Artemisinin dynamic concurrent and countercurrent extraction method

Abstract

An artemisinin dynamic cocurrent-countercurrent extraction method belongs to the technical field of artemisinin extraction, and comprises a cocurrent-countercurrent extraction device and a cocurrent-countercurrent extraction method. The concurrent and countercurrent extraction device comprises three sections of directly connected extraction tanks and a solvent bridge pipe, the extraction tanks are respectively a concurrent extraction tank, a transition extraction tank and a countercurrent extraction tank, and during extraction, sweet wormwood leaves are put into the three extraction tanks from a feed port of the concurrent extraction tank and gradually filled into the three extraction tanks; injecting a solvent into the countercurrent extraction tank, and gradually filling the three tanks with the solvent; inputting the solvent in the transition extraction tank into the down-flow extraction tank by using a solvent bridge pipe, and gradually filling the down-flow extraction tank with the solvent from the outer end of the down-flow extraction tank; then starting a stirring shaft to perform dynamic stirring extraction; the method has the beneficial effects that the extraction yield of artemisinin is effectively improved, the solvent loss is reduced, and the solvent recovery rate is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of artemisinin extraction, in particular to a dynamic cocurrent and countercurrent extraction method of artemisinin. Background Art

[0002] Artemisinin is a sesquiterpene lactone compound with antimalarial activity extracted from the Asteraceae plant Artemisia annua. Its application value in the medical field has been widely recognized and it is an effective antimalarial drug. At present, the main extraction methods of artemisinin include solvent extraction, ethanol reflux extraction, supercritical fluid extraction, microwave-assisted extraction, etc. The solvent extraction method has problems such as low extraction efficiency, large solvent consumption, and long extraction time; although the supercritical fluid extraction method has the advantages of high extraction efficiency and good product purity, it has large equipment investment and harsh operating conditions, which limits the large-scale industrial production of artemisinin. Therefore, it is of great practical significance to develop an efficient, energy-saving and environmentally friendly artemisinin extraction method. Summary of the invention

[0003] The purpose of the present invention is to provide a dynamic co-current and counter-current extraction method for artemisinin, which improves the extraction efficiency of artemisinin, reduces energy consumption, and realizes efficient extraction of artemisinin by combining dynamic counter-current with co-current technology.

[0004] In order to solve the above technical problems, the technical solution adopted by the present invention is a dynamic co-current and counter-current extraction method of artemisinin, including a co-current and counter-current extraction device and a co-current and counter-current extraction method.

[0005] The co-current and countercurrent extraction device comprises three sections of directly connected extraction tanks and solvent bridge pipes, wherein the three sections of directly connected extraction tanks are respectively a co-current extraction tank, a transition extraction tank and a countercurrent extraction tank, wherein stirring shafts and spiral stirring propulsion blades are arranged in the co-current extraction tank and the countercurrent extraction tank, wherein a feed port is arranged on the outer end tank wall of the co-current extraction tank, and an extract collecting pipe is arranged on the inner end tank wall of the co-current extraction tank; the head end of the transition extraction tank is directly connected to the inner end of the co-current extraction tank, and the tail end of the transition extraction tank is directly connected to the inner end of the countercurrent extraction tank; a slag outlet and a solvent injection pipe are arranged on the outer end tank wall of the countercurrent extraction tank; the liquid inlet end of the solvent bridge pipe is connected to the tank wall at the head end position of the transition extraction tank where the transition extraction tank is connected to the co-current extraction tank, and the liquid outlet end of the solvent bridge pipe is connected to the tank wall at the outer end position of the co-current extraction tank, and the extract collecting pipe, the solvent injection pipe and the solvent bridge pipe are all provided with an infusion pump.

[0006] Also equipped with solvent heating device.

[0007] The driving motor of the stirring shaft is a forward and reverse stepping motor. When the material needs to be pushed forward, the forward and reverse stepping motor is adjusted to always rotate forward. When the material needs to be stirred, the forward and reverse stepping motor is adjusted to intermittent forward and reverse rotation.

[0008] The co-current and counter-current extraction method comprises the following steps: S1: The Artemisia annua leaves are put into the feed port of the downstream extraction tank, and the Artemisia annua leaves are gradually filled into the downstream extraction tank, the transition extraction tank and the countercurrent extraction tank through the spiral stirring and propulsion blades in the downstream extraction tank and the countercurrent extraction tank.

[0009] S2: Input the solvent into the solvent heating device for heating, then turn on the infusion pump on the solvent injection tube, inject the solvent from the solvent injection tube into the countercurrent extraction tank, and gradually fill the countercurrent extraction tank and the transition extraction tank; this section is countercurrent extraction.

[0010] S3: Turn on the infusion pump on the solvent bridge pipe, input the solvent in the transition extraction tank into the downstream extraction tank through the solvent bridge pipe, and allow the solvent to gradually fill the downstream extraction tank from the outer end of the downstream extraction tank; this section is the downstream extraction.

[0011] S4: After the Artemisia annua leaves fill up the downstream extraction tank, the transition extraction tank and the countercurrent extraction tank, and then fill up the countercurrent extraction tank, the transition extraction tank and the downstream extraction tank with the solvent, the stirring shaft is turned on to perform slow dynamic stirring extraction.

[0012] S5: Turn on the infusion pump on the extract collection tube to output and collect the solvent in the downstream extraction tank to obtain artemisinin extract.

[0013] S6: Input the artemisinin extract into a chromatography column for separation to obtain artemisinin and recover the solvent.

[0014] S7: The Artemisia annua leaf residue is discharged from the residue outlet and put into a squeezer for drying to recover the solvent.

[0015] Extracting artemisinin according to this method only takes about 3 hours, with less energy consumption and labor, and the yield of artemisinin is over 99%. In the past, static extraction tanks were used for extraction, which required four extractions of 1 hour each, consuming a lot of energy and labor, and the yield was only about 95%. It can be seen that this method improves the yield, reduces energy consumption, and saves time.

[0016] The solvent is one of petroleum ether, ethyl acetate and acetone.

[0017] Compared with the prior art, the beneficial effects of the present invention are: the flow directions of the solvent and the material are opposite but the same, reverse flow is adopted in the solvent injection section, and forward flow is adopted in the solvent output section, and dynamic stirring is adopted during the process, which effectively improves the extraction yield of artemisinin and reduces energy consumption. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the structure of the co-current and counter-current extraction device in the present invention.

[0019] In the figure: 1. solvent bridge pipe, 2. downstream extraction tank, 3. transition extraction tank, 4. countercurrent extraction tank, 5. stirring shaft, 6. spiral stirring propulsion blade, 7. feed port, 8. extraction liquid collection pipe, 9. slag outlet, 10. solvent injection pipe, 11. infusion pump, 12. solvent heating device, 13. forward and reverse stepping motor. DETAILED DESCRIPTION

[0020] The present invention will be further described below in conjunction with examples. The following examples are intended to illustrate the present invention rather than to further limit the present invention, and should not be used to limit the scope of protection of the present invention.

[0021] As shown in the figure, the present invention first provides a co-current and countercurrent extraction device, which includes three sections of directly connected extraction tanks and a solvent bridge pipe 1, wherein the three sections of directly connected extraction tanks are respectively a co-current extraction tank 2, a transition extraction tank 3 and a countercurrent extraction tank 4, wherein the co-current extraction tank 2 and the countercurrent extraction tank 4 are provided with a stirring shaft 5 and a spiral stirring propulsion blade 6, a feed port 7 is provided on the outer end tank wall of the co-current extraction tank 2, and an extract collecting pipe 8 is provided on the inner end tank wall of the co-current extraction tank 2; the head end of the transition extraction tank 3 is directly connected to the inner end of the co-current extraction tank 2, and the transition extraction tank 3 is provided with a stirring shaft 5 and a spiral stirring propulsion blade 6; the outer end tank wall of the co-current extraction tank 2 is provided with a feeding port 7, and the inner end tank wall of the co-current extraction tank 2 is provided with an extract collecting pipe 8; the head end of the transition extraction tank 3 is directly connected to the inner end of the co-current extraction tank 2, and the The tail end is directly connected with the inner end of the countercurrent extraction tank 4; a slag outlet 9 and a solvent injection pipe 10 are provided on the outer end tank wall of the countercurrent extraction tank 4; the liquid inlet end of the solvent bridge pipe 1 is connected to the tank wall of the head end position of the transition extraction tank 3 where the transition extraction tank 3 is connected to the downstream extraction tank 2, and the liquid outlet end of the solvent bridge pipe 1 is connected to the tank wall of the outer end position of the downstream extraction tank 2; the extract collecting pipe 8, the solvent injection pipe 10 and the solvent bridge pipe 1 are all provided with an infusion pump 11; the solvent injection pipe 10 is externally connected to a solvent heating device 12; the driving motor of the stirring shaft 5 is a forward and reverse stepping motor 13.

[0022] Based on the above-mentioned co-current and counter-current extraction device, dynamic co-current and counter-current extraction of artemisinin is carried out according to the following steps: Example 1

[0023] S1: 100 kg of dried, crushed and 40-mesh sieved Artemisia annua leaf powder (artemisinin content of 18‰) is added from the feed port 7 of the downstream extraction tank 2, and the forward and reverse stepping motor 13 is adjusted to always rotate in the forward direction. The spiral stirring and propulsion blades 6 in the downstream extraction tank 2 and the countercurrent extraction tank 4 gradually fill the Artemisia annua leaves into the downstream extraction tank 2, the transition extraction tank 3 and the countercurrent extraction tank 4.

[0024] S2: Input 350L of solvent petroleum ether into the solvent heating device 12 and heat it to 40°C, then turn on the infusion pump 11 on the solvent injection pipe 10, inject the solvent from the solvent injection pipe 10 into the countercurrent extraction tank 4, and gradually fill the countercurrent extraction tank 4 and the transition extraction tank 3.

[0025] S3: Turn on the infusion pump 11 on the solvent bridge tube 1, input the solvent in the transition extraction tank 3 into the downstream extraction tank 2 through the solvent bridge tube 1, and gradually fill the downstream extraction tank 2 with the solvent starting from the outer end of the downstream extraction tank 2.

[0026] S4: After the Artemisia annua leaves fill the downstream extraction tank 2, the transition extraction tank 3 and the countercurrent extraction tank 4, and then fill the countercurrent extraction tank 4, the transition extraction tank 3 and the downstream extraction tank 2 with the solvent in turn, adjust the forward and reverse stepper motor 13 to intermittent forward rotation and reverse rotation, turn on the stirring shaft 5 to perform slow dynamic stirring extraction for 195 minutes.

[0027] S5: Turn on the infusion pump 11 on the extract collection tube 8 to output and collect the solvent in the downstream extraction tank 2 to obtain the artemisinin extract.

[0028] S6: The artemisinin extract was input into a chromatography column for separation to obtain 1.79421 kg of artemisinin and recover the solvent.

[0029] S7: The Artemisia annua leaf residue is discharged from the residue outlet and put into a squeezer for drying to recover the solvent.

[0030] According to the measurement, the total recovery of petroleum ether solvent was 345L, the solvent consumption was 5L, and the solvent consumption rate was 1.41%; the artemisinin production was 1.79421kg, and the yield was: 1.79421÷(100kg×18‰)≈99.678% Example 2

[0031] S1: 100 kg of dried, crushed and 40-mesh sieved Artemisia annua leaf powder (artemisinin content of 18‰) is added from the feed port 7 of the downstream extraction tank 2, and the forward and reverse stepping motor 13 is adjusted to always rotate in the forward direction. The spiral stirring and propulsion blades 6 in the downstream extraction tank 2 and the countercurrent extraction tank 4 gradually fill the Artemisia annua leaves into the downstream extraction tank 2, the transition extraction tank 3 and the countercurrent extraction tank 4.

[0032] S2: Input 350L of solvent petroleum ether into the solvent heating device 12 and heat it to 45°C, then turn on the infusion pump 11 on the solvent injection pipe 10, inject the solvent from the solvent injection pipe 10 into the countercurrent extraction tank 4, and gradually fill the countercurrent extraction tank 4 and the transition extraction tank 3.

[0033] S3: Turn on the infusion pump 11 on the solvent bridge tube 1, input the solvent in the transition extraction tank 3 into the downstream extraction tank 2 through the solvent bridge tube 1, and gradually fill the downstream extraction tank 2 with the solvent starting from the outer end of the downstream extraction tank 2.

[0034] S4: After the Artemisia annua leaves fill the downstream extraction tank 2, the transition extraction tank 3 and the countercurrent extraction tank 4, and then fill the countercurrent extraction tank 4, the transition extraction tank 3 and the downstream extraction tank 2 with the solvent in turn, adjust the forward and reverse stepper motor 13 to intermittent forward rotation and reverse rotation, turn on the stirring shaft 5 to perform slow dynamic stirring extraction for 180 minutes.

[0035] S5: Turn on the infusion pump 11 on the extract collection tube 8 to output and collect the solvent in the downstream extraction tank 2 to obtain the artemisinin extract.

[0036] S6: Input the artemisinin extract into a chromatography column for separation to obtain 1.79634 kg of artemisinin and recover the solvent.

[0037] S7: The Artemisia annua leaf residue is discharged from the residue outlet and put into a squeezer for drying to recover the solvent.

[0038] According to the measurement, the total recovery of petroleum ether solvent was 344.5L, the solvent consumption was 5.5L, and the solvent consumption rate was 1.57%. The artemisinin production was 1.79634kg, and the yield was 1.79634÷(100kg×18‰)≈99.796% Example 3

[0039] S1: 100 kg of dried, crushed and 40-mesh sieved Artemisia annua leaf powder (artemisinin content of 18‰) is added from the feed port 7 of the downstream extraction tank 2, and the forward and reverse stepping motor 13 is adjusted to always rotate in the forward direction. The spiral stirring and propulsion blades 6 in the downstream extraction tank 2 and the countercurrent extraction tank 4 gradually fill the Artemisia annua leaves into the downstream extraction tank 2, the transition extraction tank 3 and the countercurrent extraction tank 4.

[0040] S2: Input 350L of solvent petroleum ether into the solvent heating device 12 and heat it to 50°C, then turn on the infusion pump 11 on the solvent injection pipe 10, inject the solvent from the solvent injection pipe 10 into the countercurrent extraction tank 4, and gradually fill the countercurrent extraction tank 4 and the transition extraction tank 3.

[0041] S3: Turn on the infusion pump 11 on the solvent bridge tube 1, input the solvent in the transition extraction tank 3 into the downstream extraction tank 2 through the solvent bridge tube 1, and gradually fill the downstream extraction tank 2 with the solvent starting from the outer end of the downstream extraction tank 2.

[0042] S4: After the Artemisia annua leaves fill the downstream extraction tank 2, the transition extraction tank 3 and the countercurrent extraction tank 4, and then fill the countercurrent extraction tank 4, the transition extraction tank 3 and the downstream extraction tank 2 with the solvent in turn, adjust the forward and reverse stepper motor 13 to intermittent forward rotation and reverse rotation, turn on the stirring shaft 5 to perform slow dynamic stirring extraction for 165 minutes.

[0043] S5: Turn on the infusion pump 11 on the extract collection tube 8 to output and collect the solvent in the downstream extraction tank 2 to obtain the artemisinin extract.

[0044] S6: Input the artemisinin extract into a chromatography column for separation to obtain 1.79535 kg of artemisinin and recover the solvent.

[0045] S7: The Artemisia annua leaf residue is discharged from the residue outlet and put into a squeezer for drying to recover the solvent.

[0046] According to the measurement, the total recovery of petroleum ether solvent was 344.8L, the solvent consumption was 5.2L, and the solvent consumption rate was 1.49%. The artemisinin production was 1.79535kg, and the yield was 1.79535÷(100kg×18‰)≈99.742% The method adopts a flow direction in which the solvent and the material are first opposite and then the same, with reverse flow in the solvent injection section and forward flow in the solvent output section. Dynamic stirring is used during the process, which effectively improves the extraction efficiency of artemisinin and reduces energy consumption. The artemisinin extract drawn out in the downstream extraction tank can also be automatically cleared. According to measurements, the method only takes 3 hours to complete an artemisinin extraction yield of more than 99%. In this process, less energy consumption and less labor are required.

[0047] Although the existing static extraction method only uses one tank, it requires four extractions, each taking 1 hour, and requires four times the same amount of solvent. It consumes a lot of energy and requires a lot of manpower, but the artemisinin yield is only about 95%.

Claims

1. A dynamic cocurrent and countercurrent extraction method for artemisinin, characterized in that It includes a co-current and counter-current extraction device and a co-current and counter-current extraction method; The co-current and countercurrent extraction device comprises three sections of directly connected extraction tanks and solvent bridge pipes, wherein the three sections of directly connected extraction tanks are respectively a co-current extraction tank, a transition extraction tank and a countercurrent extraction tank, wherein the co-current extraction tank and the countercurrent extraction tank are provided with a stirring shaft and a spiral stirring propulsion blade, a feed port is provided on the outer end tank wall of the co-current extraction tank, and an extract collecting pipe is provided on the inner end tank wall of the co-current extraction tank; the head end of the transition extraction tank is directly connected to the inner end of the co-current extraction tank, and the tail end of the transition extraction tank is directly connected to the inner end of the countercurrent extraction tank; a slag outlet and a solvent injection pipe are provided on the outer end tank wall of the countercurrent extraction tank; the liquid inlet end of the solvent bridge pipe is connected to the tank wall at the head end position of the transition extraction tank, and the liquid outlet end of the solvent bridge pipe is connected to the tank wall at the outer end position of the co-current extraction tank, and the extract collecting pipe, the solvent injection pipe and the solvent bridge pipe are all provided with an infusion pump; The co-current and counter-current extraction method comprises the following steps: S1: putting the Artemisia annua leaves into the feed port of the downstream extraction tank, and gradually filling the downstream extraction tank, the transition extraction tank and the countercurrent extraction tank with the Artemisia annua leaves through the spiral stirring and propulsion blades in the downstream extraction tank and the countercurrent extraction tank; S2: Turn on the infusion pump on the solvent injection tube, inject the solvent from the solvent injection tube into the countercurrent extraction tank, and gradually fill the countercurrent extraction tank and the transition extraction tank; this section is countercurrent extraction; S3: Turn on the infusion pump on the solvent bridge pipe, input the solvent in the transition extraction tank into the downstream extraction tank through the solvent bridge pipe, and gradually fill the downstream extraction tank with the solvent from the outer end of the downstream extraction tank; this section is the downstream extraction; S4: After the Artemisia annua leaves fill the downstream extraction tank, the transition extraction tank and the countercurrent extraction tank, and then fill the countercurrent extraction tank, the transition extraction tank and the downstream extraction tank with the solvent, the stirring shaft is turned on to perform dynamic stirring extraction; S5: Turn on the infusion pump on the extract collection tube to output and collect the solvent in the downstream extraction tank to obtain artemisinin extract.

2. The dynamic cocurrent and countercurrent extraction method of artemisinin according to claim 1, characterized in that The co-current and counter-current extraction device is also equipped with a solvent heating device; during extraction, the solvent is input into the solvent heating device for heating, and then the infusion pump on the solvent injection tube is turned on to inject the solvent.

3. The dynamic co-current and counter-current extraction method of artemisinin according to claim 2, characterized in that The driving motor of the stirring shaft is a forward and reverse stepping motor. When the material needs to be pushed forward, the forward and reverse stepping motor is adjusted to always rotate forward. When the material needs to be stirred, the forward and reverse stepping motor is adjusted to intermittent forward and reverse rotation.

4. The dynamic co-current and counter-current extraction method of artemisinin according to claim 3, characterized in that The solvent is one of petroleum ether, ethyl acetate and acetone.

5. The dynamic co-current and counter-current extraction method of artemisinin according to claim 4, characterized in that The co-current and counter-current extraction method further comprises step S6: inputting the artemisinin extract into a chromatography column for separation to obtain artemisinin and recover the solvent.

6. The dynamic co-current and counter-current extraction method of artemisinin according to claim 5, characterized in that The co-current and counter-current extraction method further comprises step S7: discharging the Artemisia annua leaf residue from the residue outlet and putting it into a squeezer for drying to recover the solvent.

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