WO2019153679A1 - 一种可自动控制连续进出料的旋转蒸发仪 - Google Patents

一种可自动控制连续进出料的旋转蒸发仪 Download PDF

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Publication number
WO2019153679A1
WO2019153679A1 PCT/CN2018/099522 CN2018099522W WO2019153679A1 WO 2019153679 A1 WO2019153679 A1 WO 2019153679A1 CN 2018099522 W CN2018099522 W CN 2018099522W WO 2019153679 A1 WO2019153679 A1 WO 2019153679A1
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Prior art keywords
port
discharge
discharging
pipe
passage
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PCT/CN2018/099522
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English (en)
French (fr)
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温淑瑶
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北京师范大学
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/0082—Regulation; Control
    • 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
    • B01D3/42—Regulation; Control

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  • the present invention relates to the field of evaporation equipment, and in particular to a rotary evaporator, and more particularly to a rotary evaporator capable of automatically feeding in and out.
  • the rotary evaporator is an extraction experimental equipment for vacuum distillation of materials. It is widely used in experiments such as scale concentration, drying, extraction and recovery of samples, especially for rapid distillation of large amounts of solvents.
  • the existing rotary evaporator is usually composed of a vacuuming device, a heating device, a condensing device, a rotating device and the like.
  • the principle of the rotary evaporator is mainly controlled by electronic equipment, so that the flask is rotated at a constant speed to form a film at a constant speed. The evaporation area is increased, and the evaporation flask is brought to a negative pressure state by a vacuum pump.
  • the evaporation flask is heated in a water bath or an oil bath while being rotated, and the heating temperature is close to the boiling point of the solvent, so that the solution in the bottle is negative.
  • the film is heated and diffused by evaporation to evaporate to achieve rapid evaporation of the solvent.
  • the existing rotary evaporator has a low degree of automation, and is inseparable from the experimenter. Each step requires manual operation by the experimenter, and the fraction and the concentrate cannot be automatically taken out during use, and the rotary distillation must be interrupted during discharge.
  • the operation, the atmosphere, the vacuum pump, the distillation bottle can be removed to remove the distillation bottle for cleaning. Taking a 3L distillation bottle as an example, it takes about 18 minutes to distill about 220 mL of the solution, but the actual completion of a complete set of rotary evaporation operation is required. 60 minutes. This not only makes the work that requires continuous distillation impossible to carry out automatically and efficiently, but also increases the workload of operation and maintenance, reduces work efficiency and affects the progress of work.
  • the glass flange and the retort mouth connected to the retort are easily broken during the installation and removal of the retort.
  • Chinese patent CN203447781U discloses a rotary evaporator capable of automatically feeding in and out.
  • the rotary evaporator is provided with a four-way pipe between the condenser and the receiving bottle, and one side outlet of the four-way pipe is connected with the feeding pipe.
  • the connection realizes the automatic feeding of the liquid to be evaporated; after the end of the evaporation, the concentrated liquid can be sucked out through the feeding tube, thereby eliminating the complicated operation of removing the evaporation bottle and pouring out the concentrated liquid.
  • the device realizes the feeding and discharging under the manual command of the rotary evaporator, the inlet and the discharge share a tube has a certain degree of pollution to the feeding or discharging, and the continuous feeding and discharging under the automatic control cannot be realized. Cleaning operation. During the work process, it is still necessary to wait for the manual discharge and manual cleaning after the end of evaporation, and the continuous feeding, discharging and cleaning in the distillation process cannot be realized.
  • the invention provides a rotary evaporator with multiple modes selectable, intelligent electronic devices such as a computer or a touch screen, which can automatically control the feeding, discharging, discharging and fractionating, and can automatically repeat a complete operation step of a certain mode, and solves the present problem.
  • the rotary evaporator has low automation, can not continuously feed and discharge, clean and discharge the fraction, that is, realizes the intelligence of the rotary evaporator, and solves the problem that the rotary evaporation process cannot be separated from the experimenter.
  • the present invention provides a rotary evaporator capable of automatically feeding in and out, comprising a bracket having a detachable distillation bottle and a condenser fixed thereto, and a receiving bottle connected to the bottom of the condenser, a venting passage is formed in the condenser, the venting passage is in communication with the distillation bottle, and a vent pipe is formed at a side wall of the condenser, and a venting valve is disposed at the atmosphere of the vent pipe for controlling The interior of the distillation system is in communication with the atmosphere;
  • the venting passage is further provided with a feeding passage and a discharging passage, wherein the feeding passage and the discharging passage are respectively connected with the feeding port and the discharging port formed at the vent pipe, and pass through the feeding valve And the discharge valve for control;
  • the feeding port and the discharging port are respectively connected with a power device to realize automatic feeding and discharging.
  • the feed port and the discharge port are respectively connected with a feed pipe and a discharge pipe, and the feed pipe and the discharge pipe extend into the distillation bottle.
  • the outlet pipe extends into the end of the distillation bottle and is provided with a weighting ring.
  • a cleaning passage is further disposed in the ventilation passage, and the cleaning passage is in communication with a cleaning port formed at the ventilation pipe, and is controlled by a cleaning valve.
  • the cleaning port is connected with a cleaning tube, and the cleaning tube extends into the distillation bottle; the cleaning port is connected with a power device to realize automatic liquid inlet cleaning.
  • the venting passage is further provided with a drain passage, and the drain passage is connected with a drain port formed at the vent pipe, and is controlled by a drain valve.
  • the liquid discharge port is connected with a liquid discharge pipe, and the liquid discharge pipe extends into the distillation bottle; the liquid discharge port is connected with a power device to realize automatic discharge of the cleaning liquid.
  • the drain pipe extends into the end of the distillation bottle and is provided with a weighting ring.
  • a distillate discharge passage is also disposed in the vent passage, and the distillate discharge passage communicates with a distillate discharge port formed at the vent pipe, and is controlled by a distillate discharge valve.
  • the distillate discharge port is connected with a distillate discharge pipe, and the distillate discharge pipe extends into a lowest liquid level in the collection bottle; and the distillate discharge port is connected with a power device to realize automatic discharge of the distillate.
  • the end of the fraction discharge pipe extending into the collection bottle is provided with a weighting ring.
  • the feeding pipe, the discharging pipe, the cleaning pipe, the liquid discharging pipe and the discharging pipe are PTFE pipes;
  • the feed valve, the discharge valve, the purge valve, the drain valve and the fractionation valve are polytetrafluoroethylene valves or glass valves.
  • the vent pipe is a multi-pass pipe having a plurality of outlets integrally formed with the condenser, or the vent pipe is a multi-pass pipe that is hermetically connected to the detachable glass grinding port of the condenser.
  • An automatic control component is connected to the vacuum port on the air outlet, the feed port, the discharge port, the cleaning port, the liquid discharge port, the fraction discharge port and the condenser wall .
  • the rotary evaporator capable of automatically feeding in and out according to the present invention is creatively improved based on the structure of the existing rotary evaporator, and the passage channel common to the atmosphere and the feed is added through the feeding channel, the discharge channel, and the cleaning.
  • Channels, drain channels, and fractionation channels, each controlled by a peristaltic pump, or automatically controlled by a computer, can achieve automatic feeding and discharging, automatic cleaning and drainage, automatic fractionation, avoiding complications
  • the manual operation effectively reduces the workload, so that the distillation process can be operated automatically, continuously and efficiently, which greatly reduces the workload of operation and maintenance.
  • the rotary evaporator of the invention is further provided with an automatic control component connected to each of the inlet and outlet ends, and can set a plurality of working modes, and can automatically repeat the work of a certain mode by setting the number of times, thereby solving the experimenter's time.
  • the problem of distillation operation and a large number of repetitions of a set of operations is indispensable.
  • the rotary evaporator of the invention adopts an automatic control system to realize automatic feeding and discharging, automatic cleaning, liquid discharging and fractionating, so that the entire rotary evaporator can effectively reduce the lifting motor without using the automatic lifting assembly and its control components.
  • the components such as the hydraulic ram also reduce the high cost caused by the maintenance of the automatic lifting assembly, which effectively ensures the continuous and efficient operation of the rotary evaporator.
  • Figure 1 is a schematic view showing the first structure of the rotary evaporator of the present invention
  • FIG. 2 is a schematic view showing the second structure of the rotary evaporator of the present invention.
  • FIG. 3 is a third structural schematic view of the rotary evaporator of the present invention.
  • Figure 4 is a fourth structural schematic view of the rotary evaporator of the present invention.
  • Figure 5 is a schematic structural view of the automatic control component of the present invention.
  • the rotary evaporator of the present invention comprises a support 1 and a rotary electric machine 25 for controlling the rotation of the rotary evaporator.
  • the rotary evaporator of the present invention can also be provided with parameters for controlling the rotary electric machine.
  • the speed control panel not shown in the figure).
  • a detachable distillation bottle 2 and a condenser 3 are fixed on the bracket 1, and the distillation bottle 2 and the condenser 3 are connected to each other to realize distillation of the liquid, and the receiving bottle 4 is connected to the bottom of the condenser for receiving evaporation. Solvent.
  • the bottom of the receiving bottle 4 may be provided with a passage for discharging the fraction and a switch for controlling the passage (not shown).
  • a venting passage 5 is formed in the condenser 3, and the venting passage 5 communicates with the retort 2 for communicating with the atmosphere inside the distillation system, and the venting passage 5 passes through the condenser 3.
  • a vent pipe 6 is formed at the side wall of the condenser 3, and the vent pipe 6 is provided with a venting valve 7 at its end position at the through-air port 30 for controlling the venting port 30 Opening and closing to control the communication between the inside of the distillation system and the atmosphere.
  • the vent pipe 6 of the present invention may be a multi-pass pipe having a plurality of outlets integrally formed with the condenser 3, or the vent pipe 6 may be the same as the condenser 3 Remove the multi-way tube that is in a closed connection (such as a glass-grinding seal).
  • the venting passage 5 is further provided with a feeding passage 8 for inputting a liquid to be concentrated and a discharging passage 9 for outputting a concentrated liquid
  • the venting pipe 6 is a four-way pipe.
  • the feed passage 8 and the discharge passage 9 communicate with the feed port 10 and the discharge port 11 formed at the side wall of the vent pipe 6, respectively, and pass through a feed valve provided at the feed port 10. 12 and a discharge valve 13 disposed at the discharge port 11 perform switching control.
  • the feeding port 10 and the discharging port 11 are respectively connected with a power device, which can control the feeding and withdrawing of the liquid, thereby realizing automatic feeding and discharging, and the power device can be a peristaltic pump or a vacuum pump.
  • the vacuum system in the distillation system is realized.
  • the space between the inside of the ventilation passage 5 and the feed passage 8 and the discharge passage 9 is an atmosphere communication space, and the switch can be controlled by the ventilation valve 7.
  • the feed port 10 and the discharge port 11 are also respectively connected with a feed pipe 14 and a discharge pipe 15, and the feed pipe 14 and the discharge pipe 15 both extend into the distillation.
  • the discharge pipe 15 extends into the end of the distillation bottle 2 and is further provided with a weighting ring 16 so that the discharge pipe 15 can often be in the distillation.
  • the lowest liquid level of the bottle 2 is discharged as much as possible, and the weighting ring 16 is preferably a weighting ring made of a polytetrafluoroethylene material.
  • the feed pipe 14 and the discharge pipe 15 of the present invention are polytetrafluoroethylene pipes, and the feed valve 12 and the discharge valve 13 are also designed as polytetrafluoroethylene. Vinyl valve or glass valve.
  • the vent pipe 6 is a five-way pipe structure, and the vent passage 5 is further provided with a feed passage 8 for inputting a liquid to be concentrated, and for outputting the concentrate.
  • the material channel 9 and the cleaning channel 17 for inputting a cleaning liquid such as distilled water or ethanol.
  • the feed channel 8, the discharge channel 9 and the cleaning channel 17 are respectively connected to the inlet port 10, the discharge port 11 and the cleaning port 18 formed at the side wall of the vent pipe 6, and are disposed through the The feed valve 12 at the feed port 10, the discharge valve 13 provided at the discharge port 11, and the purge valve 19 provided at the cleaning port 18 perform switching control.
  • the feed port 10, the discharge port 11 and the cleaning port 18 are respectively connected with a peristaltic pump or a vacuum pump to evacuate the distillation system, etc., and the liquid can be controlled to be fed in and out.
  • automatic feeding and discharging and automatic cleaning are realized.
  • the space between the inside of the ventilation passage 5 and the feeding passage 8, the discharge passage 9 and the washing passage 17 is an atmosphere communication space, and the switch can be controlled by the ventilation valve 7.
  • the feed channel 8, the discharge channel 9 and the cleaning channel 17 are also respectively connected with a feed pipe 14, a discharge pipe 15, and a cleaning pipe 20, the feed pipe 14, and the discharge pipe Both the tube 15 and the cleaning tube 20 extend into the distillation bottle 2.
  • the discharge pipe 15 extends into the end of the distillation bottle 2 and is also provided with a weighting ring 16 so that the end of the discharge pipe 15 can often be in the distillation bottle 2
  • the weighting ring 16 is preferably a weighting ring made of a polytetrafluoroethylene material.
  • the feed pipe 14, the discharge pipe 15 and the cleaning pipe 20 of the present invention are polytetrafluoroethylene pipes, and the feed valve 12, the discharge valve 13 and the cleaning
  • the valve 19 is also designed as a Teflon valve or a glass valve.
  • the vent pipe 6 is a six-way pipe structure, and the vent passage 5 is further provided with a feed passage 8 for inputting a liquid to be concentrated, and for outputting the concentrate.
  • the feed channel 8, the discharge channel 9, the cleaning channel 17, and the liquid discharge channel 21 are respectively formed with the inlet port 10, the discharge port 11, the cleaning port 18, and the liquid discharge port formed at the side wall of the vent pipe 6.
  • the drain valve 23 provided at the drain port 22 performs switching control.
  • the feed port 10, the discharge port 11, the cleaning port 18 and the liquid discharge port 22 are respectively connected with a peristaltic pump or a power device such as a vacuum pump, which can control the feeding and withdrawing of the liquid.
  • the space between the interior of the venting passage 5 and the feeding passage 8, the discharge passage 9, the washing passage 17, and the drain passage 21 is an atmosphere communication space, and is controlled by the vent valve 7.
  • the switch can connect or block the atmosphere.
  • the feed port 10, the discharge port 11, the cleaning port 18, and the liquid discharge port 22 are also connected with a feed pipe 14, a discharge pipe 15, a cleaning pipe 20, and a drain pipe 24, respectively.
  • the feed pipe 14, the discharge pipe 15, the cleaning pipe 20, and the drain pipe 24 all extend into the distillation bottle 2.
  • the discharge pipe 15 and the discharge pipe 24 extend into the end of the distillation bottle 2 and are respectively provided with a weighting ring 16 so that the discharge pipe 15 and the discharge pipe 24 can often be at the lowest liquid level of the retort 2, expelling the concentrate and the cleaning liquid as much as possible, and the weighting ring 16 is preferably a weighting ring made of a polytetrafluoroethylene material.
  • the feeding tube 14, the discharging tube 15, the cleaning tube 20 and the liquid discharging tube 24 of the present invention are polytetrafluoroethylene tubes, and the feeding valve 12 and the out The material valve 13, the purge valve 19 and the drain valve 23 are also designed as Teflon valves or glass valves.
  • the vent pipe 6 is a seven-way pipe structure, that is, based on the structure of the rotary evaporator shown in FIG. 3, the ventilating passage 5 is also provided with useful
  • the fraction of the output fraction is discharged from the passage 26, and the fraction discharge passage 26 communicates with the fraction discharge port 28 formed at the side wall of the vent pipe 6, and passes through the distillate discharge valve 29 provided at the distillate discharge port 28. Switching control is performed, and the fraction discharge port 28 is connected to the fraction discharge pipe 27 to discharge the fraction.
  • the other end of the fraction discharge pipe 27 extends into the bottom of the collection bottle 4 and is provided with a weighting ring 16.
  • the fraction discharge port 28 is also connected with a peristaltic pump or a power device such as a vacuum pump, which can control the extraction of the liquid, thereby realizing the automatic extraction of the fraction.
  • the collection bottle 4 can also be a structure with a lower end liquid discharge port generally in the prior art, and the liquid discharge port can be controlled by a valve.
  • the discharge port can also be connected to a power device such as a peristaltic pump or a vacuum pump to achieve direct discharge of the fraction.
  • the through port 30, the feed port 10, the discharge port 11, the cleaning port 18, the liquid discharge port 22, the distillate discharge port 28, and the condenser wall An automatic control unit is connected to the vacuum nozzle to achieve automatic control of the entire rotary evaporator.
  • the control assembly structure shown in FIG. 5 has an interface end L1 connected to the feed port 10 and controlled by a solenoid valve K1 and a trim valve N, and connected to the feed tank P1 through a pipe, the trim valve N can replace the feed valve 12 to control the feeding process.
  • the electronic scale B is arranged under the feeding tank P1 to control the accurate feeding.
  • the electronic scale B has the communication function and can communicate with the computer.
  • the interface end L2 is connected to the cleaning port 18, and is controlled by the electromagnetic valve K2 and the ball valve V2, and is connected to the cleaning liquid tank P2 through a pipe.
  • the ball valve V2 can be replaced by the cleaning liquid valve 19.
  • Control, the electronic scale B under the cleaning liquid tank P2 controls the amount of the cleaning liquid accurately.
  • the interface end L3 is connected to the through port 30 of the vent pipe 6 through a pipe, and is controlled by a solenoid valve K3 and a ball valve V3, and the ball valve V3 can replace the vent valve 7 .
  • the interface end L4 is connected to the liquid discharge port 22, and is controlled by the electromagnetic valve K4 and the ball valve V4-1, and is connected to the waste washing liquid tank P4 through the pipe, and the ball valve V4-1 can be Instead of the drain valve 23, a waste drain port is provided under the waste washer tank P4, and a venting port is provided thereon, which is controlled by ball valves V4-2 and V4-3, respectively.
  • the waste washing liquid tank P4 is connected to the vacuum pump D through a pipe (and is connected with a pressure gauge M and a filter F), and the waste washing liquid is discharged by vacuuming.
  • the interface end L5 is connected to the discharge port 11, and is controlled by a solenoid valve K5 and a ball valve V5-1, and is connected to the concentration liquid tank P5 through a pipe, the ball valve V5- 1 can replace the discharge valve 13, the concentrated liquid tank P5 is provided with a liquid discharge port, and there is a venting port, which is controlled by ball valves V5-2 and V5-3 respectively.
  • the concentrating liquid tank P5 is connected to the vacuum pump D through a pipe (and a pressure gauge M and a filter F are connected), and the distillation concentrate is discharged by vacuuming.
  • the interface end L6 is connected to the distillate discharge port 28, and is controlled by a solenoid valve K6 and a ball valve V6-1, and is connected to the fraction collection tank P6 through a pipe, the ball valve V6-1
  • the distillate discharge valve 29 can be replaced, and the distillate collection tank P6 is provided with a liquid discharge port, and a venting port is provided thereon, which is controlled by ball valves V6-2 and V6-3, respectively.
  • the fraction collection tank P6 is connected to the vacuum pump D through a pipe (and is connected with a pressure gauge M and a filter F), and the fraction is discharged by evacuation.
  • the interface end L7 is connected to the vacuum port on the condenser wall through a pipe, and is connected to the solenoid valve K7 and the ball valve V7 and the vacuum pump D (and the pressure gauge M and the filter F are connected).
  • control component all the solenoid valves are controlled and turned on and off by a computer, and the computer also controls the temperature control and time of the electronic scale, the motor, the vacuum pump, and the heating pot with communication functions.
  • a plurality of working modes are set in the computer, and the computer controls the rotary evaporator to perform each step according to a set mode.
  • the mode is completely controlled by the computer.
  • the specific steps include:
  • the mode is completely controlled by the computer, and the specific operation steps include:
  • the mode is completely controlled by the computer, and the specific operation steps include:
  • the mode is completely controlled by the computer, and the specific operation steps include:
  • the mode is completely controlled by the computer, and the specific steps include:
  • the mode is completely controlled by the computer, and the specific steps include:
  • the solenoid valve K3 is kept open, the solenoid valves K6 and K7 are opened, and the fraction in the collection bottle is drained (time control), and K6 is closed after completion;

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

Abstract

一种可自动控制连续进出料的旋转蒸发仪，包括支架(1)，支架(1)上固定有可拆卸的蒸馏瓶(2)和冷凝器(3)，冷凝器(3)底部连接有接收瓶(4)，冷凝器(3)内成型有通气通道(5)，通气通道(5)与蒸馏瓶(2)相连通，并在冷凝器(3)的侧壁处形成通气管(6)，通气管(6)的通大气口(30)处设置有通气阀(7)用于控制蒸馏系统内部与大气的连通；通气通道(5)内还设置有进料通道(8)和出料通道(9)，进料通道(8)和出料通道(9)分别与成型于通气管(6)处的进料口(10)和出料口(11)相连通，并通过进料阀(12)和出料阀(13)进行控制；进料口(10)和出料口(11)分别连接有动力装置，实现在旋转蒸发仪使用过程中的自动进料和出料，避免了频繁的人工操作。

Description

一种可自动控制连续进出料的旋转蒸发仪 技术领域
本发明涉及蒸发设备技术领域，特别地，涉及一种旋转蒸发仪，特别涉及一种可自动进出料的旋转蒸发仪。
背景技术
旋转蒸发仪是对物料进行减压蒸馏浓缩的一种提取实验设备，其广泛应用于样品的规模浓缩、干燥、提取回收等实验中，尤其用于快速蒸馏大量溶剂。现有旋转蒸发仪通常由抽真空装置、加热装置、冷凝装置、旋转装置等组件组成，旋转蒸发仪的原理主要是通过电子设备控制，使烧瓶在最适合转速下，恒速旋转使溶剂形成薄膜，增大蒸发面积，并通过真空泵使蒸发烧瓶处于负压状态，蒸发烧瓶在旋转的同时置于水浴锅或油浴锅中恒温加热，加热温度可接近该溶剂的沸点，使得瓶内溶液在负压下进行加热扩散而蒸发，实现溶剂的快速蒸发。
但是，现有的旋转蒸发仪自动化程度低，时时离不开实验人员，每一步骤均需实验人员手动操作，并且在使用过程中无法将馏分、浓缩液自动取出，出料时必须中断旋转蒸馏的运行、通大气、关真空泵，升高蒸馏瓶才能取下蒸馏瓶进行清理，以3L蒸馏瓶为例，一次蒸馏约220mL溶液需要约18分钟，但实际一整套旋转蒸发蒸馏操作的完成约需60分钟。这不仅使得需要连续蒸馏的工作无法自动、高效地进行，而且增加了运行维护的工作量，降低了工作效率，影响工作的进度。另外，与蒸馏瓶连接的玻璃法兰及蒸馏瓶口部在多次的蒸馏瓶安装、卸下过程中很容易破裂。
如中国专利CN203447781U公开了一种可自动进出料的旋转蒸发仪，该旋转蒸发仪通过在冷凝器和接收瓶之间设置四通管，并将四通管的其中一侧出口与进料管相连接，实现了待蒸发料液的自动进料；待蒸发结束后，又可以通过进料管将浓缩液吸出，省去了卸下蒸发瓶倒出浓缩液 的繁复操作。该装置虽然实现了旋转蒸发仪的手动指令下的进料和出料，但其进、出料共用一管对进料或出料存在一定程度的污染，并且无法实现自动控制下的连续进出料及清洗操作。工作过程中依然需要等待一次蒸发结束后手动出料及人工清洗，无法实现蒸馏过程中的连续进料、出料及清洗。
发明内容
本发明提供了一种有多种模式可选择、有计算机或触摸屏等智能电子设备可自动控制进出料、清洗及排馏分、可自动连续重复某一模式整套操作步骤的旋转蒸发仪，解决了现有技术中旋转蒸发仪自动化程度低、不能连续进出料、清洗及排馏分的问题，即实现旋转蒸发仪的智能化，解决了旋转蒸发过程离不开实验人员的问题。
为实现上述目的，本发明提出了一种可自动进出料的旋转蒸发仪，包括支架，所述支架上固定有可拆卸的蒸馏瓶和冷凝器，所述冷凝器底部连接有接收瓶，所述冷凝器内成型有通气通道，所述通气通道与所述蒸馏瓶相连通，并在所述冷凝器的侧壁处形成通气管，所述通气管的通大气口处设置有通气阀用于控制所述蒸馏系统内部与大气的连通；
所述通气通道内还设置有进料通道和出料通道，所述进料通道和出料通道分别与成型于所述通气管处的进料口和出料口相连通，并通过进料阀和出料阀进行控制；
所述进料口和所述出料口分别连接有动力装置，实现自动进出料。
所述进料口和所述出料口分别连接有进料管和出料管，所述进料管和出料管伸入所述蒸馏瓶内。
所述出料管伸入所述蒸馏瓶的端部设置有加重圈。
所述通气通道内还设置有清洗通道，所述清洗通道与成型于所述通气管处的清洗口相连通，并通过清洗阀进行控制。
所述清洗口连接有清洗管，所述清洗管伸入所述蒸馏瓶内；所述清洗口连接有动力装置，实现自动进液清洗。
所述通气通道内还设置有排液通道，所述排液通道与成型于所述通气管处的排液口相连通，并通过排液阀进行控制。
所述排液口连接有排液管，所述排液管伸入所述蒸馏瓶内；所述排液口连接有动力装置，实现清洗液的自动排出。
所述排液管伸入所述蒸馏瓶的端部设置有加重圈。
所述通气通道内还设置有馏分排出通道，所述馏分排出通道与成型于所述通气管处的馏分排出口相连通，并通过馏分排出阀进行控制。
所述馏分排出口连接有馏分排出管，所述馏分排出管伸入所述收集瓶内最低液面处；所述馏分排出口连接有动力装置，实现馏分的自动排出。
所述馏分排出管伸入所述收集瓶的端部设置有加重圈。
所述进料管、出料管、清洗管、排液管和排馏分管为聚四氟乙烯管；
所述进料阀、出料阀、清洗阀、排液阀和排馏分阀为聚四氟乙烯阀或玻璃阀。
所述通气管为与所述冷凝器一体成型的具有多出口的多通管，或者，所述通气管为与所述冷凝器可拆卸玻璃磨口密闭连接的多通管。
所述通大气口、所述进料口、所述出料口、所述清洗口、所述排液口、所述馏分排出口和所述冷凝器壁上的真空管口处连接有自动控制组件。
本发明所述的可自动进出料的旋转蒸发仪，以现有旋转蒸发仪的结构为基础进行创造性改进，将以往通大气、进料共用的通道，通过增设进料通道、出料通道、清洗通道、排液通道、排馏分通道的方式，并各自利用蠕动泵予以控制，或者利用计算机自动控制，即可实现自动进料和出料、自动清洗和排清洗液、自动排馏分，避免了繁复人工操作，有效减少了工作量，使得蒸馏过程可以自动、连续、高效的运行，大大减少了运行维护的工作量。
本发明所述旋转蒸发仪还设置有与各进出口端连接的自动控制组件，并可设置多种工作模式，可通过设定次数自动多次重复某一种模式的工作，解决了实验人员时时离不开蒸馏操作和大量重复某一套操作的问题。
本发明所述旋转蒸发仪，由于采用了自动控制系统实现了自动进出料、自动清洗、排液和排馏分，使得整个旋转蒸发仪可以不使用自动升降组件及其控制组件，有效减少了升降电机及液压顶杆等组件，还减少了因自动升降组件维护而导致的高成本，有效确保了旋转蒸发仪的连续高效工作。
附图说明
图1为本发明所述旋转蒸发仪的第一种结构示意图；
图2为本发明所述旋转蒸发仪的第二种结构示意图；
图3为本发明所述旋转蒸发仪的第三种结构示意图；
图4为本发明所述旋转蒸发仪的第四种结构示意图；
图5为本发明所述自动控制组件结构示意图；
图中标记为：1-支架，2-蒸馏瓶，3-冷凝器，4-接收瓶，5-通气通道，6-通气管，7-通气阀，8-进料通道，9-出料通道，10-进料口，11-出料口，12-进料阀，13-出料阀，14-进料管，15-出料管，16-加重圈，17-清洗通道，18-清洗口，19-清洗阀，20-清洗管，21-排液通道，22-排液口，23-排液阀，24-排液管，25-旋转电机，26-馏分排出通道，27-馏分排出管，28-馏分排出口，29-馏分排出阀，30-通大气口。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合附图和具体实施方式对本发明作进一步详细的说明。
如图1所示的结构，本发明所述旋转蒸发仪，包括支架1，以及用于控制所述旋转蒸发仪旋转的旋转电机25(本发明旋转蒸发仪还可设有控制所述旋转电机参数转速的控制面板，图中未示出)。所述支架1上固定有可拆卸的蒸馏瓶2和冷凝器3，所述蒸馏瓶2和冷凝器3相连通实现液体的蒸馏，且所述冷凝器底部连接有接收瓶4，用于接收蒸发的溶剂。所述接收瓶4底部可以设置有排出馏分的通道及控制通道的开关(图中未示出)。所述冷凝器3内成型有通气通道5，所述通气通道5与所述蒸馏瓶2相连通，用于实现所述蒸馏系统内部与大气连通，所述通气通道5穿过所述冷凝器3的内部并在所述冷凝器3的侧壁处形成通气管6，所述 通气管6在其端部位置的通大气口30处设置有通气阀7，用于控制所述通大气口30的开闭，以控制所述蒸馏系统内部与大气的连通。
作为可以变换的结构，本发明所述的通气管6可以是与所述冷凝器3一体成型的具有多出口的多通管，或者，所述通气管6也可为与所述冷凝器3可拆卸密闭连通(如玻璃磨口密封)的多通管。
如图1所示的结构，所述通气通道5内还设置有用于输入待浓缩液的进料通道8和用于输出浓缩液的出料通道9，所述通气管6为四通管，所述进料通道8和出料通道9分别与成型于所述通气管6侧壁处的进料口10和出料口11相连通，并通过设置于所述进料口10处的进料阀12和设置于所述出料口11处的出料阀13进行开关控制。同时，所述进料口10和所述出料口11处还分别连接有动力装置，可控制液体的送入和抽出，进而实现自动进出料，所述动力装置可以为蠕动泵或者真空泵通过给蒸馏系统内抽真空的方式实现。所述通气通道5内部与所述进料通道8和所述出料通道9之间的空间即为大气连通空间，通过所述通气阀7控制开关即可。
如图1所示的结构，所述进料口10和出料口11还分别连接有进料管14和出料管15，所述进料管14和出料管15均伸入所述蒸馏瓶2内，为了实现更好的出料控制，所述出料管15伸入所述蒸馏瓶2的端部处还设置有加重圈16，使得所述出料管15能够常处于所述蒸馏瓶2的最低液面位置，尽可能的将浓缩液排出，所述加重圈16优选为聚四氟乙烯材料制得的加重圈。
为了更好的适应不同浓缩液的进出料，本发明所述进料管14和出料管15为聚四氟乙烯管，以及所述进料阀12和出料阀13也设计为聚四氟乙烯阀或玻璃阀。
作为可以变换的结构，如图2所示，所述通气管6为五通管结构，所述通气通道5内还设置有用于输入待浓缩液的进料通道8、用于输出浓缩液的出料通道9，以及用于输入清洗液(如蒸馏水或乙醇等)的清洗通道17。所述进料通道8、出料通道9和清洗通道17分别与成型于所述通气管6侧壁处的进料口10、出料口11和清洗口18相连通，并通过设置 于所述进料口10处的进料阀12、设置于所述出料口11处的出料阀13以及设置于所述清洗口18处的清洗阀19进行开关控制。同时，所述进料口10、所述出料口11和所述清洗口18处还分别连接有蠕动泵或通过真空泵给蒸馏系统内抽真空的方式等，可控制液体的送入和抽出，进而实现自动进出料和自动清洗。所述通气通道5内部与所述进料通道8、所述出料通道9和所述清洗通道17之间的空间即为大气连通空间，通过所述通气阀7控制开关即可。
如图2所示的结构，所述进料通道8、出料通道9和清洗通道17还分别连接有进料管14、出料管15和清洗管20，所述进料管14、出料管15和清洗管20均伸入所述蒸馏瓶2内。为了实现更好的出料控制，所述出料管15伸入所述蒸馏瓶2的端部处还设置有加重圈16，使得所述出料管15端部能够常处于所述蒸馏瓶2的最低液面位置，尽可能的将浓缩液排出，所述加重圈16优选为聚四氟乙烯材料制得的加重圈。
为了更好的适应不同浓缩液的进出料，本发明所述进料管14、出料管15和清洗管20为聚四氟乙烯管，以及所述进料阀12、出料阀13和清洗阀19也设计为聚四氟乙烯阀或玻璃阀。
作为可以变换的结构，如图3所示，所述通气管6为六通管结构，所述通气通道5内还设置有用于输入待浓缩液的进料通道8、用于输出浓缩液的出料通道9、用于输入清洗液(如蒸馏水或乙醇等)的清洗通道17，以及用于排出清洗液的排液通道21。所述进料通道8、出料通道9、清洗通道17和排液通道21分别与成型于所述通气管6侧壁处的进料口10、出料口11、清洗口18和排液口22相连通，并通过设置于所述进料口10处的进料阀12、设置于所述出料口11处的出料阀13、设置于所述清洗口18处的清洗阀19、以及设置于所述排液口22处的排液阀23进行开关控制。同时，所述进料口10、所述出料口11、所述清洗口18和所述排液口22处还分别连接有蠕动泵或通过真空泵等动力装置，可控制液体的送入和抽出，进而实现自动进出料及自动清洗。所述通气通道5内部与所述进料通道8、所述出料通道9、所述清洗通道17和所述排液通道21之间的空间即为大气连通空间，通过所述通气阀7控制开关即可连 通或阻断大气。
如图3所示的结构，所述进料口10、出料口11、清洗口18和排液口22还分别连接有进料管14、出料管15、清洗管20和排液管24，所述进料管14、出料管15、清洗管20和排液管24均伸入所述蒸馏瓶2内。为了实现更好的出料控制，所述出料管15和排液管24伸入所述蒸馏瓶2的端部处还分别设置有加重圈16，使得所述出料管15和排液管24能够常处于所述蒸馏瓶2的最低液面位置，尽可能的将浓缩液和清洗液排出，所述加重圈16优选为聚四氟乙烯材料制得的加重圈。
为了更好的适应不同浓缩液的进出料，本发明所述进料管14、出料管15、清洗管20和排液管24为聚四氟乙烯管，以及所述进料阀12、出料阀13、清洗阀19和排液阀23也设计为聚四氟乙烯阀或者玻璃阀。
如果需要接收瓶4也可如蒸馏瓶2设置清洗和排清洗液的组件。
作为可以变换的结构，如图4所示的旋转蒸发仪，所述通气管6为七通管结构，即在图3所示旋转蒸发仪结构的基础上，所述通气通道5内还设置有用于输出馏分的馏分排出通道26，所述馏分排出通道26与成型于所述通气管6侧壁处的馏分排出口28相连通，并通过设置于所述馏分排出口28处的馏分排出阀29进行开关控制，所述馏分排出口28连接有馏分排出管27实现馏分的排出。所述馏分排出管27的另一端伸入所述收集瓶4底部并设置有加重圈16。同时，所述馏分排出口28处还连接有蠕动泵或通过真空泵等动力装置，可控制液体的抽出，进而实现自动抽出馏分。
作为可以变换的结构，本发明所述旋转蒸发仪中，所述收集瓶4还可以为现有技术中一般的带有下端放液口的结构，所述放液口可以通过阀门控制，所述放液口处还可以连接如蠕动泵或通过真空泵等动力装置，实现馏分的直接排出。
作为可以变换的结构，本发明所述旋转蒸发仪中，所述通大气口30、进料口10、出料口11、清洗口18、排液口22、馏分排出口28和冷凝器壁上真空管口处连接有自动控制组件，实现整个旋转蒸发仪的自动控制。
如图5所示的控制组件结构，其接口端L1与所述进料口10连接， 并通过电磁阀K1及微调阀N进行控制，并与进料罐P1通过管子相连接，所述微调阀N可以取代进料阀12对进料过程进行控制，进料罐P1下设置有电子秤B以控制准确进料，电子秤B具备通讯功能，可与计算机通信联系。
所述控制组件中，接口端L2与所述清洗口18连接，并通过电磁阀K2、球阀V2进行控制，并与清洗液罐P2通过管子相连接，所述球阀V2可以取代清洗液阀19进行控制，所述清洗液罐P2下有电子秤B控制准确进清洗液的量。
所述控制组件中，其接口端L3与所述通气管6的所述通大气口30通过管子相连接，并通过电磁阀K3、球阀V3进行控制，所述球阀V3可以取代所述通气阀7。
所述控制组件中，其接口端L4与所述排液口22相连接，并通过电磁阀K4及球阀V4-1进行控制，并与废洗液罐P4通过管子相连接，球阀V4-1可以取代所述排液阀23，废洗液罐P4下设有排液口，上有放空口，分别通过球阀V4-2和V4-3进行控制。所述废洗液罐P4通过管子与真空泵D相连(并连接有压力表M和过滤器F)，利用抽真空排出废洗液。
所述控制组件中，其接口端L5与所述出料口11相连接，并通过电磁阀K5及球阀V5-1进行控制，并与提浓缩液罐P5通过管子相连接，所述球阀V5-1可以取代出料阀13，提浓缩液罐P5下设有排液口，上设有放空口，分别通过球阀V5-2和V5-3进行控制。提浓缩液罐P5通过管子与真空泵D相连(并连接有压力表M和过滤器F)，利用抽真空排出蒸馏浓缩液。
所述控制组件中，其接口端L6与所述馏分排出口28相连接，并通过电磁阀K6及球阀V6-1进行控制，并与馏分收集罐P6通过管子相连接，所述球阀V6-1可以取代馏分排出阀29，馏分收集罐P6下设有排液口，上设有放空口，分别通过球阀V6-2和V6-3进行控制。馏分收集罐P6通过管子与真空泵D相连(并连接有压力表M和过滤器F)，利用抽真空排出馏分。
所述控制组件中，其接口端L7与冷凝器壁上抽真空口通过管子相连 接，并与电磁阀K7及球阀V7及真空泵D相连(并连接有压力表M和过滤器F)。
所述控制组件中，所有电磁阀均由计算机控制开和关，计算机还控制具备通讯功能的电子秤、电机、真空泵、加热锅的温控及时间。在计算机中设定多种工作模式，由计算机控制旋转蒸发仪按照设定的某一模式进行每一步操作。
例如，在全流程工作模式下，该模式完全由计算机控制执行，具体操作步骤包括：
(1)开加热按钮(具备通讯功能)，同时关闭电磁阀K3，打开K1、K7，按预设进料量准确进料(电子秤控制，具备通讯功能)，进料完成后K1关闭；
(2)开电机(具备通讯功能)控制蒸馏瓶旋转蒸发(转速、时间控制)，完成后关电机；
(3)停止加热，并打开电磁阀K3、K5，排空蒸馏瓶中浓缩液(时间控制)，完成后K5关闭；
(4)打开电磁阀K6，排空馏分(时间控制)，完成后K6、K3关闭；
(5)打开电磁阀K2及电机，进清洗液(电子秤控制)，控制蒸馏瓶旋转(时间控制)，完成后K2及电机关闭，并打开K3、K4，排空清洗液(时间控制)，完成后将K4、K3关闭；重复步骤(5)中操作3次，至认为清洗干净，关闭K7及整个系统；并按预设周期，重复执行上述步骤(1)-(5)。
例如，在无清洗流程的工作模式下，该模式完全由计算机控制执行，具体操作步骤包括：
(1)打开加热按钮(具备通讯功能)，关闭电磁阀K3，打开K1、K7，按预设进料量准确进料(电子秤控制，具备通讯功能)，进料完成后K1关闭；
(2)开电机(具备通讯功能)，控制蒸馏瓶旋转蒸发(转速、时间控制)，完成后关电机；
(3)停止加热，打开电磁阀K3、K5，排空蒸馏瓶中浓缩液(时间 控制)，完成后K5关闭；
(4)打开电磁阀K6，排空馏分(时间控制)，完成后K6、K7关闭，并按预设周期，重复执行(1)-(4)。
例如，在加料流程的工作模式下，该模式完全由计算机控制执行，具体操作步骤包括：
(1)关闭电磁阀K3，打开电磁阀K1、K7，按预设进料量进料(电子秤控制)，进料完成后K1关闭；
(2)打开电磁阀K3，关闭K7，并按预设周期，重复执行上述步骤(1)-(2)。
例如，在清洗流程的工作模式下，该模式完全由计算机控制执行，具体操作步骤包括：
(1)关闭电磁阀K3，开K2、K7及电机，同时进清洗液(电子秤控制)，待蒸馏瓶旋转(转速、时间控制)，完成后K2关闭；
(2)电机关闭，蒸馏瓶停止旋转，开K3、K4，排空清洗液(时间控制)，完成后开K4，K7关闭，并按预设周期，重复执行步骤(1)-(2)。
例如，在排浓缩液流程的工作模式下，该模式完全由计算机控制执行，具体操作步骤包括：
(1)电磁阀K3保持开状态，开K5、K7，排空蒸馏瓶中浓缩液(时间控制)，完成后K5关闭；
(2)关K7，按预设周期，重复执行步骤(1)-(2)。
例如，在排馏分流程的工作模式下，该模式完全由计算机控制执行，具体操作步骤包括：
(1)电磁阀K3保持开状态，开电磁阀K6、K7，排空收集瓶中馏分(时间控制)，完成后K6关闭；
(2)关电磁阀K7，按预设周期，重复执行步骤(1)-(2)。
以上对本发明实施例进行了详细介绍，本文中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处，综上 所述，本说明书内容不应理解为对本发明的限制。

Claims (10)

  1. 一种可自动控制连续进出料的旋转蒸发仪，其特征在于，包括支架(1)，所述支架(1)上固定有可拆卸的蒸馏瓶(2)和冷凝器(3)，所述冷凝器底部连接有接收瓶(4)，所述冷凝器(3)内成型有通气通道(5)，所述通气通道(5)与所述蒸馏瓶(2)相连通，并在所述冷凝器(3)的侧壁处形成通气管(6)，所述通气管(6)的通大气口(30)处设置有通气阀(7)用于控制蒸馏系统内部与大气的连通；
    所述通气通道(5)内还设置有进料通道(8)和出料通道(9)，所述进料通道(8)和出料通道(9)分别与成型于所述通气管(6)处的进料口(10)和出料口(11)相连通，并通过进料阀(12)和出料阀(13)进行控制；
    所述进料口(10)和所述出料口(11)分别连接有动力装置，实现自动进出料。
  2. 根据权利要求1所述的可自动控制连续进出料的旋转蒸发仪，其特征在于，所述进料口(10)和所述出料口(11)分别连接有进料管(14)和出料管(15)，所述进料管(14)和出料管(15)伸入所述蒸馏瓶(2)内。
  3. 根据权利要求1或2所述的可自动控制连续进出料的旋转蒸发仪，其特征在于，所述通气通道(5)内还设置有清洗通道(17)，所述清洗通道(17)与成型于所述通气管(6)处的清洗口(18)相连通，并通过清洗阀(19)进行控制。
  4. 根据权利要求3所述的可自动控制连续进出料的旋转蒸发仪，其特征在于，所述清洗通道(17)连接有清洗管(20)，所述清洗管(20)伸入所述蒸馏瓶(2)内；所述清洗口(18)连接有动力装置，实现自动进液清洗。
  5. 根据权利要求1-4任一项所述的可自动控制连续进出料的旋转蒸发仪，其特征在于，所述通气通道(5)内还设置有排液通道(21)，所述排液通道(21)与成型于所述通气管(6)处的排液口(22)相连通，并通过排液阀(23)进行控制。
  6. 根据权利要求5所述的可自动控制连续进出料的旋转蒸发仪，其特征在于，所述排液通道(21)连接有排液管(24)，所述排液管(24)伸入所述蒸馏瓶(2)内；所述排液口(22)连接有动力装置，实现清洗液的自动排出。
  7. 根据权利要求1-6任一项所述的可自动控制连续进出料的旋转蒸发仪，其特征在于，所述通气通道(5)内还设置有馏分排出通道(26)，所述馏分排出通道(26)与成型于所述通气管(6)处的馏分排出口(28)相连通，并通过馏分排出阀(29)进行控制。
  8. 根据权利要求7所述的可自动控制连续进出料的旋转蒸发仪，其特征在于：所述馏分排出通道(26)连接有馏分排出管(27)，所述馏分排出管(27)伸入所述收集瓶(4)内最低液面处；所述馏分排出口(28)连接有动力装置，实现馏分的自动排出。
  9. 根据权利要求1-8任一项所述的可自动控制连续进出料的旋转蒸发仪，其特征在于，所述通气管(6)为与所述冷凝器(3)一体成型的 具有多出口的多通管，或者，所述通气管(6)为与所述冷凝器(3)可拆卸玻璃磨口密封连接的多通管。
  10. 根据权利要求1-8任一项所述的可自动控制连续进出料的旋转蒸发仪，其特征在于，所述通大气口(30)、所述进料口(10)、所述出料口(11)、所述清洗口(18)、所述排液口(22)、所述馏分排出口(28)和所述冷凝器壁上的真空管口处连接有自动控制组件，所述自动控制组件通过计算机或触摸屏发出的指令可在多种预先设定的工作模式下完成蒸馏过程及清洗过程中的各项工作。
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