CN102304134A - Process method for extracting dihydroartemisinin from waste mother liquor in production of dihydroartemisinin - Google Patents
Process method for extracting dihydroartemisinin from waste mother liquor in production of dihydroartemisinin Download PDFInfo
- Publication number
- CN102304134A CN102304134A CN2010102266177A CN201010226617A CN102304134A CN 102304134 A CN102304134 A CN 102304134A CN 2010102266177 A CN2010102266177 A CN 2010102266177A CN 201010226617 A CN201010226617 A CN 201010226617A CN 102304134 A CN102304134 A CN 102304134A
- Authority
- CN
- China
- Prior art keywords
- mother liquor
- add
- dihydroartemisinin
- production
- dihydroarteannuin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000012452 mother liquor Substances 0.000 title claims abstract description 18
- 239000002699 waste material Substances 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title abstract description 9
- BJDCWCLMFKKGEE-ISOSDAIHSA-N artenimol Chemical compound C([C@](OO1)(C)O2)C[C@H]3[C@H](C)CC[C@@H]4[C@@]31[C@@H]2O[C@H](O)[C@@H]4C BJDCWCLMFKKGEE-ISOSDAIHSA-N 0.000 title abstract 4
- 229960002521 artenimol Drugs 0.000 title abstract 4
- 229930016266 dihydroartemisinin Natural products 0.000 title abstract 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000009461 vacuum packaging Methods 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 238000002386 leaching Methods 0.000 claims abstract description 3
- 229930187998 Dihydroarteannuin Natural products 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 8
- 238000003672 processing method Methods 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 5
- 238000001953 recrystallisation Methods 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000010612 desalination reaction Methods 0.000 claims description 2
- 239000002689 soil Substances 0.000 claims description 2
- 238000011033 desalting Methods 0.000 abstract description 2
- 239000000706 filtrate Substances 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 2
- 239000005457 ice water Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- BLUAFEHZUWYNDE-NNWCWBAJSA-N artemisinin Chemical compound C([C@](OO1)(C)O2)C[C@H]3[C@H](C)CC[C@@H]4[C@@]31[C@@H]2OC(=O)[C@@H]4C BLUAFEHZUWYNDE-NNWCWBAJSA-N 0.000 description 4
- 229960004191 artemisinin Drugs 0.000 description 4
- 229930101531 artemisinin Natural products 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention relates to a process method for extracting dihydroartemisinin from waste mother liquor in production of dihydroartemisinin. The process method is characterized by comprising the following steps of: a, concentration: mixing all waste mother liquor in production, and concentrating at 60 DEG C until the volume is 1/20 of the original volume; b, desalting: quickly cooling, adding ice water in an amount which is about 1/5 of the volume of the mother liquor, performing centrifugal filtration with stirring, discarding filtrate, and repeating the step for four times; c, extraction: adding pure water in an amount which is about 10 times weight of coarse crystals, adding equivoluminal chloroform, extracting for three times, concentrating until crystals are separated out, cooling to 0 DEG C for crystallization, and repeating the step once more; d, salt leaching: putting the crystals into a centrifuge, rotating the centrifuge at a speed of 200 rpm, adding ice water in an amount which is 10 times weight of the crystals, performing centrifugal filtration, discarding filtrate, adding a small amount of methanol before the rotation is stopped, dissolving a dry product by using an aqueous solution of NaOH, and controlling the pH value to be 7-9; and e, drying and packaging: performing vacuum drying at the temperature of between 50 and 60DEG C, and performing vacuum packaging. By the process method, production cost is saved, and enterprise benefit is improved.
Description
Technical field
The present invention relates to from produce the dihydroarteannuin waste mother liquor, extract the processing method of dihydroarteannuin.
Background technology
In the process of utilizing the synthetic dihydroarteannuin of Artemisinin, can produce a large amount of waste mother liquors, be in the preparation feedback of solution with methyl alcohol, the main component of waste mother liquor is a methyl alcohol.Wherein except a large amount of methyl alcohol and inorganic salt, also contain the dihydroarteannuin of certain content.If utilize traditional technology; Can't obtain the high dihydroarteannuin of purity; In the technical study of preparation dihydroarteannuin; Domestic a lot of manufacturing enterprise just abandons after with Methanol Recovery, does not further separate dihydroarteannuin, and this must cause the waste of resource; Utilize the waste mother liquor that produces in the production process; Produce the dihydroarteannuin rate, directly related enterprise production cost does the high performance of enterprises.
Summary of the invention
The problem that the present invention will solve provides a kind of processing method of from produce the dihydroarteannuin waste mother liquor, extracting dihydroarteannuin.
The present invention extracts the processing method of dihydroarteannuin from produce the dihydroarteannuin waste mother liquor, it is characterized in that including following steps:
A. concentrate: merge all waste mother liquors in the production, under 60 ℃ of conditions, be concentrated into 1/20 of original volume;
B. desalination: the cooling of fast speed, add the frozen water of mother liquor volume about 1/5, stir centrifuging, discard filtrating, repeat four times;
C. extraction: add the pure water of 10 times of about coarse crystallization, add isopyknic chloroform extraction again three times, be concentrated into crystal and separate out, be cooled to crystallization under 0 ℃ of condition; Recrystallization once again;
D. the desalinization of soil by flooding or leaching: crystal is put into whizzer, rotate whizzer with 200 rev/mins speed, add the frozen water of 10 times of crystallizations simultaneously, centrifuging discards filtered liquid; Before stopping operating, add a little methyl alcohol; With NaOH aqueous solution dissolving dry product, control ph value is 7-9;
E. baking is wrapped: vacuum-drying under 50 ℃ of-60 ℃ of conditions, vacuum packaging.
The present invention extracts the processing method of dihydroarteannuin from produce the dihydroarteannuin waste mother liquor, desalting through pure water adds the centrifugal technology that desalts, and dihydroarteannuin solution saves production cost in the extraction waste mother liquor, does the high performance of enterprises.
Embodiment
Embodiment 1,
1, merging with the 1KG Artemisinin is the mother liquor 10L of raw material production dihydroarteannuin, under 60 ℃ of conditions, is concentrated into the 500ml of original volume.
2, in the chuck of reactor, feed frozen water, the cooling of fast speed adds the 2L frozen water in reactor, stirs 10 minutes, and centrifuging discards filtrating, repeats four times.
3, add the 1L pure water, add the 1L chloroform extraction three times, be concentrated into the 340ml of original nut liquid volume, be placed in crystallization under 0 ℃ of condition, recrystallization once.
4, crystal is put into whizzer, rotate whizzer with 200 rev/mins speed, add the 9L frozen water simultaneously, centrifuging discards filtered liquid.Before stopping operating, add 200ml methyl alcohol.
5, detect with high performance liquid phase, purity is 98.2%, vacuum-drying under 50-60 ℃ of condition, the 74.7g that weighs, vacuum packaging, 20 ℃ of room temperature preservations.
Embodiment 2:
1, merging with the 10KG Artemisinin is the mother liquor 100L of raw material production dihydroarteannuin, under 60 ℃ of conditions, is concentrated into the 5L of original volume.
2, in the chuck of reactor, feed frozen water, the cooling of fast speed adds the 20L frozen water in reactor, stirs 18 minutes, and centrifuging discards filtrating, repeats four times.
3, add the 11L pure water, add the 11L chloroform extraction three times, be concentrated into the 3.5L of original nut liquid volume, be placed in crystallization under 0 ℃ of condition, recrystallization once.
4, crystal is put into whizzer, rotate whizzer with 200 rev/mins speed, add the 110L frozen water simultaneously, centrifuging discards filtered liquid.Before stopping operating, add 3L methyl alcohol.
5, detect with high performance liquid phase, purity is 98.6%, vacuum-drying under 50-60 ℃ of condition, the 831.7g that weighs, vacuum packaging, 20 ℃ of room temperature preservations.
Embodiment 3:
1, merging with the 20KG Artemisinin is the mother liquor 200L of raw material production dihydroarteannuin, under 60 ℃ of conditions, is concentrated into the 11L of original volume.
2, in the chuck of reactor, feed frozen water, the cooling of fast speed adds the 40L frozen water in reactor, stirs 20 minutes, and centrifuging discards filtrating, repeats four times.
3, add the 20L pure water, add the 20L chloroform extraction three times, be concentrated into the 7L of original nut liquid volume, be placed in crystallization under 0 ℃ of condition, recrystallization once.
4, crystal is put into whizzer, rotate whizzer with 200 rev/mins speed, add the 200L frozen water simultaneously, centrifuging discards filtered liquid.Before stopping operating, add 6.5L methyl alcohol.
5, detect with high performance liquid phase, purity is 98.1%, vacuum-drying under 50-60 ℃ of condition, the 1694.1g that weighs, vacuum packaging, 20 ℃ of room temperature preservations.
Claims (1)
1. from produce the dihydroarteannuin waste mother liquor, extract the processing method of dihydroarteannuin, it is characterized in that including that following steps: a. concentrates: merge all waste mother liquors in the production, under 60 ℃ of conditions, be concentrated into 1/20 of original volume;
B. desalination: the cooling of fast speed, add the frozen water of mother liquor volume about 1/5, stir centrifuging, discard filtrating, repeat four times;
C. extraction: add the pure water of 10 times of about coarse crystallization, add isopyknic chloroform extraction again three times, be concentrated into crystal and separate out, be cooled to crystallization under 0 ℃ of condition; Recrystallization once again;
D. the desalinization of soil by flooding or leaching: crystal is put into whizzer, rotate whizzer with 200 rev/mins speed, add the frozen water of 10 times of crystallizations simultaneously, centrifuging discards filtered liquid; Before stopping operating, add a little methyl alcohol; With NaOH aqueous solution dissolving dry product, control ph value is 7-9;
E. baking is wrapped: vacuum-drying under 50 ℃ of-60 ℃ of conditions, vacuum packaging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010226617 CN102304134B (en) | 2010-07-10 | 2010-07-10 | Process method for extracting dihydroartemisinin from waste mother liquor in production of dihydroartemisinin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010226617 CN102304134B (en) | 2010-07-10 | 2010-07-10 | Process method for extracting dihydroartemisinin from waste mother liquor in production of dihydroartemisinin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102304134A true CN102304134A (en) | 2012-01-04 |
| CN102304134B CN102304134B (en) | 2013-06-26 |
Family
ID=45378067
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010226617 Expired - Fee Related CN102304134B (en) | 2010-07-10 | 2010-07-10 | Process method for extracting dihydroartemisinin from waste mother liquor in production of dihydroartemisinin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102304134B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634554A (en) * | 2012-04-14 | 2012-08-15 | 向华 | Method for efficiently converting artemisinin from waste mother liquor after artemisinin separation |
| CN104910173A (en) * | 2015-06-12 | 2015-09-16 | 重庆华方武陵山制药有限公司 | Treatment method for artesunate crystallization mother liquid |
| CN106543198A (en) * | 2016-08-31 | 2017-03-29 | 重庆华方武陵山制药有限公司 | A kind of method that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor |
| CN107522712A (en) * | 2017-06-30 | 2017-12-29 | 禹州市天源生物科技有限公司 | A kind of production technology for synthesizing dihydroartemisinine waste mother liquor extraction dihydroartemisinine |
| CN111499651A (en) * | 2019-01-30 | 2020-08-07 | 昆药集团股份有限公司 | Dihydroartemisinin Form A crystal Form and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524527B (en) * | 2013-10-25 | 2015-09-16 | 广州合诚三先生物科技有限公司 | A kind of method simultaneously extracting arteannuinic acid and dihydroartemisinic acid from the rear waste liquid of Artemisinin separation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1132207A (en) * | 1995-03-25 | 1996-10-02 | 中国科学院上海药物研究所 | Method for prepn. of dihydro arteannuin |
| US20030181513A1 (en) * | 2002-03-25 | 2003-09-25 | Council Of Scientific & Industrial Research | Single pot conversion of artemisinin into artemether |
-
2010
- 2010-07-10 CN CN 201010226617 patent/CN102304134B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1132207A (en) * | 1995-03-25 | 1996-10-02 | 中国科学院上海药物研究所 | Method for prepn. of dihydro arteannuin |
| US20030181513A1 (en) * | 2002-03-25 | 2003-09-25 | Council Of Scientific & Industrial Research | Single pot conversion of artemisinin into artemether |
Non-Patent Citations (2)
| Title |
|---|
| A. BROSSI，等: "Arteether, a New Antimalarial Drug: Synthesis and Antimalarial Properties", 《JOURNAL OF MEDICINAL CHEMISTRY》, vol. 31, no. 3, 31 March 1988 (1988-03-31), XP001061731, DOI: doi:10.1021/jm00398a026 * |
| LAI-KING SY，等: "Synthesis of 6,7-dehydroartemisinic acid", 《JOURNAL OF THE CHEMICAL SOCIETY，PERKIN TRANSACTION 1》, no. 19, 11 September 2001 (2001-09-11) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634554A (en) * | 2012-04-14 | 2012-08-15 | 向华 | Method for efficiently converting artemisinin from waste mother liquor after artemisinin separation |
| CN104910173A (en) * | 2015-06-12 | 2015-09-16 | 重庆华方武陵山制药有限公司 | Treatment method for artesunate crystallization mother liquid |
| CN106543198A (en) * | 2016-08-31 | 2017-03-29 | 重庆华方武陵山制药有限公司 | A kind of method that dihydroartemisinine is reclaimed in the crystallization from artesunate mother liquor |
| CN107522712A (en) * | 2017-06-30 | 2017-12-29 | 禹州市天源生物科技有限公司 | A kind of production technology for synthesizing dihydroartemisinine waste mother liquor extraction dihydroartemisinine |
| CN111499651A (en) * | 2019-01-30 | 2020-08-07 | 昆药集团股份有限公司 | Dihydroartemisinin Form A crystal Form and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102304134B (en) | 2013-06-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102304134B (en) | Process method for extracting dihydroartemisinin from waste mother liquor in production of dihydroartemisinin | |
| CN101914054B (en) | Comprehensive method for extracting L-tryptophan from fermentation liquor | |
| CN101518291B (en) | Preparation method for instant tea | |
| CN102976923B (en) | New process for extracting lactic acid from lactic acid fermentation liquid | |
| CN104593447B (en) | A kind of energy-conservation preparation technology of high-quality powdered glucose | |
| CN102586496A (en) | Process for producing xylose | |
| CN101628924A (en) | Process for extracting rebaudioside C in stevioside | |
| CN110724045B (en) | Preparation method of curcumin with low solvent residue | |
| CN104262251B (en) | A kind of method extracting huperzine A from Herba Lycopodii serrati | |
| CN104109078B (en) | A kind of method that in Sulpyrine production, ethanol reclaims | |
| CN105061532A (en) | Production method for hesperidin | |
| CN102839202A (en) | Method for processing erythritol fermentation liquor | |
| CN111777493A (en) | Xylitol mother liquor utilization system and method | |
| CN112266362B (en) | Method for extracting tetrahydropyrimidine by combining aqueous two-phase extraction with ion exchange chromatography | |
| CN112047362A (en) | Multistage purification equipment and process for high-salt-content wastewater | |
| CN102807497A (en) | Method for recovering chloroacetic acid method glycine catalyst methenamine | |
| CN109320400B (en) | Method for extracting natural mannitol from waste liquid of mogroside production | |
| CN101492484B (en) | Synthetic circulation production process for guanine nucleoside | |
| CN114591382B (en) | Preparation method of high-content hesperidin | |
| CN111547916A (en) | Salt and nitrate separation method for nitrate-rich wastewater | |
| CN107074718A (en) | Purify forulic acid and/or the method for its salt | |
| CN109553645B (en) | Method for extracting low-content erythromycin A in fermentation solution | |
| WO2014114031A1 (en) | Mixed solvent for refining surfactants and surfactant purification method | |
| CN107955051A (en) | A kind of preparation method of aurantiin | |
| CN111254231B (en) | Method for extracting crystalline xylose from xylose mother liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130626 |