency rotary evaporator apparatus as set forth in claim 4 wherein: a water depth measuring probe (72) is arranged in the temperature control water bath pot (7), and the height of the water depth measuring probe (72) can be adjusted.
6. A high efficiency rotary evaporator apparatus as set forth in claim 5 wherein: the rotating device (8) comprises a fixing clamp (81), a shaft sleeve (82) and a rotating shaft (83), the shaft sleeve (82) is fixed by the fixing clamp (81), and the rotating shaft (83) is arranged in the shaft sleeve (82).
7. A high efficiency rotary evaporator apparatus as set forth in claim 4 wherein: and a first exhaust port (21) and a second exhaust port (31) are arranged on the first condensing device (2) and the second condensing device (3).
8. A method of operating a high efficiency rotary evaporator apparatus as set forth in any one of claims 1-9 wherein: the method comprises the following steps:
a1, firstly, mounting the whole device on a bracket (1), adding a reaction solution into the device, and mounting an evaporator (5) on a rotating device (8);
a2, adjusting the adjusting rod (71) to lift the temperature control water bath (7) and place the evaporator (5) in the temperature control water bath (7);
a3, closing the first control valve (45), and pumping the device to negative pressure through the vacuum pumping port (42);
a4, opening a temperature control water bath (7) for heating, wherein the reaction in the device can be rectified or extracted;
a5, the gas after rectification and extraction enters a collecting bottle (12) through a condensing device to finish the functional operations of rectification, extraction and the like.
9. A method of operating a high efficiency rotary evaporator apparatus as set forth in claim 8 wherein: the rectification comprises the following steps:
s1, firstly, mounting the whole device on a bracket (1), adding reaction liquid into an evaporator (5), and mounting the evaporator on a rotating device (8);
s2, adjusting the adjusting rod (71) to lift the temperature control water bath (7) and place the evaporator (5) in the temperature control water bath (7);
s3, closing the first control valve (45), pumping the device to negative pressure through the vacuumizing port (42), and introducing condensed water into the first condensing device (2);
s4, opening the temperature control water bath (7) for heating, and separating different components of the reaction liquid through the functional device (6);
s5, the first exhaust port (21) and the second exhaust port (31) are connected through a hose, different components of the reaction liquid enter the first condensing device (2) through the second condensing device (3) and the hose to be condensed into liquid, and then enter a collecting bottle below the pipeline (9) to finish separation.
10. A method of operating a high efficiency rotary evaporator apparatus as set forth in claim 8 wherein: the extraction comprises the following steps:
b1, firstly, mounting the whole device on a bracket (1), and mounting an evaporator (5) on a rotating device (8);
b2, adjusting the adjusting rod (71) to lift the temperature control water bath (7) and place the evaporator (5) in the temperature control water bath (7);
b3, closing the first control valve (45), adding the reaction liquid into the functional device (6), and connecting and installing the second condensing device (3) on the functional device;
b4, pumping the device to negative pressure through a vacuumizing port (42), and introducing condensed water into the second condensing device (3);
b5, opening the temperature control water bath (7) for heating, and heating the reaction liquid in the functional device (6) to enter the four-way pipe (4) and then enter the evaporator (5);
b6, opening the temperature control water bath (7) for heating, and heating the reaction liquid in the functional device (6) to enter the four-way pipe (4) and then enter the evaporator (5);
b7, closing the second control valve (46), opening the temperature control water bath (7) for heating, condensing the reaction liquid through the pipeline (9), and then feeding the solution into a collecting bottle below the pipeline (9) to finish separation.
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