CN111603794A - Rotary evaporator - Google Patents

Rotary evaporator Download PDF

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Publication number
CN111603794A
CN111603794A CN201910334135.4A CN201910334135A CN111603794A CN 111603794 A CN111603794 A CN 111603794A CN 201910334135 A CN201910334135 A CN 201910334135A CN 111603794 A CN111603794 A CN 111603794A
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CN
China
Prior art keywords
container
sample
vapor
rotary evaporator
tube
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CN201910334135.4A
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Chinese (zh)
Inventor
高野诚
林伸明
木原胜彦
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Yamato Scientific Co Ltd
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Yamato Scientific Co Ltd
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Publication of CN111603794A publication Critical patent/CN111603794A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/08Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/10Vacuum distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42Regulation; Control

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The rotary evaporator of the present invention suppresses inflow (reverse flow) of condensate into a sample container. The sample bottle (15) is connected to one end (13a) of a communication tube (13), and the other end (13b) of the communication tube opens into the container unit (45). A sample introduction tube (47) is inserted from the opposite side of the container unit from the communication tube. A protection pipe (59) is provided So as to cover the upper side of the sample introduction pipe and the vapor vent (So) of the communication pipe. An opening (59a) is formed at the lower part of the protective tube. The vapor of the sample (17) in the sample bottle (15) flows out from the opening into the container portion through a slit (50) between the communication tube and the sample introduction tube. The vapor flowing out into the container part reaches the condenser (35) at the upper part and is condensed. When the condensate drops from the condenser toward the receiving bottle (27), the condensate is protected by the protection pipe and prevented from flowing back into the communication pipe.

Description

Rotary evaporator
Technical Field
The present invention relates to a rotary evaporator for evaporating a sample to perform separation and concentration.
Background
The rotary evaporator ejects vapor generated by evaporating a sample from the tip of a communication pipe connected to a sample container while rotating the sample container in which the sample is stored, and the ejected vapor is condensed by a condenser to generate a condensate. The condensate accumulates in a receiver bottle located below the condenser.
Documents of the prior art
Patent document 1: japanese patent laid-open No. 2007-98246
The vapor outlet at the front end of the communicating pipe for ejecting vapor is positioned below the condenser. Therefore, in the rotary evaporator described in patent document 1, in order to suppress inflow of condensate dripping from the condenser to the vapor discharge port, the condensate dripping port is positioned outside the axial region of the communication pipe. This suppresses the inflow (reverse flow) of the condensate into the sample container.
Disclosure of Invention
The present invention has been made in view of the above circumstances, and an object thereof is to suppress inflow (reverse flow) of condensate into a sample container.
The rotary evaporator according to claim 1 is characterized by comprising: a sample container for storing a sample; a communicating pipe having one end connected to the sample container and the other end provided with a vapor outlet for discharging vapor evaporated from the sample; a driving unit that drives the communicating tube to rotate together with the sample container; a container portion having a space in which the vapor vent is open; a condenser provided above the space of the container portion and condensing the vapor discharged from the vapor discharge port; a condensate container provided below the space of the container portion and receiving condensate condensed by the condenser through the space; and a covering portion provided in the space of the container portion and covering an upper side of the vapor vent. The covering portion has one end connected to a side of the container portion on which the vapor spouting port opens and the other end connected to a side of the container portion opposite to the side of the container portion on which the vapor spouting port opens, and an opening portion formed in a lower portion thereof for allowing vapor spouted from the vapor spouting port to flow out into the space.
In the rotary evaporator according to claim 1, the vapor evaporated in the sample container flows into the space inside the container unit through the communication pipe, reaches the condenser from the container unit, and is condensed, and the condensed condensate is accumulated in the condensate container through the container unit. At this time, the covering portion can suppress inflow of the condensate dripping from the condensate into the vapor ejection port, thereby suppressing inflow (backflow) of the condensate into the sample container.
The rotary evaporator according to claim 2 is characterized in that a sample supply tube for supplying the sample to the sample container from the outside of the container portion on the other end side of the covering portion passes through the lower side of the covering portion and is inserted into the communication tube.
In the rotary evaporator described in claim 2, the covering portion prevents the condensate dripping from the condensate from adhering to the sample supply tube, and thus the condensate can be prevented from flowing along the sample supply tube and flowing into the sample container (flowing back).
The rotary evaporator according to claim 3, wherein the one end and the other end of the covering portion are connected to the container portion in a sealed state.
In the rotary evaporator according to claim 3, the condensate flowing along the inner surface of the container portion can be prevented from entering the inside of the covering portion.
The rotary evaporator according to claim 4 is characterized in that the container portion and the cover portion are made of glass, and the container portion and the one end and the other end of the cover portion are connected by glass welding.
In the rotary evaporator according to claim 4, the container portion and the cover portion can be connected in a sealed state by a simple operation of glass welding.
The rotary evaporator according to claim 5 is characterized in that the covering portion is bent inward of the covering portion so that both side edge portions of a portion corresponding to the opening in the direction in which the communication pipe extends are close to each other.
In the rotary evaporator according to claim 5, the condensate dripping from the condenser onto the cover portion can be prevented from flowing along the outer surface of the cover portion and flowing into the inside of the cover portion.
The rotary evaporator according to claim 6 is characterized in that a cross-sectional shape of the covering portion in a direction orthogonal to a direction connecting the one end and the other end is an arc shape.
In the rotary evaporator according to claim 6, the condensate dripping from the condenser onto the cover portion flows downward rapidly along the outer surface of the circular arc-shaped cover portion.
The rotary evaporator according to claim 7, wherein the covering portion has a gap formed between both side portions between the one end and the other end and an inner surface of the container portion.
In the rotary evaporator according to claim 7, the vapor flowing out of the opening of the cover portion passes through the gaps on both sides of the cover portion and then moves upward, so that the vapor flows into the condenser more uniformly.
The rotary evaporator according to claim 8, wherein the driving unit is provided with: the sample container and the container unit are rotatable with respect to the base together with the communication pipe, the sample container, and the container unit, with a horizontal direction orthogonal to an extending direction of the communication pipe as a central axis.
In the rotary evaporator according to claim 8, since the covering portion always covers the upper side of the communication pipe including the vapor vent, even if the container portion and the covering portion are inclined by the rotation of the driving portion, the inflow (reverse flow) of the condensate into the sample container can be suppressed.
The effects of the invention are as follows.
According to the present invention, the covering portion can suppress inflow of condensate dripping from the condenser to the vapor vent, and can suppress inflow (backflow) of condensate to the sample container.
Drawings
Fig. 1 is a perspective view of a rotary evaporator according to an embodiment.
Fig. 2 is a perspective view of the rotary evaporator of fig. 1, viewed from the rear.
Fig. 3 is a front view of the rotary evaporator of fig. 1.
Fig. 4 is a sectional view of the rotary evaporator of fig. 3.
FIG. 5 is a side view of a sample introduction valve for use with the rotary evaporator of FIG. 1.
Fig. 6 is a cross-sectional view VI-VI of fig. 5.
Fig. 7 is a cross-sectional view showing a state in which the sample introduction valve is rotated to the "atmosphere open position" with respect to fig. 4.
Fig. 8 is a cross-sectional view showing a state where the sample introduction valve is rotated to be in the "sample replenishment position" with respect to fig. 4.
FIG. 9 is a side view of the cooling vessel used in the rotary evaporator of FIG. 1, as viewed from the right side of FIG. 3.
Fig. 10 is an X-X sectional view of fig. 9.
Fig. 11 is a cross-sectional view XI-XI of fig. 10.
Fig. 12 is a view from XII in fig. 10.
Fig. 13 is a front view of the state in which the inclination angle of the sample bottle is changed from that of fig. 3.
In the figure:
1-rotary evaporator, 11-driving part, 13-communicating tube, 13 a-one end of communicating tube, 13 b-the other end of communicating tube, 15-sample bottle (sample container), 17-sample, 27-receiving bottle (condensate container), 35-condenser, 43-lower space (space where vapor vent is open), 45-container part, 47-sample introduction tube (sample supply tube), 59-protective tube (cover part), 59a opening part of protective tube, 59b, 59 c-both side edge parts of protective tube, 61, 63-gap, So-vapor vent of communicating tube.
Detailed Description
Hereinafter, embodiments will be described with reference to the drawings.
As shown in fig. 1 to 3, in the rotary evaporator 1 of the present embodiment, a support column 5 is erected on a plate-like base 3 having a substantially T-shape in plan view. The pedestal 3 and the support column 5 constitute a base. The support column 5 includes a fixed portion 5a fixed to the base 3 and a movable portion 5b attached to the fixed portion 5a so as to be movable in the vertical direction. An operation lever 7 projects horizontally from a lower portion of the movable portion 5b on the side opposite to the fixed portion 5 a. The operating lever 7 includes a base portion 7a attached to the movable portion 5b, and a rotating portion 7b rotatable with respect to the base portion 7 a. The movable portion 5b is moved up and down with respect to the fixed portion 5a by rotating the rotating portion 7b with respect to the base portion 7a and releasing the lock.
A motor case 9 having a motor, not shown, built therein is attached to an upper portion of the movable portion 5b on the side opposite to the fixed portion 5 a. The motor and the motor housing 9 are collectively referred to as a drive section 11. The motor housing 9 has a substantially rectangular parallelepiped shape elongated in the extending direction of the operation lever 7. As shown in fig. 4, a communication pipe 13 is inserted into the drive unit 11 so as to penetrate through both side surfaces of the motor case 9 having a substantially rectangular parallelepiped shape, the side surfaces facing each other. The communication pipe 13 is made of glass and is rotated by a motor of the driving part 11. In a state where the communication pipe 13 is held in the driving portion 11 so as to penetrate therethrough, the nut member 12 is screwed into an external thread portion, not shown, which is rotated together with the communication pipe 13 by driving of the motor. Therefore, when the communication pipe 13 is rotated, the nut member 12 is also rotated integrally.
Since four peripheral surfaces of the motor case 9 in the substantially rectangular parallelepiped shape in the longitudinal direction are inclined with respect to the horizontal plane and the vertical plane, the communication pipe 13 is also inclined with respect to the horizontal plane. The motor housing 9 is attached to the movable portion 5b to be rotatable about the extending direction of the operation lever 7 as a central axis. In other words, the motor housing 9 is attached to be rotatable with respect to the movable portion 5b with a horizontal direction orthogonal to the extending direction of the communication pipe 13 as a central axis. Therefore, the inclination angle of both the communication pipe 13 and the motor housing 9 with respect to the horizontal plane is variable. When the inclination angle of the motor housing 9 is changed, the locking is released by rotating the lock knob 14 attached to one side surface of the motor housing 9.
As for the communication pipe 13, one end 13a on the right side and the other end 13b on the left side in fig. 4 are open. Communication pipe 13 is inclined such that one end 13a is located lower than the other end 13 b. One end 13a has a vapor suction port Si, and the other end 13b has a vapor ejection port So. One end 13a protrudes from the motor housing 9 to the outside, and a sample bottle 15 as a sample container is connected to the protruding end portion. The sample bottle 15 contains a liquid sample 17. One end 13a of the communication tube 13 is inserted into a cylindrical connection port 15a at the distal end of the sample bottle 15. In this state, the clamp 18 is fixed to be clamped from above the connection port 15a and the one end 13 a. Therefore, the communication tube 13, the nut member 12, and the sample bottle 15 are integrally rotated by the driving of the driving unit 11.
As shown in fig. 4, a water tank 19 serving as a heating container is provided on the side of the pedestal 3. The water tank 19 contains warm water 21. The hot water 21 is heated by a heater 22 provided below the water tank 19. By immersing a part of the sample bottle 15 in the warm water 21, the sample 17 inside is heated and evaporated.
The other end 13b of the communication pipe 13 protrudes from the motor case 9 to the outside on the opposite side of the sample container 15, and the protruding end portion is inserted into the cooling container 23 made of glass. The cooling container 23 has a cylindrical shape elongated in the vertical direction, and a cylindrical mounting portion 23a protruding obliquely downward to the right in fig. 4 is formed on a side portion inclined in a conical shape at the lower portion. A nut member 25 for fixing is rotatably attached to the outer periphery of the attachment portion 23 a. The cooling container 23 can be attached to the motor case 9 by screwing the nut member 25 into an unillustrated male screw portion provided in the motor case 9. At this time, the other end 13b of the communication pipe 13 is inserted into the mounting portion 23a, and the vapor outlet So at the tip opens into the internal space of the cooling container 23.
A receiving bottle 27 serving as a condensate container for receiving condensate is attached to the lower end of the cooling container 23. The distal end of a cylindrical lower end connection port 23b formed at the lower end of the cooling container 23 is inserted into the connection port 27a of the receiving bottle 27. In this state, the clamp 28 is fixed to be clamped from above the connection port 27a and the lower end connection port 23 b.
A vacuum connection port 23c is formed in an upper portion of the cooling container 23 so as to protrude therefrom, and a vacuum nozzle 29 is connected to the vacuum connection port 23 c. The vacuum pump is connected to the vacuum nozzle 29 via a vacuum hose, not shown, and the inside of the cooling container 23 is evacuated by driving the vacuum pump. Since the inside of the cooling container 23 is communicated with the communication tube 13 and the sample bottle 15, the insides thereof are also vacuumed. The inside of the receiver bottle 27 is also vacuumed. The entire space kept in vacuum is referred to as "closed space". The position of the vacuum connection port 23c is not limited to the upper portion of the cooling container 23, and may be the lower portion of the cooling container 23, or in short, may be a position where the inside of the cooling container 23 can be evacuated.
The upper portion of the cooling container 23 is a condenser 35 in which the cooling pipe 33 is housed. The outer peripheral side of the cooling container 23 corresponding to the condenser 35 is covered with a heat insulating material 37. A coolant such as cooling water flows through the cooling pipe 33. A center pipe 39 protruding downward from the upper end of the center of the inside of the cooling container 23 is provided, and the cooling pipe 33 is provided so as to surround the center pipe 39. Inlet pipe 33a and outlet pipe 33b at the lower part of cooling pipe 33 protrude downward from the side of cooling tank 23. The heat insulating material 37 may not be provided.
Inside the cooling container 23, the inlet pipe 33a is connected in communication with an outer wrap portion 33c spirally wound along the inner surface of the cooling container 23. Inside the cooling container 23, the outlet pipe 33b is connected in communication with an inner wrap portion 33d that is spirally wound along between the outer wrap portion 33c and the center pipe 39. Although not shown, a coolant pump is connected to the inlet pipe 33a, and the coolant delivered from the coolant pump flows in. The coolant flowing into the inlet pipe 33a flows along the outer wrap portion 33c and rises, then flows along the inner wrap portion 33d and falls, and is discharged from the outlet pipe 33b to the outside.
An upper space 41 is formed above the cooling pipe 33 in the cooling container 23. A lower space 43 having a larger space volume than the upper space 41 is formed below the cooling pipe 33 in the cooling container 23 in which the vacuum connection port 23c is opened in the upper space 41. The vapor outlet So of the communication pipe 13 is opened in the lower space 43. The cooling container 23 at a position corresponding to the lower space 43 serves as a container portion 45. The upper space 41 and the lower space 43 communicate with each other through a gap between the cooling pipes 33, and a gap between the cooling pipes 33 and the inner surface of the cooling container 23 and the outer surface of the center pipe 39.
A cylindrical connection port 23d is formed in the container portion 45 at a position facing the vapor vent So, in other words, at a position of the container portion 45 at the front (the opposite side to the sample bottle 15) on the extension line of the communication tube 13 in the lower space 43 So as to protrude outward. A hollow glass sample introduction valve 49 is inserted into the connection port 23d, and a sample introduction tube 47 as a sample supply tube is connected to the tip of the sample introduction valve 49.
As shown in fig. 5 and fig. 6 which is a cross-sectional view VI-VI of fig. 5, the sample introduction valve 49 has a substantially T-shaped cross-section and includes a grip portion 51 and an insertion portion 53. The grip portion 51 is a portion to be gripped by an operator. The insertion portion 53 is a portion inserted into the connection port 23d, and includes a tapered portion 53a having a tapered tip, and a tube connection portion 53b located on the opposite side of the tapered portion 53a from the grip portion 51.
In a state where the sample introduction valve 49 is inserted into the connection port 23d, the outer peripheral surface of the tapered portion 53a is in close contact with the inner peripheral surface of the connection port 23 d. The tube connecting portion 53b is connected to be inserted into the interior of the sample introduction tube 47 made of resin. In a state where the sample introduction valve 49 is inserted into the connection port 23d, the sample introduction tube 47 penetrates the lower space 43 in the container unit 45 and the communication tube 13, and the distal end portion protrudes into the sample bottle 15. The sample introduction pipe 47 passes through the center of the communication pipe 13. Therefore, an annular gap 50 is formed between the outer peripheral surface of the sample introduction pipe 47 and the inner peripheral surface of the communication pipe 13. The slit 50 communicates the inside of the sample bottle 15 with the inside of the container portion 45, and serves as a vapor flow passage.
The sample introduction valve 49 has a communication path 55 formed inside the insertion portion 53. The communication path 55 has a sample inlet 55a opened to a side of the tapered portion 53a, and a sample discharge port 55b opened to a tip of the pipe connecting portion 53 b. The communication path 55 includes a linear portion 55c formed linearly from the sample ejection port 55b to the tapered portion 53a, and a curved portion 55d curved from an end portion of the linear portion 55c on the opposite side from the sample ejection port 55b toward the outer peripheral surface of the tapered portion 53 a. By forming the inner tube 57 inside the tapered portion 53a, a part of the linear portion 55c and the bent portion 55d are formed. The other part of the linear portion 55c is formed in the pipe connecting portion 53 b.
As shown in fig. 4, a through hole 23d1 is formed in the upper portion of the connection port 23d to pass through the inside and the outside of the connection port 23 d. A sample replenishment port 23d2 protruding obliquely downward is formed in a lower portion of the connection port 23d facing the through hole 23d 1. Although not shown, a sample replenishment hose is connected to the sample replenishment port 23d 2.
In a state where the sample introduction valve 49 is inserted into the connection port 23d, the sample introduction port 55a of the communication path 55 is aligned with the through hole 23d1, whereby the "closed space" inside the sample bottle 15, the communication tube 13, and the cooling container 23 is opened to the atmosphere through the sample introduction tube 47 communicating with the communication path 55. This state is referred to as "atmosphere open position" shown in fig. 7.
In a state where the sample introduction valve 49 is rotated by 180 degrees from the "atmosphere open position", the sample introduction port 55a of the communication passage 55 communicates with the sample replenishment port 23d 2. This state is referred to as "sample replenishment position" shown in fig. 8. In the "sample replenishment position", the sample can be replenished from the sample replenishment hose to the sample bottle 15 through the sample replenishment port 23d2, the communication path 55, and the sample introduction tube 47.
In a state where the sample introduction valve 49 is positioned between the "atmosphere opening position" and the "sample replenishment position" with respect to the connection port 23d, the sample introduction port 55a of the communication passage 55 is blocked by the inner surface of the connection port 23 d. At this time, the "sealed space" is kept in a vacuum state, and this state is referred to as a "vacuum holding position" shown in fig. 4.
As shown in fig. 4, a protective tube 59 made of glass as a covering member is attached between the attachment portion 23a and the connection port 23d which are located at positions facing the container portion 45. The protection pipe 59 is connected to the container portion 45 in a sealed state by glass welding. The protection pipe 59 is provided in the lower space 43 So as to cover the upper side of the communication pipe 13 including the vapor outlet So and the upper side of the sample introduction pipe 47. Therefore, similarly to the sample introduction tube 47, the protection tube 59 is inclined so that the attachment portion 23a side is lower in vertical height than the connection port 23d side.
The protection tube 59 has an opening 59a formed at a lower portion thereof. The opening 59a is a vapor flow outlet for allowing the vapor jetted from the vapor jetting port So to flow out to the lower space 43. The opening 59a is an elongated hole formed over substantially the entire length between the attachment portion 23a and the connection port 23 d. The protection tube 59 has an opening 59a formed in a tapered cylindrical tube. The cylindrical tube, which is a material of the protection tube 59 before the opening 59a is formed, has a circular cross section, and the diameter of the cylindrical tube is larger on the mounting portion 23a side and gradually decreases toward the connection port 23d side.
The opening 59a is formed below the center of the circular cross section of the cylindrical pipe. Therefore, as shown in fig. 11, the protective tube 59 is bent toward the inside of the protective tube 59 so that both side edge portions 59b and 59c of the portion corresponding to the opening portion 59a in the extending direction of the communication pipe 13 are close to each other.
As shown in fig. 11, the protection pipe 59 is located at the center in the diameter direction of the cooling vessel 23. Therefore, gaps 61 and 63 are formed between the left and right side portions of the protective tube 59 and the inner surface of the container portion 45 in fig. 11. The steam flowing out downward from the opening 59a rises through the gaps 61 and 63.
In the rotary evaporator configured as described above, the cooling liquid is circulated from the inlet pipe 33a to the cooling pipe 33, thereby cooling the inside of the cooling container 23. By operating the vacuum pump, the "closed space" including the inside of the cooling container 23 is vacuumed by the vacuum pipe 29. At this time, the sample introduction valve 49 is in the "vacuum holding position" shown in fig. 4.
Before the sample bottle 15 is attached to the communication tube 13, the sample 17 is put into the sample bottle 15 in advance. When the sample bottle 15 is attached to the communication tube 13, the sample bottle 15 is attached to a position separated upward from the water tank 19 with respect to the position of fig. 4, and after the attachment, the movable portion 5b of the support 5 is lowered with respect to the fixed portion 5 a. As a result, the sample bottle 15 descends, and the sample 17 enters the hot water 21 as shown in fig. 4. The warm water 21 is heated by a heater 22.
In this state, the operation panel 64 shown in fig. 1 and 3 is operated to drive the motor in the motor housing 9, thereby rotating the communication tube 13 together with the sample bottle 15. By rotating the sample bottle 15, the sample 17 becomes a liquid film and adheres to the inner surface of the sample bottle 15. The sample 17 is evaporated from the liquid film and the liquid surface adhering to the inner surface of the sample bottle 15 to become a vapor 65. Since a liquid film is formed, the evaporation efficiency becomes high. Since the "closed space" is vacuum, the boiling point of sample 17 is lowered and evaporation becomes easier.
As shown by arrow a in fig. 4, the vapor 65 flows from the inside of the sample bottle 15 through the vapor suction port Si, enters the gap 50 between the communication pipe 13 and the sample introduction pipe 47, and flows toward the cooling container 23 in the gap 50. The steam flowing along the slit 50 flows out from the steam spouting port So to the lower space 43 of the container portion 45. Since the upper side of the vapor spouting port So is covered with the protection pipe 59, the vapor spouting port So does not move upward immediately after flowing out, but moves downward from the opening 59a in the lower portion, and then passes through the gaps 61 and 63 and rises in the lower space 43 as shown by an arrow B in fig. 11.
The vapor that has risen in the lower space 43 further rises in the condenser 35. The vapor exchanges heat by contacting the cooling pipe 33 to become a condensate 67, and drops into the lower space 43. At this time, since the center pipe 39 is disposed at the center of the cooling container 23, the vapor efficiently flows to the cooling pipe 33 outside the center pipe 39, and the condensation efficiency in the condenser 35 is increased.
The condensate 67 drips from the cooling pipe 33 and the center pipe 39 to become a concentrated liquid and is stored in the receiving bottle 27 shown in fig. 4. At this time, the condensate 67, which has dropped particularly from the vicinity of the center tube 39, drops on the protective tube 59, flows down along the curved surface of the outer surface of the protective tube 59, and flows toward the receiver bottle 27.
In this case, the condensate 67 dripping from the condenser 35 can be prevented from contacting the sample introduction pipe 47 by the protection pipe 59. Therefore, the condensate 67 can be prevented from flowing along the sample introduction tube 47 and flowing back into the sample bottle 15. Since the protection tube 59 covers the upper side of the communication tube 13 including the vapor vent So, the condensate 67 dropped from the condenser 35 is prevented from entering the communication tube 13 from the vapor vent So and flowing back into the sample bottle 15.
In the process of performing the separation and concentration operation, when the sample in the sample bottle 15 is reduced and the separation and concentration operation is further continued, the inclination angle of the sample bottle 15 is changed more steeply as shown in fig. 13. When the inclination angle of the sample bottle 15 is changed, the driving unit 11 including the motor housing 9 is rotated with respect to the movable unit 5b of the column 5. At this time, the cooling container 23 and the receiver bottle 27 are also rotated integrally and tilted.
Since the inclination angle of the sample bottle 15 becomes steeper (becomes closer to the vertical state), the sample (liquid film) which has adhered to the entire inner surface of the sample bottle 15 and has not evaporated easily flows down toward the bottom of the sample bottle 15. This enables efficient separation and concentration even when the amount of the sample decreases.
When the separation and concentration operation is further continued, the sample introduction valve 49 is rotated to change the "vacuum holding position" in fig. 4 to the "sample replenishing position" in fig. 8. In the "sample addition position", the sample is added from a sample addition hose, not shown, connected to the sample addition port 23d 2. The sample is replenished by vacuum suction in a state where the "closed space" is kept in a vacuum state. The sample drawn out by vacuum suction is supplied to the sample bottle 15 through the sample introduction tube 47. After the sample is replenished, the sample introduction valve 49 is rotated to return to the "vacuum holding position" in fig. 4.
The rotary evaporator 1 of the present embodiment includes: a sample bottle 15 for storing a sample 17; a communication tube 13 having one end 13a connected to the sample bottle 15 and the other end 13b provided with a vapor outlet So for discharging vapor evaporated from the sample 17; and a driving unit 11 for driving the communicating tube 13 to rotate together with the sample bottle 15. The rotary evaporator 1 has: a container portion 45 having a lower space 43 in which a vapor vent So opens; a condenser 35 provided above the lower space 43 and condensing the vapor ejected from the vapor ejection port So; and a receiver bottle 27 provided below the lower space 43 and receiving the condensate condensed by the condenser 35 through the lower space 43.
A protection pipe 59 is provided in the lower space 43 of the container portion 45, and the protection pipe 59 covers the upper side of the vapor spouting port So. The protection pipe 59 has one end connected to the side of the container portion 45 where the vapor spouting port So is open and the other end connected to the side of the container portion 45 opposite to the side where the vapor spouting port So is open, and has an opening portion 59a formed in a lower portion thereof for allowing the vapor spouted from the vapor spouting port So to flow out to the lower space 43.
Therefore, the condensate 67 dropped from the condenser 35 can be prevented from entering the communication tube 13 from the vapor outlet So and flowing back into the sample bottle 15. By suppressing the backflow of the condensate 67 to the sample bottle 15, the condensate can be recovered more efficiently, and the separation and concentration operation can be performed more efficiently.
In the present embodiment, the sample introduction tube 47 for supplying the sample 17 from the outside of the container portion 45 on the other end side of the protection tube 59 to the sample bottle 15 is inserted into the communication tube 13 through the lower side of the protection tube 59. In this case, the condensate 67 dripping from the condenser 35 can be prevented from contacting the sample introduction pipe 47 by the protection pipe 59. This can prevent the condensate 67 from flowing back into the sample vial 15 along the sample introduction tube 47. By suppressing the backflow of the condensate 67 to the sample bottle 15, the condensate can be recovered more efficiently, and the separation and concentration operation can be performed more efficiently.
One end and the other end of the protection tube 59 of the present embodiment are connected to the container portion 45 in a sealed state. Therefore, the condensate flowing down along the inner surface of the container portion 45 can be prevented from entering the inner side of the protection tube 59, and the condensate can be prevented from flowing back into the sample vial 15.
The container portion 45 and the protection pipe 59 of the present embodiment are made of glass, and the container portion 45 and one end and the other end of the protection pipe 59 are connected by glass welding. Therefore, the container portion 45 and the protection pipe 59 can be connected in a sealed state by a simple operation of glass welding.
The protection pipe 59 of the present embodiment is bent toward the inside of the protection pipe 59 so that both side edge portions 59b, 59c of a portion corresponding to the opening portion 59a in the extending direction of the communication pipe 13 are close to each other. In this case, when condensate dripping on the protective tube 59 flows down along the outer surface of the protective tube 59, it is difficult to enter the inside of the protective tube 59. Therefore, the condensate can be more reliably prevented from coming into contact with sample introduction tube 47 and flowing into vapor vent So of communication tube 13, and the condensate can be more reliably prevented from flowing back into sample bottle 15.
The protective tube 59 of the present embodiment has a circular arc-shaped cross section in a direction orthogonal to a direction connecting one end and the other end. Therefore, the condensate dripping on the protective tube 59 quickly flows down along the outer surface of the arc shape of the protective tube 59, and can be efficiently accumulated in the receiver bottle 27.
In the protection tube 59 of the present embodiment, gaps 61 and 63 are formed between both side portions between the one end and the other end and the inner surface of the container portion 45. Therefore, the vapor flowing out of the opening portion 59a of the protection pipe 59 into the lower space 43 passes through the gaps 61 and 63 on both sides of the protection pipe 59, and the vapor flows into the condenser 35 more uniformly.
The drive unit 11 of the present embodiment is configured to be rotatable with respect to the movable portion 5b of the column 5 together with the communication tube 13, the sample bottle 15, and the container unit 45, with a horizontal direction orthogonal to the extending direction of the communication tube 13 as a central axis. At this time, since the protection tube 59 always covers the upper side of the sample introduction tube 47 and the upper side of the vapor ejection port So, even if the container portion 45 and the protection tube 59 are inclined by the rotation of the driving portion 11, the inflow (reverse flow) of the condensate into the sample bottle 15 can be suppressed.
While the embodiments of the present invention have been described above, the above embodiments are merely simple examples described for easy understanding of the present invention, and the present invention is not limited to the embodiments. The technical scope of the present invention is not limited to the specific technical matters disclosed in the above embodiments, but includes various modifications, alterations, substitutions, and the like that can be easily derived from the technical matters.
For example, the protection pipe 59 is not limited to the circular arc shape in cross section, and may be opened at the lower portion and have a triangular or rectangular cross section. The protection tube 59 need not have a tapered shape in the longitudinal direction, but may be formed in a cylindrical shape having a constant diameter in the longitudinal direction and have an opening formed at the lower portion. In short, the protection pipe 59 may be configured to cover the vapor outlet So of the communication pipe 13 and the upper side of the sample introduction pipe 47. As shown in fig. 12, one opening 59a of the protection tube 59 is formed in an elliptical shape, but a plurality of openings such as circular openings may be formed.

Claims (8)

1. A rotary evaporator, comprising:
a sample container for storing a sample;
a communicating pipe having one end connected to the sample container and the other end provided with a vapor outlet for discharging vapor evaporated from the sample;
a driving unit that drives the communicating tube to rotate together with the sample container;
a container portion having a space in which the vapor vent is open;
a condenser provided above the space of the container portion and condensing the vapor discharged from the vapor discharge port;
a condensate container provided below the space of the container portion and receiving condensate condensed by the condenser through the space; and
a covering part which is provided in the space of the container part and covers an upper side of the steam vent,
the covering portion has one end connected to a side of the container portion on which the vapor spouting port opens and the other end connected to a side of the container portion opposite to the side of the container portion on which the vapor spouting port opens, and an opening portion formed in a lower portion thereof for allowing vapor spouted from the vapor spouting port to flow out into the space.
2. A rotary evaporator according to claim 1,
a sample supply tube for supplying the sample to the sample container from the outside of the container portion on the other end side of the covering portion passes through the lower side of the covering portion and is inserted into the communication tube.
3. A rotary evaporator according to claim 1 or 2,
the one end and the other end of the covering portion are connected to the container portion in a sealed state.
4. A rotary evaporator according to claim 3,
the container portion and the cover portion are made of glass, and the container portion and the one end and the other end of the cover portion are connected by glass welding.
5. A rotary evaporator according to any one of claims 1 to 4,
the covering portion is bent toward the inside of the covering portion so that both side edge portions of a portion corresponding to the opening portion in the extending direction of the communication pipe are close to each other.
6. A rotary evaporator according to any one of claims 1 to 5,
the cross-sectional shape of the covering portion in a direction orthogonal to a direction connecting the one end and the other end is an arc shape.
7. A rotary evaporator according to any one of claims 1 to 6,
the covering part forms a gap between the inner surface of the container part and both side parts between the one end and the other end.
8. A rotary evaporator according to any one of claims 1 to 7,
the drive section is configured to: the sample container and the container unit are rotatable with respect to the base together with the communication pipe, the sample container, and the container unit, with a horizontal direction orthogonal to an extending direction of the communication pipe as a central axis.
CN201910334135.4A 2019-02-22 2019-04-24 Rotary evaporator Pending CN111603794A (en)

Applications Claiming Priority (2)

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JP2019-030202 2019-02-22
JP2019030202A JP7209346B2 (en) 2019-02-22 2019-02-22 rotary evaporator

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08168602A (en) * 1994-12-15 1996-07-02 Tokyo Rika Kikai Kk Cooler for rotary evaporator
CN102006937A (en) * 2008-05-09 2011-04-06 严永禄 Teflon container for sample decomposition using gas condensation by air cooling
CN105823353A (en) * 2016-03-23 2016-08-03 东华大学 High-efficiency condenser
CN206152366U (en) * 2016-10-20 2017-05-10 绿城农科检测技术有限公司 Rotary evaporato and be used for rotary evaporato's anti -return piecing devices
CN108815873A (en) * 2018-06-30 2018-11-16 淮阴工学院 A kind of acetic acid rectifying column built in condenser, reboiler

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE202011106544U1 (en) 2011-10-08 2013-01-09 Knf Neuberger Gmbh rotary evaporator

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08168602A (en) * 1994-12-15 1996-07-02 Tokyo Rika Kikai Kk Cooler for rotary evaporator
CN102006937A (en) * 2008-05-09 2011-04-06 严永禄 Teflon container for sample decomposition using gas condensation by air cooling
CN105823353A (en) * 2016-03-23 2016-08-03 东华大学 High-efficiency condenser
CN206152366U (en) * 2016-10-20 2017-05-10 绿城农科检测技术有限公司 Rotary evaporato and be used for rotary evaporato's anti -return piecing devices
CN108815873A (en) * 2018-06-30 2018-11-16 淮阴工学院 A kind of acetic acid rectifying column built in condenser, reboiler

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