Reduced pressure distillation device

Abstract

The utility model relates to a reduced pressure distillation device, which is used for distilling and purifying complex organic materials, particularly OLED (organic light emitting diode) materials, and comprises a solvent adsorption system and a pump system which are connected through a main pipeline, the pump system comprises a first vacuum pump (1), a second vacuum pump (2) and a molecular pump (3) which are respectively communicated with the main pipeline, and opening and closing between the main pipeline and the first vacuum pump (1), between the main pipeline and the second vacuum pump (2) and between the main pipeline and the molecular pump (3) are independently controlled through valves; the second vacuum pump (2) and the molecular pump (3) are communicated and controlled to be opened and closed through a valve.

Description

Technical Field

[0001] The utility model relates to organic material purification equipment, in particular to a vacuum distillation device. Background Art

[0002] Distillation purification is one of the widely used raw material purification methods in the industrial production of organic material purification. It has many advantages, such as simple equipment, easy manufacturing, large processing capacity, convenient operation, avoiding the introduction of any reagents, and separation accuracy up to ppb level. The distillation tower has a high separation efficiency for fractions with different boiling points, but the fraction span of OLED materials is large, and the existing OLED material separation equipment such as high vacuum sublimation furnace has poor universality and is difficult to meet the needs of purification production of various types of materials. Utility Model Content

[0003] In view of the above-mentioned deficiencies of the existing distillation and purification equipment, the utility model provides a vacuum distillation device.

[0004] The technical solution of the utility model is achieved by the following method: providing a vacuum distillation device, characterized in that it comprises a solvent adsorption system and a pump system connected by a main pipeline;

[0005] The solvent adsorption system includes at least one of a condensation unit for condensing a solvent, an alkaline drying unit filled with an alkaline desiccant, and an acidic drying unit filled with an acidic desiccant;

[0006] The pump system includes a first vacuum pump, a second vacuum pump, and a molecular pump respectively connected to the main pipeline. The opening and closing of the main pipeline and the first vacuum pump, the second vacuum pump, and the molecular pump are independently controlled by valves; the second vacuum pump is connected to the molecular pump and the opening and closing are controlled by a valve.

[0007] In one embodiment of the present invention, the vacuum degree provided by the first vacuum pump is less than the vacuum degree provided by the second vacuum pump.

[0008] In one embodiment of the present invention, the first vacuum pump is a water pump or a vacuum diaphragm pump, and the second vacuum pump is a mechanical pump.

[0009] In one embodiment of the present invention, the pump system further includes: a first vacuum controller used in conjunction with the first vacuum pump, and a second vacuum controller used in conjunction with the second vacuum pump.

[0010] In one embodiment of the present invention, it also includes an external interface for connecting to a gas source.

[0011] In one embodiment of the utility model, a valve and a third vacuum controller are provided on the external interface.

[0012] In one embodiment of the utility model, a protective gas inlet is provided on the external interface, and the opening and closing of the protective gas inlet is controlled by a valve.

[0013] In one embodiment of the present invention, it further comprises a shell, wherein the solvent adsorption system and the pump system are arranged in the shell.

[0014] In one embodiment of the present invention, the solvent adsorption system comprises a condensation unit, an alkaline drying unit and an acidic drying unit which are connected in sequence, and the condensation unit, the alkaline drying unit and the acidic drying unit are all detachably connected.

[0015] In one embodiment of the present invention, a spherical tube furnace for sublimating fractions is further included, wherein the spherical tube furnace includes at least two spherical tubes connected in series and at least two temperature zones with different temperatures.

[0016] The beneficial effects are as follows: the three-stage pump system is integrated into one device, different parts are started for different fractions, and the universality of miniaturized equipment is achieved. It is particularly suitable for the distillation purification of OLED materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 The utility model is a schematic diagram of the structure of the vacuum distillation device.

[0018] Figure 2 It is a schematic diagram of the structure of a spherical tube furnace in an embodiment of the utility model. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical solution and advantages of the utility model clearer, the technical solution of the utility model will be clearly and completely described below in combination with the specific embodiments of the utility model and the corresponding drawings. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0020] The utility model is further described in detail below with reference to the accompanying drawings and embodiments.

[0021] The vacuum distillation device provided by the utility model comprises a solvent adsorption system and a pump system, and the solvent adsorption system and the pump system are connected through a main pipeline. The structure of the vacuum distillation device in this embodiment is as follows Figure 1 shown.

[0022] The pump system is the core component of the vacuum distillation unit. By adjusting the opening and closing of valves and the start-up of specific units, the adjustment of different working conditions can be achieved. The solvent adsorption system prevents the solvent from entering the core to prevent damage to the pump system.

[0023] The solvent adsorption system includes at least one of a condensation unit 11, an alkaline drying unit 12 and an acidic drying unit 13; the condensation unit 11 is used to condense the solvent, the alkaline drying unit 12 is filled with an alkaline desiccant, and the acidic drying unit 13 is filled with an acidic desiccant. These three units can work individually or simultaneously, depending on the type of gas source.

[0024] The pump system includes a first vacuum pump 1, a second vacuum pump 2, and a molecular pump 3. The first vacuum pump 1, the second vacuum pump 2, and the molecular pump 3 are respectively connected to the main pipeline and are independently controlled to open and close by setting valves. In addition, the second vacuum pump 2 is connected to the molecular pump 3 and is controlled to open and close by a valve.

[0025] In one embodiment of the present invention, the pump system has three working modes: 1. the first vacuum pump 1 , 2. the second vacuum pump 2 , 3. the second vacuum pump 2 + the molecular pump 3 .

[0026] The solvent adsorption system has three components: a condensation unit 11, an alkaline drying unit 12 and an acidic drying unit 13, which are used to condense common solvents, acidic and alkaline solvents or gases respectively.

[0027] 7, 8, 9, 10, 15 and 16 are two-way valve switches. Arrows 4, 5, 6, 14, 17 and 20 are air flow directions.

[0028] Three working modes of the pump system, usage process and instructions:

[0029] First, turn off the second vacuum pump 2 and the molecular pump 3, turn off the two-way valve switches 8, 9, 10 and the N2 switch 16, turn on the first vacuum pump 1 and the valve 7 and the external main valve 15, and use the first vacuum pump 1 to distill the low-boiling point solvent; preferably, a first vacuum controller used in conjunction with the first vacuum pump 1 can be provided here, which can display the vacuum degree and adjust the vacuum as needed. Rotary evaporators such as BUCHI and Tokyo Rika have similar controllers; in this state, the first vacuum pump 1 works alone;

[0030] Then, close the valve switch 7 and the first vacuum pump 1, open the second vacuum pump 2 and valve 8, and use the second vacuum pump 2 to vacuum distill the medium-boiling-point solvent or product; preferably, a second vacuum controller used in conjunction with the second vacuum pump 2 can be provided here, which can display the vacuum degree and adjust the vacuum as needed. Work until no more samples appear, in which case the second vacuum pump 2 works alone; since the boiling point of the fraction is high in this state, the vacuum degree needs to be higher, and the vacuum degree provided by the second vacuum pump 2 is greater than the vacuum degree provided by the first vacuum pump 1. For example, the first vacuum pump 1 is a water pump or a vacuum diaphragm pump, and the second vacuum pump 2 is a mechanical pump.

[0031] Finally, close valve 8, open valve 9, start molecular pump 3, open valve 10, and use the second vacuum pump 2 and molecular pump 3 system to distill and purify the high-boiling point solvent or product (preferably, equipped with a vacuum gauge). After the distillation and purification is completed, close valves 15 and 10, turn off the molecular pump 3 switch, and turn off valve 9 and the second vacuum pump 2. Open valve 16 and fill the external system with nitrogen to relieve pressure. In this state, the second vacuum pump 2 + molecular pump 3 work together.

[0032] In one embodiment of the present invention, the vacuum distillation apparatus further comprises a housing 21, wherein the solvent adsorption system and the pump system are arranged in the housing 21. The three-stage pump system is integrated into one device, and different parts are started for different fractions.

[0033] In one embodiment of the utility model, the vacuum distillation apparatus further comprises an external interface for connecting to a gas source 2019. Preferably, the external interface is arranged on the housing 21 to form an independent system adapted to various gas sources 20. The external interface may be provided with a valve 15 and a third vacuum controller 18. The external interface is provided with a protective gas inlet 17, and the opening and closing of the protective gas inlet 17 is controlled by a valve 16.

[0034] In one embodiment of the utility model, the solvent adsorption system comprises a condensation unit 11, an alkaline drying unit 12 and an acidic drying unit 13 connected in sequence, and the condensation unit 11, the alkaline drying unit 12 and the acidic drying unit 13 are all detachably connected. The desiccant in the alkaline drying unit 12 and the acidic drying unit 13 can be replaced frequently. The alkaline drying unit 12 and the acidic drying unit 13 are partially optional and are not essential accessories.

[0035] In the present invention, if the second vacuum pump 2 is a mechanical pump, the mechanical pump needs to be frequently changed in oil, and it is best to be able to move within a certain range. If the first vacuum pump 1 is a water pump, it needs to be connected to an external water source to facilitate water replacement. The pipeline of the entire pump system must ensure that the vacuum degree finally connected can reach the maximum, and the thickness of the pipeline and the interface must be carefully considered to prevent the loss of vacuum degree.

[0036] In one embodiment of the present invention, the vacuum distillation apparatus further comprises a gas source 20, wherein the gas source 20 is a spherical tube furnace for subliming the fraction. The structure of the spherical tube furnace in this embodiment is as follows: Figure 2 The spherical tube furnace includes at least two spherical tubes 22 connected in series and at least two temperature zones with different temperatures.

[0037] The spherical tube 22 is convenient for receiving liquid, and the joints are detachable, and at the same time, the airtightness must be ensured to prevent liquid leakage from the connection; the spherical tube is fixed to the rotating fitting, which is used to fix at least two spherical tubes 22 in series, and has a rotating function to ensure that the purified sample is heated evenly. The design here can refer to the similar function of the rotary evaporator, but the material needs to be resistant to high temperature.

[0038] The heating system 24 realizes one-time separation of the mixture by setting different temperature zones.

[0039] The tube furnace is designed with an adjustable tilt angle to ensure that the liquid material does not easily flow out.

[0040] When connecting the vacuum pump system, all volatiles must be absorbed before connecting the pump to prevent them from entering the pump system and damaging the pump.

[0041] Preferably, the spherical tube furnace further includes a quartz outer tube 23; at least two spherical tubes 22 connected in series are located inside the quartz outer tube 23 to ensure the vacuum degree of the system.

[0042] The structures listed above are only partial representatives, and other spherical tube 22 settings, sealing settings, and pressure relief system settings with the same concept are all within the protection scope of this utility model.

[0043] Although the embodiments of the present invention have been shown and described above, it can be understood that the above embodiments are exemplary and cannot be understood as limitations of the present invention. Ordinary technicians in the field can change, modify, replace and modify the above embodiments within the scope of the present invention.

Claims

1. A vacuum distillation apparatus, characterized in that: It includes a solvent adsorption system and a pump system connected through a main pipeline; The solvent adsorption system comprises at least one of a condensation unit (11) for condensing a solvent, an alkaline drying unit (12) filled with an alkaline drying agent, and an acidic drying unit (13) filled with an acidic drying agent; The pump system comprises a first vacuum pump (1), a second vacuum pump (2), and a molecular pump (3) respectively connected to the main pipeline; the opening and closing between the main pipeline and the first vacuum pump (1), the second vacuum pump (2), and the molecular pump (3) are independently controlled by valves; the second vacuum pump (2) is connected to the molecular pump (3) and the opening and closing are controlled by the valve.

2. The vacuum distillation apparatus according to claim 1, characterized in that The vacuum degree provided by the first vacuum pump (1) is lower than the vacuum degree provided by the second vacuum pump (2).

3. The vacuum distillation apparatus according to claim 2, characterized in that: The first vacuum pump (1) is a water pump or a vacuum diaphragm pump, and the second vacuum pump (2) is a mechanical pump.

4. The vacuum distillation apparatus according to claim 1, characterized in that: The pump system further comprises: a first vacuum controller for use in conjunction with the first vacuum pump (1), and a second vacuum controller for use in conjunction with the second vacuum pump (2).

5. The vacuum distillation apparatus according to claim 1, characterized in that: It also includes an external interface for connecting to a gas source (19).

6. The vacuum distillation apparatus according to claim 5, characterized in that: The external interface is provided with a valve and a third vacuum controller.

7. The vacuum distillation apparatus according to claim 5, characterized in that: A protective gas inlet (17) is arranged on the external interface, and the opening and closing of the protective gas inlet (17) is controlled by a valve.

8. The vacuum distillation apparatus according to claim 1, characterized in that: It also comprises a housing (21), wherein the solvent adsorption system and the pump system are arranged in the housing (21).

9. The vacuum distillation apparatus according to claim 1, characterized in that: The solvent adsorption system comprises a condensation unit (11), an alkaline drying unit (12) and an acidic drying unit (13) which are connected in sequence, and the condensation unit (11), the alkaline drying unit (12) and the acidic drying unit (13) are all detachably connected.

10. The vacuum distillation apparatus according to claim 1, characterized in that: Also included is a spherical tube furnace for subliming fractions, the spherical tube furnace comprising at least two spherical tubes (22) connected in series and at least two temperature zones with different temperatures.

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