A microwave enhanced liquid-liquid heterogeneous extraction device

Abstract

The application discloses a microwave reinforced liquid-liquid heterogeneous extraction device, which comprises a microwave cavity and an extraction column tube arranged in the microwave cavity. The extraction column tube is divided into three parts from top to bottom, and the three parts are a light phase layering area, a filler area and a heavy phase layering area in sequence. A light phase outlet at the top of the light phase layering area and a heavy phase inlet at the middle of the light phase layering area are respectively connected with a light phase discharge pipe and a heavy phase feeding pipe through pipelines. A light phase inlet is arranged between the filler area and the heavy phase layering area and is connected with the light phase feeding pipe through a pipeline. A heavy phase outlet at the bottom of the heavy phase layering area is connected with a heavy phase discharge pipe through a pipeline. The extraction device utilizes the selective heating characteristics of microwaves, increases the microwave action range of materials by shunting the materials to be separated in the form of a column tube and arranging fillers in the column tube, accelerates the heat and mass transfer between liquid-liquid heterogeneous systems, utilizes the coalescence effect of microwaves on liquid droplets in the liquid-liquid heterogeneous system, reinforces the layering process of the liquid-liquid heterogeneous system and improves the extraction efficiency.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of liquid-liquid heterogeneous extraction, in particular to a microwave-enhanced liquid-liquid heterogeneous extraction device. BACKGROUND

[0002] Extraction is a common separation and purification technique widely used in chemistry, chemical industry, pharmaceutical industry, food industry, environmental science, etc. It separates target substances from mixtures by taking advantage of the difference in solubility of substances in different solvents. Extraction column is a device for realizing multi-stage extraction. Common extraction columns include the following types: packed extraction column, sieve plate extraction column, rotating disc extraction column, pulsating extraction column, etc.

[0003] Traditional extraction columns break the liquid into droplets by external energy (pulsation, stirring, etc.) or by changing the structure (sieve plate, packing, etc.) to achieve sufficient contact between the two phases and improve separation efficiency. However, for low interfacial tension extraction systems, the introduction of strong drag force pulsing energy or strong shear force stirring energy can easily cause over-pulverization of dispersed phase droplets or even emulsification (CN118389825A); packing plays an important role in the extraction process, but in the case of small density difference between the two phases and large viscosity of the continuous phase, the axial backmixing in the packed extraction column is very serious, especially the axial backmixing of the continuous phase, which not only restricts the production capacity of the extraction column, but also seriously affects the separation efficiency of the extraction column (CN102698465A). SUMMARY

[0004] In view of the above technical problems existing in the prior art, the purpose of the present application is to provide a microwave-enhanced liquid-liquid heterogeneous extraction device. The device shortens the settling time between liquid-liquid heterogeneous phases, enhances the mass transfer efficiency, and improves the extraction efficiency through the high efficiency energy transmission of the microwave field.

[0005] The technical solution adopted by the present application is as follows:

[0006] A microwave-enhanced liquid-liquid heterogeneous extraction device, comprising a microwave cavity and an extraction column arranged in the microwave cavity, the extraction column being divided into three parts from top to bottom, namely a light phase layering zone, a packing zone and a heavy phase layering zone; the light phase outlet at the top of the light phase layering zone and the heavy phase inlet at the middle thereof are connected by pipelines with a light phase discharge pipe and a heavy phase feed pipe respectively, a light phase inlet is arranged between the packing zone and the heavy phase layering zone and connected by a pipeline with a light phase feed pipe, and the heavy phase outlet at the bottom of the heavy phase layering zone is connected by a pipeline with a heavy phase discharge pipe.

[0007] Further, the material of the packing in the packing zone is ceramic or glass, and the material of the extraction column is quartz.

[0008] Further, the microwave cavity is provided with waveguides and temperature sensors, the number of waveguides is at least two and the waveguides are arranged on opposite sides of the microwave cavity, the waveguides are connected with the microwave generating device, and the microwaves generated by the microwave generating device enter the microwave cavity through the waveguides.

[0009] Further, the radius of the extraction column is not greater than the penetration depth of the microwaves generated by the microwave generating device into the light phase solution or the heavy phase solution in the extraction column.

[0010] Further, the number of extraction columns is at least two, a first intelligent liquid layering instrument for monitoring the state of the light phase after layering is arranged on the upper part of the light phase layering area of the extraction column, a heavy phase shunt pipe is connected to the heavy phase inlet in the middle of the light phase layering area, the heavy phase shunt pipe is combined with the total pipe after penetrating out of the microwave cavity and is connected with the heavy phase feed pipe, a first electromagnetic valve is arranged on the heavy phase shunt pipe, the first electromagnetic valve is signal connected with the first intelligent liquid layering instrument through the PLC control system, the liquid separation state signal monitored by the first intelligent liquid layering instrument is transmitted to the PLC control system, and then the flow rate of the input heavy phase solution is adjusted by adjusting the opening degree of the first electromagnetic valve.

[0011] Further, the number of extraction columns is at least two, a second intelligent liquid layering instrument for monitoring the state of the heavy phase after layering is arranged on the lower part of the heavy phase layering area of the extraction column, a light phase shunt pipe is connected to the light phase inlet on the extraction column, the light phase shunt pipe is combined with the total pipe after penetrating out of the microwave cavity and is connected with the light phase feed pipe, a second electromagnetic valve is arranged on the light phase shunt pipe, the second electromagnetic valve is signal connected with the second intelligent liquid layering instrument through the PLC control system, the liquid separation state signal monitored by the second intelligent liquid layering instrument is transmitted to the PLC control system, and then the flow rate of the input light phase solution is adjusted by adjusting the opening degree of the second electromagnetic valve.

[0012] Further, flow meters and valves are arranged on the light phase outlet pipe, the heavy phase inlet pipe, the light phase inlet pipe and the heavy phase outlet pipe.

[0013] Further, a pipe through hole is arranged on the microwave cavity, so that the corresponding pipe penetrates into the microwave cavity and is connected with the light phase outlet, the heavy phase inlet, the light phase inlet and the heavy phase outlet on the extraction column, respectively.

[0014] Compared with the prior art, the present application has the following beneficial effects:

[0015] The application increases the microwave action volume, increases the heat exchange area, makes the microwave heating more uniform, and improves the heat transfer rate by shunting the material to be separated in the form of a tube; the built-in packing in the tube promotes the liquid droplet breaking, coalescence and re-breaking process of the liquid-liquid heterogeneous system, increases the mass transfer and microwave action area between the liquid-liquid heterogeneous system, and improves the liquid-liquid extraction efficiency; the selective heating characteristics of the microwave are used to strengthen the heating of the liquid with strong polarity in the heterogeneous liquid-liquid system, reduce the viscosity of the liquid droplet, strengthen the coalescence of the liquid droplet, and speed up the settlement and layering of the heterogeneous liquid-liquid system. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 is a structural schematic diagram of a microwave enhanced liquid-liquid heterogeneous extraction device of the application;

[0017] Figure 2 is a structural schematic diagram of a single extraction tube of the application;

[0018] The drawing number: 1-microwave cavity, 2-light phase discharge pipe, 3-extraction tube, 31-light phase layering area, 32-packing area, 33-heavy phase layering area, 34-light phase outlet, 35-heavy phase outlet, 36-light phase inlet, 37-heavy phase inlet, 4-temperature sensor, 5-heavy phase feeding pipe, 61-first intelligent liquid layering instrument, 62-second intelligent liquid layering instrument, 7-light phase feeding pipe, 8-heavy phase discharge pipe, 10-waveguide. DETAILED DESCRIPTION

[0019] The application will be further described below in combination with specific embodiments, but the protection scope of the application is not limited thereto.

[0020] Example: control Figures 1-2

[0021] A microwave enhanced liquid-liquid heterogeneous extraction device, comprising a microwave cavity 1 and an extraction tube 3 arranged in the microwave cavity 1, the extraction tube 3 is divided into three parts from top to bottom, in turn, a light phase layering area 31, a packing area 32 and a heavy phase layering area 33. The light phase outlet 34 at the top of the light phase layering area 31, the heavy phase inlet 37 in the middle are respectively connected by pipelines with the light phase discharge pipe 2 and the heavy phase feeding pipe 5, the light phase inlet 36 is arranged between the packing area 32 and the heavy phase layering area 33 and connected by a pipeline with the light phase feeding pipe 7, and the heavy phase outlet 35 at the bottom of the heavy phase layering area 33 is connected by a pipeline with the heavy phase discharge pipe 8.

[0022] The material of the packing in the packing area 32 is a wave-transparent material such as ceramic or glass, and the material of the extraction tube 3 is quartz.

[0023] Control Figure 1In the microwave cavity 1, waveguides 10 and temperature sensors 4 are arranged, the number of waveguides 10 is at least two and arranged on opposite sides of the microwave cavity 1, the waveguides 10 are connected with microwave generating devices, and the microwaves generated by the microwave generating devices enter the microwave cavity 1 through the waveguides 10.

[0024] Control Figure 1 In the microwave cavity 1, waveguides 10 and temperature sensors 4 are arranged, the number of waveguides 10 is at least two and arranged on opposite sides of the microwave cavity 1, the waveguides 10 are connected with microwave generating devices, and the microwaves generated by the microwave generating devices enter the microwave cavity 1 through the waveguides 10.

[0025] The upper part of the light phase layering area 31 of the extraction column 3 is provided with a first intelligent liquid layering instrument 61 for monitoring the state after light phase layering, the heavy phase inlet 37 in the middle part of the light phase layering area 31 is connected with a heavy phase shunt pipe, the heavy phase shunt pipe is combined in the main pipe after penetrating out of the microwave cavity 1 and connected with the heavy phase feed pipe 5, a first electromagnetic valve is arranged on the heavy phase shunt pipe, and the first electromagnetic valve is signal connected with the first intelligent liquid layering instrument 61 through the PLC control system, the liquid separation state signal monitored by the first intelligent liquid layering instrument 61 is transmitted to the PLC control system, and then the flow rate of the input heavy phase solution is adjusted by adjusting the opening degree of the first electromagnetic valve.

[0026] The lower part of the heavy phase layering area 33 of the extraction column 3 is provided with a second intelligent liquid layering instrument 62 for monitoring the state after heavy phase layering, the light phase inlet 36 on the extraction column 3 is connected with a light phase shunt pipe, the light phase shunt pipe is combined in the main pipe after penetrating out of the microwave cavity 1 and connected with the light phase feed pipe 7, a second electromagnetic valve is arranged on the light phase shunt pipe, and the second electromagnetic valve is signal connected with the second intelligent liquid layering instrument 62 through the PLC control system, the liquid separation state signal monitored by the second intelligent liquid layering instrument 62 is transmitted to the PLC control system, and then the flow rate of the input light phase solution is adjusted by adjusting the opening degree of the second electromagnetic valve.

[0027] In the present application, the first intelligent liquid layering instrument 61 and the second intelligent liquid layering instrument 62 can all use commercially available intelligent liquid layering instruments, and the detection principle is that the response values of conductivity, capacitance, inductance and impedance are combined into a value of 0-100 for output, the interface detection is realized by using the differences in physical properties of light components and heavy components, and the good and bad of the layering effect of light components and heavy components can be reflected.

[0028] Flow meters and valves are arranged on the light phase discharge pipe 2, the heavy phase feed pipe 5, the light phase feed pipe 7 and the heavy phase discharge pipe 8.

[0029] Control Figure 1In the microwave cavity 1, a pipe through hole is arranged, so that the corresponding pipe is inserted into the microwave cavity 1 and connected with the light phase outlet 34, the heavy phase inlet 37, the light phase inlet 36 and the heavy phase outlet 35 on the extraction column 3 respectively.

[0030] Application Examples

[0031] The microwave enhanced liquid-liquid heterogeneous extraction device as shown in Figure 1 is applied to the process of removing the homogeneous catalyst in the preparation of methyl ricinoleate. Castor oil and methanol are reacted for 1 h under the catalysis of the homogeneous catalyst KOH, and after removing methanol and glycerol, a raw material liquid I is obtained, which mainly contains methyl ricinoleate, glycerol and KOH. The raw material liquid I contains 5% glycerol and 0.03% KOH by mass percentage.

[0032] In order to remove KOH, pure glycerol is used as an extractant to extract KOH in the raw material liquid I, so as to realize efficient removal of KOH in the preparation of methyl ricinoleate and rapid separation of methyl ester and glycerol. The following application examples 1-3 all extract the raw material liquid I.

[0033] Application Example 1

[0034] A glass extraction tube with a radius of 10 cm and a length of 20 cm is placed in the microwave cavity of the microwave enhanced liquid-liquid heterogeneous extraction device. The packing zone of the extraction tube is not placed with any packing. First, the extraction tube is filled with the raw material liquid I, and then the microwave generating device (the microwave frequency is 2450 MHz) is turned on. The microwave generated by the microwave generating device enters the microwave cavity through the waveguide to heat the material in the extraction tube by microwave radiation. The temperature of the liquid in the extraction tube is controlled at 40°C. The raw material liquid I is pumped into the light phase feed pipe 7, and the pure glycerol is pumped into the heavy phase feed pipe 5. The flow rate of the light phase into the extraction tube is 10 ml / min, and the volume flow rate ratio of the light phase and the heavy phase is 10:1. After countercurrent and separation, the raffinate is obtained from the heavy phase outlet pipe 9, and the product is obtained from the light phase outlet pipe 2.

[0035] According to the above method, after running for 20 min, the sample is taken at the light phase outlet pipe 2. After titration analysis, the content of KOH in the product is 0.03%, and the content of glycerol is 5%. After running for 40 min, the second sample is taken. After titration analysis, the content of KOH in the product is 0.01%, and the content of glycerol is 3%. After running for 60 min, the third sample is taken. After analysis, the content of KOH in the product is 0.002%, and the content of glycerol is 2.5%. After running for 80 min, the fourth sample is taken. The content of KOH in the product is 10 ppm, and the content of glycerol is 2%. Subsequent sampling analysis shows that the product content is basically stable.

[0036] Application Example 2

[0037] A glass extraction tube with a radius of 10 cm and a length of 20 cm is placed in the microwave cavity of the microwave-enhanced liquid-liquid heterogeneous extraction device. Ceramic Raschig ring fillers are placed in the filler area of the extraction tube. First, the extraction tube is filled with raw material liquid one, then the microwave generating device (microwave frequency is 2450 MHz) is turned on, and the microwave generated by the microwave generating device enters the microwave cavity through the waveguide to heat the material in the extraction tube. The temperature of the liquid in the extraction tube is controlled at 40°C. The raw material liquid one is pumped into the light phase feed pipe 7, and the pure glycerol is pumped into the heavy phase feed pipe 5. The flow rate of the light phase into the extraction tube is 10 ml / min, and the volume flow rate ratio of the light phase and the heavy phase is 10:1. After countercurrent and stratification, the raffinate is obtained from the heavy phase outlet pipe 9, and the product is obtained from the light phase outlet pipe 2.

[0038] According to the above method, after running for 20 min, sample is taken at the light phase outlet pipe 2, and after titration analysis, the content of KOH in the product is 0.01%, and the content of glycerol is 4.5%; after running for 40 min, the second sample is taken, and after titration analysis, the content of KOH in the product is 0.003%, and the content of glycerol is 3%; after running for 60 min, the third sample is taken, and after analysis, the content of KOH in the product is 8 ppm, and the content of glycerol is 2%; subsequent sampling and analysis show that the product content is basically stable.

[0039] Application Example 3

[0040] Two glass extraction tubes with a radius of 5 cm and a length of 20 cm are placed in the microwave cavity of the microwave-enhanced liquid-liquid heterogeneous extraction device, and the tube diameter is determined according to the penetration depth of 2450 MHz microwave in each material. Ceramic Raschig ring fillers are placed in the filler area of the extraction tube. First, the extraction tube is filled with raw material liquid one, then the microwave generating device (microwave frequency is 2450 MHz) is turned on, and the microwave generated by the microwave generating device enters the microwave cavity through the waveguide to heat the material in the extraction tube. The temperature of the liquid in the extraction tube is controlled at 40°C. The raw material liquid one is pumped into the light phase feed pipe 7 and then divided into two extraction tubes, and the pure glycerol is pumped into the heavy phase feed pipe 5 and then divided into two extraction tubes. The flow rate of the light phase into the two extraction tubes is 5 ml / min, and the volume flow rate ratio of the light phase and the heavy phase is 10:1. After the material is divided into two extraction tubes, countercurrent and stratification are performed, and the raffinate is obtained from the heavy phase outlet pipe 9, and the product is obtained from the light phase outlet pipe 2.

[0041] According to the above method, sampling is performed at the light phase discharge pipe 2 after 20 minutes of operation, and after titration analysis, the content of KOH in the product is 0.003%, and the content of glycerol is 3%; sampling is performed for the second time after 40 minutes of operation, and after titration analysis, the content of KOH in the product is 0.001%, and the content of glycerol is 2%; sampling is performed for the third time after 60 minutes of operation, and after analysis, the content of KOH in the product is 4 ppm, and the content of glycerol is 2%; subsequent sampling analysis shows that the product content is basically stable.

[0042] The content described in the specification is merely a list of forms of the inventive concept, and the protection scope of the present application should not be regarded as being limited to the specific forms stated in the embodiments.

Claims

1. A microwave enhanced liquid-liquid heterogeneous extraction device, characterized by: The application relates to a microwave extraction column, which comprises a microwave cavity (1) and an extraction column (3) arranged in the microwave cavity (1). The extraction column (3) is divided into three parts from top to bottom, namely a light phase separation zone (31), a filler zone (32) and a heavy phase separation zone (33). The light phase outlet (34) at the top of the light phase separation zone (31) and the heavy phase inlet (37) in the middle are respectively connected with a light phase discharge pipe (2) and a heavy phase feeding pipe (5) through pipelines. A light phase inlet (36) is arranged between the filler zone (32) and the heavy phase separation zone (33) and is connected with a light phase feeding pipe (7) through a pipeline. The heavy phase outlet (35) at the bottom of the heavy phase separation zone (33) is connected with a heavy phase discharge pipe (8) through a pipeline. The material of the filler in the filler zone (32) is ceramic or glass, and the material of the extraction column (3) is quartz. The radius of the extraction column (3) is not greater than the penetration depth of the microwave generated by a microwave generating device into the light phase solution or the heavy phase solution in the extraction column (3).

2. A microwave intensified liquid-liquid non-homogeneous extraction device as claimed in claim 1, wherein: A waveguide (10) and a temperature sensor (4) are arranged on the microwave cavity (1). The number of the waveguides (10) is at least two, and the waveguides (10) are arranged on opposite sides of the microwave cavity (1). The waveguides (10) are connected with a microwave generating device. The microwave generated by the microwave generating device enters the microwave cavity (1) through the waveguides (10).

3. A microwave intensified liquid-liquid non-homogeneous extraction device as claimed in claim 1, wherein: The number of the extraction columns (3) is at least two. A first intelligent liquid separation instrument (61) for monitoring the state of the light phase separation is arranged on the upper part of the light phase separation zone (31) of the extraction column (3). A heavy phase shunt pipe is connected with the heavy phase inlet (37) in the middle of the light phase separation zone (31). The heavy phase shunt pipe is combined with a total pipe after penetrating out of the microwave cavity (1) and is connected with the heavy phase feeding pipe (5). A first electromagnetic valve is arranged on the heavy phase shunt pipe. The first electromagnetic valve is signal-connected with the first intelligent liquid separation instrument (61) through a PLC control system. The liquid separation state signal monitored by the first intelligent liquid separation instrument (61) is transmitted to the PLC control system. Then, the flow rate of the input heavy phase solution is regulated by regulating the opening degree of the first electromagnetic valve.

4. A microwave intensified liquid-liquid non-homogeneous extraction device as claimed in claim 1, wherein: The number of the extraction columns (3) is at least two. A second intelligent liquid separation instrument (62) for monitoring the state of the heavy phase separation is arranged on the lower part of the heavy phase separation zone (33) of the extraction column (3). A light phase shunt pipe is connected with the light phase inlet (36) on the extraction column (3). The light phase shunt pipe is combined with a total pipe after penetrating out of the microwave cavity (1) and is connected with the light phase feeding pipe (7). A second electromagnetic valve is arranged on the light phase shunt pipe. The second electromagnetic valve is signal-connected with the second intelligent liquid separation instrument (62) through a PLC control system. The liquid separation state signal monitored by the second intelligent liquid separation instrument (62) is transmitted to the PLC control system. Then, the flow rate of the input light phase solution is regulated by regulating the opening degree of the second electromagnetic valve.

5. A microwave intensified liquid-liquid non-homogeneous extraction device as claimed in claim 1, wherein: Flowmeters and valves are arranged on the light phase discharge pipe (2), the heavy phase feeding pipe (5), the light phase feeding pipe (7) and the heavy phase discharge pipe (8).

6. A microwave intensified liquid-liquid non-homogeneous extraction apparatus as claimed in claim 1, wherein: The microwave cavity (1) is provided with a pipeline through hole, so that the corresponding pipeline is inserted into the microwave cavity (1) and connected with the light phase outlet (34), the heavy phase inlet (37), the light phase inlet (36) and the heavy phase outlet (35) on the extraction column (3) respectively.

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