CN104628739A - Extraction technology of artemisinin - Google Patents
Extraction technology of artemisinin Download PDFInfo
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- CN104628739A CN104628739A CN201310550808.2A CN201310550808A CN104628739A CN 104628739 A CN104628739 A CN 104628739A CN 201310550808 A CN201310550808 A CN 201310550808A CN 104628739 A CN104628739 A CN 104628739A
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- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
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Abstract
The invention relates to an extraction technology of artemisinin, and belongs to the technical field of natural plant extraction. The extraction technology comprises the following steps: (1) drying raw materials: putting the raw materials in a drying facility to dry the raw materials; (2) primary preparation of artemisinin: putting the dried raw materials in an extraction tank, adding petroleum ether into the extraction tank, heating, carrying out reflux extraction, discharging the liquid extract from the extraction tank after the reflux extraction, allowing the liquid extract to stand still for a while, collecting the supernate, making the supernate go through a silica gel column, then washing the silica gel column by petroleum ether, collecting the fractions containing artemisinin, transferring the fractions to a condensing tank, condensing the fractions, transferring the condensed liquid to a crystallization tank when the liquid in the condensing tank start to crystallize, carrying out crystallization in the crystallization tank, filtering to obtain the crystals, and drying the crystals so as to obtain crude artemisinin; (3) artemisinin refinement: placing the crude artemisinin in an alcohol-precipitation tank, dissolving the crude artemisinin by ethanol with a concentration of 85-95%, wherein the volume of the ethanol is 60 to 70 times of that of the crude artemisinin, allowing the solution to stand still for a while, collecting the supernate, subjecting the supernate to fine filtration, transferring the filtrate to a condensing tank, condensing the filtrate, allowing the condensed filtrate to stand still so as to carry out crystallization, filtering to obtain the crystals, and finally drying the crystals in vacuum so as to obtain refined artemisinin.
Description
Technical field
The present invention relates to natural plain extractive technique field, particularly a kind of extraction process of Artemisinin.
Background technology
Artemisinin (artemisin) is the artemisinin-based drug extracted from medicinal plant Herba Artemisiae annuae (artemisia annua L.), for the sesquiterpene lactones compound containing peroxy radicals, being the Chinese herbal medicine extract by Western medicine development that China uniquely obtains international endorsement, is the anti-malarial bulk drug that the World Health Organization's clear stipulaties replaces quinine.The Artemisinin volume of production and marketing of China accounts for more than 90% of global volume of production and marketing, and the extractive technique of China also just represents world standard.
The organic solvent extraction separation that the technique of Artemisinin is mainly traditional is extracted in current domestic Herba Artemisiae annuae, namely adopt organic solvent as ethanol, acetone, gasoline etc. carry out after extraction obtains extracting solution medicinal extract to Herba Artemisiae annuae, Artemisinin sterling is obtained again through macroporous resin or silicagel column fractional crystallization, this technical matters is simply ripe, and domestic most Artemisinin manufacturing enterprise all continues to use the extracting method of this classics.Its main shortcoming is that extraction time is long, and extraction yield is low, and greatly, environmental pollution is large for solvent, energy consumption.Because the large production application of this method starts from 2004, so far less than ten years, the space of thus improving is very large.
Supercritical carbon dioxide extraction method also claims green extraction method, and this method is widely used for the extraction of spices, has that environment is good, operational safety, does not have that pest is residual, product quality is high and can keep the features such as intrinsic smell.After entering for the 90's, supercritical carbon dioxide extraction method starts to apply to extract effective medicinal components etc. from medicinal plant, also there is research in China at the supercritical fluid extraction of Artemisinin according to reports, but it is large to there is equipment investment in whole therefore method, throughput is low, running cost is high, there is no the shortcoming of the market competitiveness, still do not have an enterprise to carry out large-scale industrial production at home and abroad so far.
Summary of the invention
Object of the present invention provides a kind of energy-conservation, consumption reduction, clean, the Green extraction process for artemisinin that significantly reduces waste discharge, the low applicable large-scale commercial production of cost.
The technical solution used in the present invention is to achieve the above object of the invention: a kind of Green extraction process for artemisinin, this extraction process comprises the following steps: sweet wormwood raw material is put in microwave energy saving drying plant and carried out drying treatment by (1), in drying process, the temperature of microwave energy saving drying plant is set to 50-70 DEG C, the drying treatment time is 30-40 minute, when reducing to 6-8% to sweet wormwood raw material moisture, take out the pack of sweet wormwood raw material, warehouse-in is preserved;
(2) the first system of Artemisinin: the sweet wormwood raw material after drying treatment in step (1) is put in extractor, close the dog-house of extractor, the fuel charging valve opening extractor adds sherwood oil in extractor, heating countercurrent extraction, temperature controls within the scope of 60-80 DEG C, after countercurrent extraction liquid is released extractor, extracting solution is left standstill, after the assorted precipitation in countercurrent extraction liquid, get supernatant liquor makes it pass through silicagel column, sherwood oil eluting silica gel post is used again after silicagel column is saturated, collection takes off and concentrates from silicagel column containing Artemisinin stream part and putting it in concentration tank of coming out, when having crystal to separate out to concentration tank, concentrated solution is put crystallization 18-24 hour to crystallizer, during crystallization, crystallizer water coolant forces cooling to keep Tc to control at 25 DEG C-35 DEG C, crystal is obtained after being filtered by mother liquor in concentration tank after crystallization completes, crystal is drying to obtain Artemisinin crude product,
(3) Artemisinin is refining: leave standstill after the Artemisinin crude product obtained in step (2) being placed in Alcohol-settling tank 60-70 times of 85-90% dissolve with ethanol, get supernatant liquor secondary filter, after filtrate is placed in concentration tank the 1/2-3/4 being concentrated into original volume, concentrated solution is put in crystallizer, leave standstill spontaneous nucleation 18-24 hour at normal temperatures, obtain crystal after being fallen by mother liquor suction filtration after crystallization completes, crystal obtains Artemisinin fine work after vacuum drying treatment.
After the mother liquor that wherein suction filtration goes out from step (3) is concentrated into the 1/2-3/4 of its volume again, leave standstill spontaneous nucleation 18-24 hour at normal temperatures again, same method process mother liquor three to four times, gained crystal is Artemisinin crude product, and Artemisinin crude product obtains Artemisinin fine work by step (3) process again.
When wherein getting supernatant liquor by silicagel column in step (2), flow out stream part of silicagel column, part free from foreign meter direct back dissolving agent stock use again, impure part is by after concentration and recovery sherwood oil, and gained concentrated solution is the material A containing Herba Artemisiae Annuae oil and sweet wormwood wax; Also collect in eluting silica gel post process flow out from silicagel column impure, not containing part stream part of Artemisinin composition, after concentration and recovery sherwood oil, gained concentrated solution is the material B containing Herba Artemisiae Annuae oil and sweet wormwood wax.
Wherein after step (3), also comprise step (4) recovery and reuse of waste: the mother liquor leach step (2) and gained are collected containing Herba Artemisiae Annuae oil and sweet wormwood wax material A and material B and be placed in extractor and be heated to 60-75 DEG C, the sherwood oil gasified is reclaimed by with the tank connected device of extraction, residue mother liquor passes through steam distillation again, reclaim by with the tank connected device of extraction the Herba Artemisiae Annuae oil gasified, cool and collect remaining material sweet wormwood wax in extractor.
Wherein in step (2), heating countercurrent extraction need carry out 3 times, and extraction time first time is 2-3 hour, and second time extraction time is 1-2 hour, and extraction time third time is 0.5-1 hour.
After wherein countercurrent extraction liquid and solvent oil being released extractor in step (2), also include following technique: close oil drain valve, the steaming valve that rushes opening extractor carries out punching steaming to sweet wormwood slag, after the sherwood oil in sweet wormwood slag volatilizees recovery completely, is discharged outside extractor by sweet wormwood slag.
Wherein in step (2), contain 5%-10% ethyl acetate for the sherwood oil of eluting silica gel post.
After wherein using sherwood oil eluting silica gel post in step (2), also comprise the technique with the hot water cleaning silicagel column reclaimed.
Green extraction process for artemisinin of the present invention is adopted to have following beneficial effect:
1, can effectively reduce production cost, increase economic efficiency
Usual sweet wormwood raw material only one month collection period, and processing period reaches 10 months, the raw material (water content 14%) purchased by state-promulgated pharmacopoeia standard is under field conditions (factors) more than 90 days, in raw material, artemislnin content can progressively decline, investigation record analysis through for many years proves, the major cause causing artemislnin content to decline is moisture content and temperature, wherein moisture content account for about 70%, temperature
Account for about 30%, in the raw material that (is generally June August to next year then) within a production cycle, the content of Artemisinin on average declines 20%, and Green extraction process for artemisinin of the present invention is provided with the step to raw material drying process, feed moisture content is made to drop to less than 7% with free of contamination raw material drying treatment process, delay the decline of raw material artemislnin content in stock, meanwhile, owing to extracting
Solvent is water-fast sherwood oil, sweet wormwood feed moisture content declines, sherwood oil can be improved and enter deal in sweet wormwood raw material, more Artemisinin in sweet wormwood raw material is made to be dissolved in sherwood oil, during as supposed that sweet wormwood raw material moisture content per ton is 14%, the Artemisinin in 140 ㎏ sweet wormwood raw materials is just had not extract in 1 ton of sweet wormwood raw material, when sweet wormwood raw material moisture content is 7%, the Artemisinin in 70 ㎏ sweet wormwood raw materials is just only had not extract in 1 ton of sweet wormwood raw material, sweet wormwood raw material per ton just can improve the utilization ratio of 70 ㎏ raw materials, the calculating of average artemislnin content 7 ‰ is put in storage with sweet wormwood material recall, traditional extraction technique 1 ton of sweet wormwood raw material can extract Artemisinin 4.2 ㎏, adopt green extraction process of the present invention 1 ton of sweet wormwood raw material can extract Artemisinin 5.33 ㎏ in theory, extraction yield is significantly improved, effectively can reduce production cost, increase economic efficiency.In addition, the sherwood oil after countercurrent extraction in remaining sweet wormwood slag is essentially completely recovered and step (4) recovery and reuse of waste reclaims sherwood oil, Herba Artemisiae Annuae oil from waste mother liquor, sweet wormwood is cured also can effectively increase economic efficiency.Green through statistical study Artemisinin of the present invention compared with traditional production technique
Look extraction process can make production cost can decline 1/3rd, and energy consumption reduces by 2/3rds, and the discharge of the three wastes reduces more than 3/4ths, has the economic results in society of aobvious chopsticks.
2, Artemisinin decomposes and affect the problem of yield in leaching process is solved
Artemisinin is heat-sensitive substance, and the Artemisinin not only in sweet wormwood raw material can decomposes under hot summer days hot conditionss, in leaching process warm-up time grown Artemisinin also can decomposes and affect yield.The present invention solves Artemisinin decomposes and affect the problem of yield in leaching process by shortening extraction time and control temperature technology: adopt countercurrent extraction technology to shorten batch 2 hours (1000 ㎏) extraction times, next selects the good low-boiling extraction solvent of quality, then controls Extracting temperature and delays Artemisinin decomposes speed and make Artemisinin yield to greatest extent not by too much influence.
3, energy-conservation, consumption reduction, clean, significantly reduce waste discharge
Solvent consumption index in traditional mode of production Artemisinin technique often produces one kilogram of Artemisinin to consume petroleum ether 36kg, acetone 2kg, wherein sherwood oil is taken away by residue and is consumed with tail gas volatilization in leaching process, takes away in the impurity process of acetone then in eluting silica gel post with silica gel.Green extraction process for artemisinin of the present invention adopts countercurrent extraction technology, reduce the consumption of sherwood oil, recovery part sherwood oil in step (4) recovery and reuse of waste, sherwood oil after countercurrent extraction in remaining sweet wormwood slag is also essentially completely recovered, therefore the consumption of sherwood oil significantly reduces, the present invention replaces the impurity in acetone eluting silica gel with the hot water reclaimed after sherwood oil eluting silica gel post in addition, no longer consume acetone, really accomplish energy-conservation, consumption reduction, cleaner production, also significantly can reduce waste discharge.
Below in conjunction with embodiment, Green extraction process for artemisinin of the present invention is further described.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment one:
Green extraction process for artemisinin of the present invention, this extraction process comprises the following steps:
(1) raw material drying process: (sweet wormwood raw material is firsthand medicinal plant Herba Artemisiae annuae by sweet wormwood raw material, water content is 14%) put in microwave energy saving drying plant and carry out drying treatment, in drying process, the temperature of microwave energy saving drying plant is set to 45 DEG C, the drying treatment time is 30 minutes, when reducing to 7% to sweet wormwood raw material moisture, take out the pack of sweet wormwood raw material, warehouse-in is preserved;
(2) the first system of Artemisinin: the sweet wormwood raw material l000kg after drying treatment in step (1) is put in extractor, close the dog-house of extractor, the fuel charging valve opening extractor adds sherwood oil in extractor, heating countercurrent extraction, it is 60 DEG C that temperature controls, in the present embodiment, heating countercurrent extraction need carry out 3 times, extraction time first time is 2 hours, second time extraction time is 1.5 hours, extraction time third time is 0.5 hour, after countercurrent extraction liquid and solvent oil being released extractor after countercurrent extraction completes, countercurrent extraction liquid is left standstill, after countercurrent extraction liquid and solvent oil are released extractor, close oil drain valve simultaneously, the steaming valve that rushes opening extractor carries out punching steaming to sweet wormwood slag, after the sherwood oil in sweet wormwood slag volatilizees recovery completely, sweet wormwood slag is discharged outside extractor, (impurity is mainly wax to the impurity treating in countercurrent extraction liquid, moisture etc.) get supernatant liquor and make it pass through silicagel column after precipitation, flow out stream part of silicagel column, part free from foreign meter direct back dissolving agent stock use again, impure part is by after concentration and recovery sherwood oil, gained concentrated solution is the material A containing Herba Artemisiae Annuae oil and sweet wormwood wax, material A stays subsequent handling for subsequent use, sherwood oil eluting silica gel post is used again after silicagel column is saturated, sherwood oil in the present embodiment for eluting silica gel post contains 5% ethyl acetate, collect from silicagel column de-come out containing Artemisinin stream part, be put in concentration tank concentrated by what collect containing Artemisinin stream part, when having crystal to separate out to concentration tank, again concentrated solution to be put to crystallizer crystallization 15 hours, during crystallization, crystallizer water coolant forces cooling to keep Tc to control at 25 DEG C, obtain crystal after being fallen by mother liquor suction filtration in concentration tank after crystallization completes, crystal is drying to obtain Artemisinin crude product, also collect in eluting silica gel post process flow out from silicagel column impure, not containing part stream part of Artemisinin composition, after concentration and recovery sherwood oil, gained concentrated solution is the material B containing Herba Artemisiae Annuae oil and sweet wormwood wax, material B stays subsequent handling for subsequent use, after above-mentioned sherwood oil eluting silica gel post, also comprise the technique with the hot water cleaning silicagel column reclaimed, have partial impurities not clean up, can be burnt completely by the impurity do not washed clean during silica gel activating with water cleaning silicagel column,
(3) Artemisinin is refining: the Artemisinin crude product obtained in step (2) is placed in Alcohol-settling tank and leaves standstill with after 60 times of 95% dissolve with ethanol, get supernatant liquor secondary filter, filtrate be placed in concentration tank be concentrated into original volume 1/3 after, standing spontaneous nucleation at normal temperatures 15 hours, crystal is obtained after being filtered by mother liquor after crystallization completes, crystal obtains Artemisinin fine work 5.33kg after vacuum drying treatment, (European Pharmacopoeia HPLC method is adopted to detect) after testing, in Artemisinin fine work, artemislnin content is 99.5%, related substances and clarity qualified, Artemisinin extraction yield is 85%, after the mother liquor that suction filtration goes out is concentrated into 1/3 of its volume again, standing spontaneous nucleation at normal temperatures 15 hours again, same method process mother liquor three to four times, gained crystal is Artemisinin crude product, Artemisinin crude product again in repeating step (3) the extracting method process of Artemisinin fine work obtain Artemisinin fine work,
(4) recovery and reuse of waste: the mother liquor that step (2) is leached and collect containing the material A of Herba Artemisiae Annuae oil and sweet wormwood wax and material B and be placed in extractor and be heated to 75 DEG C, the sherwood oil gasified is reclaimed by with the tank connected device of extraction, pure sherwood oil 20kg free from foreign meter can be obtained, residue mother liquor (containing Herba Artemisiae Annuae oil and sweet wormwood wax) passes through steam distillation again, the Herba Artemisiae Annuae oil gasified is reclaimed by with the tank connected device of extraction, obtain Herba Artemisiae Annuae oil 1.5kg, cool and collect remaining material sweet wormwood wax in extractor, obtain sweet wormwood wax 9kg, the sweet wormwood slag produced in step (2) is used for making fuel for coal after can utilize boiler exhaust gas drying in process of production, dry sweet wormwood slag per ton can replace 0.317 ton, raw coal after measured, substantially the heat energy needs of processing one ton of sweet wormwood raw material can be met, sweet wormwood slag burn later residual ash can do farm manure use.
Through statistical study, calculate with the average price of 2010, the traditional extraction technique sweet wormwood raw material output value=4.2kg × 2800 per ton yuan=11760 yuan.Adopt green extraction process of the present invention, after its Raw, dry technology makes raw material per ton have a net increase of 3084 yuan on year-on-year basis; Technique integrated innovation makes raw material per ton have a net increase of 255.12 yuan on year-on-year basis; Comprehensive utilization waste mother liquor and waste residue make raw material per ton have a net increase of 484 yuan on year-on-year basis, and three add up to 3793.12 yuan.To be equivalent in the traditional extraction technique raw material output value=4.2kg × 2800 per ton yuan=11760 yuan increase economic efficiency 32.25%.Add the labour cost of production capacity and the reduction increased thus, total production cost can decline more than one of three parts.
Above-mentioned data calculate according to method below:
(1) content that after raw material, dry technology delays sweet wormwood material inventory declines the benefit produced
Calculate with material recall warehouse-in average content 7 ‰, water content is the Artemisinin theoretical content of 1 ton of raw material of 14% is 7 ㎏, and before process, raw material per ton can receive Artemisinin=7 ㎏ × 80%(stock content decline 20%) × recovery rate 75%=4.2 ㎏; After process, feed moisture content per ton drops to 7% from 14%, be equivalent to be left 930kg after 70kg moisture content deducted by raw material per ton, but content is constant, still containing Artemisinin 7kg in 930kg raw material: the artemislnin content in other words after process in raw material per ton becomes 7 ㎏ ÷ 930kg=7.53 ‰ from 7 ‰.Theoretical content=7.53 ㎏ × 93%(stock content declines 7%) remain 7 ㎏; (in order to strengthen the convenience of comparability and cost keeping, after we still deduct moisture content 1 ton of raw material, remaining 930kg is considered as 1 ton);
In order to strengthen comparability, when traditional technology recovery rate 75% is constant, 1 ton of raw material can be received Artemisinin=7kg × 93%(stock content and decline 7% after drying treatment later) × recovery rate 75%=4.88 ㎏; But novel process is because decreasing the repulsion of water to oil after raw material drying, refluxing extraction is replaced again by countercurrent extraction, make extraction more fully more complete, so actual recovery rate is more than 85%, Artemisinin=7kg × 93%(stock content can be received and decline 7%) × recovery rate 85%=5.33 ㎏, increase 1.13 ㎏ than before process, increase income 3164 yuan by Artemisinin contract price per kilogram in 2010 2800 yuan, deduction drying cost 80 yuan has a net increase of 3084 yuan;
(2) by benefit that series of processes integrated innovation produces: by with the Wen equipment that returns of advanced person with often produce one kilogram of Artemisinin ether that consumes petroleum with water for ketone technology and be reduced to 20kg from 36kg, save sherwood oil 16 ㎏, save acetone 2 ㎏, be equivalent to raw material ratio traditional technology per ton and save sherwood oil=16 ㎏ × (5.33 ㎏-4.2 ㎏) × 9 Yuan/㎏=162 .72 unit, save Yuan/㎏=92.40 yuan, ㎏ × 11, ㎏ × 4.2, acetone=2, two add up to 255.12 yuan;
(3) economic benefit that waste mother liquor and waste residue produce is fully utilized: the recyclable 1.5kg Herba Artemisiae Annuae oil of mother liquor that sweet wormwood raw material per ton produces, the cured and 20kg sherwood oil of about 9kg sweet wormwood; By like product reference price: 1.5kg Herba Artemisiae Annuae oil × 150 yuan=225 yuan, 9kg sweet wormwood is cured × 3 yuan=27 yuan, 20kg sherwood oil × 9 yuan=180 yuan; Reduce cost recovery 240 yuan, rise in value 270 yuan; Utilize the dry sweet wormwood dregs of a decoction of boiler exhaust gas then for coal technology, dry sweet wormwood slag per ton can replace 0.44 ton, raw coal after measured, substantially can meet the heat energy needs of production one ton of sweet wormwood raw material; By raw coal valency 800 yuan per ton, dry sweet wormwood slag per ton is worth 352 yuan, deduction drying cost 60 yuan, and joint 292 yuan, two add up to 484 yuan.
Therefore, green extraction process of the present invention is adopted can effectively to reduce production cost, increase economic efficiency.
Table one is often produced a public jin Celadon artemisin for statistical analysis and is adopted friendly process of the present invention and traditional technology unit consumption of energy and roll over standard coal parameter below, calculate with material recall warehouse-in Ping Jun Celadon artemisin content 7 ‰, Artemisinin 4.2 ㎏ received by traditional processing technology raw material per ton; Artemisinin 5.33 ㎏ received by green extraction process raw material per ton.
Table one:
| Energy consumption project | Friendly process | Folding standard coal | Traditional technology | Folding standard coal | Signature coefficient |
| Unit power consumption | 34.52Kwh | 13.95㎏ | 43.81Kwh | 17.70㎏ | 0.404 |
| Unit water consumption | 2.25M 3 | 0.58 ㎏ | 2.86M3 | 0.74 ㎏ | 0.257 |
| Unit coal consumption | 31.52 ㎏ | 23.21 ㎏ | 144.76 ㎏ | 103.36 ㎏ | 0.714 |
| Sherwood oil consumes | 20.00㎏ | 28.80 ㎏ | 36.00 ㎏ | 51.84 ㎏ | 1.44 |
| Folding standard coal summation | 66.54 ㎏ | 173.64 ㎏ |
As seen from the above table: often produce a public jin Celadon artemisin, green extraction process reduces energy consumption folding standard coal 107.10 ㎏ than traditional processing technology, and energy consumption reduces by more than 2/3rds.
Significantly can reduce the environmental pollution that environmental pollution-than former technique reduces 3/4ths: green extraction process is often produced a Gong Jin Celadon artemisin and consumed raw coal 31.52 ㎏ (for silica gel activating), carbonic acid gas 2620 ㎏ is produced by often burn one ton of standard coal of Industrial Boiler, sulfurous gas 8.5 ㎏, oxynitride 7.4 ㎏. nest calculate, produce carbonic acid gas 82.58 ㎏, sulfurous gas 0.27 ㎏, oxynitride 0.23 ㎏., add up to 83.08 ㎏, add in residue sherwood oil 20 ㎏ totally 103.08 ㎏ taking away and burn; And traditional processing technology is often produced a Gong Jin Celadon artemisin and consumed raw coal 144.76 ㎏, the waste of generation is that 4.59 times of green extraction process reach 473.14 ㎏, adds sherwood oil 36 ㎏ totally 509.14 ㎏ taken away in residue.That is green extraction process is only 20.25% of traditional processing technology environmental, namely reduce 3/4ths close to 4/5ths environmental pollution.Therefore, green extraction process of the present invention is adopted really can to accomplish energy-conservation, consumption reduction, cleaner production, significantly reduce waste discharge.
Embodiment two:
The present embodiment technical process is identical with embodiment one, and only some processes parameter is different, Green extraction process for artemisinin of the present invention, and this extraction process comprises the following steps:
(1) raw material drying process: sweet wormwood raw material is put in microwave energy saving drying plant and carries out drying treatment, in drying process, the temperature of microwave energy saving drying plant is set to 60 DEG C, the drying treatment time is 35 minutes, when reducing to 6% to sweet wormwood raw material moisture, take out the pack of sweet wormwood raw material, warehouse-in is preserved;
(2) the first system of Artemisinin: the sweet wormwood raw material l000kg in (1) after drying treatment puts in extractor, close the dog-house of extractor, the fuel charging valve opening extractor adds sherwood oil in extractor, heating countercurrent extraction, it is 60 DEG C that temperature controls, in the present embodiment, heating countercurrent extraction need carry out 3 times, extraction time first time is 2.5 hours, second time extraction time is 1 hour, extraction time third time is 0.8 hour, after countercurrent extraction liquid and solvent oil being released extractor after countercurrent extraction completes, countercurrent extraction liquid is left standstill, after countercurrent extraction liquid and solvent oil are released extractor, close oil drain valve simultaneously, the steaming valve that rushes opening extractor carries out punching steaming to sweet wormwood slag, after the sherwood oil in sweet wormwood slag volatilizees recovery completely, sweet wormwood slag is discharged outside extractor, (impurity is mainly wax to the impurity treating in countercurrent extraction liquid, moisture etc.) get supernatant liquor and make it pass through silicagel column after precipitation, flow out stream part of silicagel column, part free from foreign meter direct back dissolving agent stock use again, impure part is by after concentration and recovery sherwood oil, gained concentrated solution is the material A containing Herba Artemisiae Annuae oil and sweet wormwood wax, material A stays subsequent handling for subsequent use, sherwood oil eluting silica gel post is used again after silicagel column is saturated, sherwood oil in the present embodiment for eluting silica gel post contains 8% ethyl acetate, collect from silicagel column de-come out containing Artemisinin stream part, be put in concentration tank concentrated by what collect containing Artemisinin stream part, when having crystal to separate out to concentration tank, again concentrated solution to be put to crystallizer crystallization 18 hours, during crystallization, crystallizer water coolant forces cooling to keep Tc to control at 20 DEG C, obtain crystal after being fallen by mother liquor suction filtration in concentration tank after crystallization completes, crystal is drying to obtain Artemisinin crude product, also collect in eluting silica gel post process flow out from silicagel column impure, not containing part stream part of Artemisinin composition, after concentration and recovery sherwood oil, gained concentrated solution is the material B containing Herba Artemisiae Annuae oil and sweet wormwood wax, and material B stays subsequent handling for subsequent use, after above-mentioned sherwood oil eluting silica gel post, also comprise the technique with the hot water cleaning silicagel column reclaimed, have partial impurities not clean up, can be burnt completely by the impurity do not washed clean during silica gel activating with water cleaning silicagel column,
(3) Artemisinin is refining: the Artemisinin crude product obtained in step (2) is placed in Alcohol-settling tank and leaves standstill with after 66 times of 93% dissolve with ethanol, get supernatant liquor secondary filter, filtrate be placed in concentration tank be concentrated into original volume 3/4 after, standing spontaneous nucleation at normal temperatures 18 hours, crystal is obtained after being filtered by mother liquor after crystallization completes, crystal obtains Artemisinin fine work 5.35kg after vacuum drying treatment, (European Pharmacopoeia HPLC method is adopted to detect) after testing, in Artemisinin fine work, artemislnin content is 99.6%, related substances and clarity qualified, Artemisinin extraction yield is 86.5%, after the mother liquor that suction filtration goes out is concentrated into 3/4 of its volume again, standing spontaneous nucleation at normal temperatures 18 hours again, same method process mother liquor three to four times, gained crystal is Artemisinin crude product, Artemisinin crude product again in repeating step (3) the extracting method process of Artemisinin fine work obtain Artemisinin fine work,
(4) recovery and reuse of waste: the mother liquor that step (2) is leached and collect containing the material A of Herba Artemisiae Annuae oil and sweet wormwood wax and material B and be placed in extractor and be heated to 75 DEG C, the sherwood oil gasified is reclaimed by with the tank connected device of extraction, pure sherwood oil 22kg free from foreign meter can be obtained, residue mother liquor (containing Herba Artemisiae Annuae oil and sweet wormwood wax) passes through steam distillation again, the Herba Artemisiae Annuae oil gasified is reclaimed by with the tank connected device of extraction, obtain Herba Artemisiae Annuae oil 1.8 kg, cool and collect remaining material sweet wormwood wax in extractor, obtaining sweet wormwood wax 8kg.
The present embodiment also can reach technique effect described in embodiment one, at this no longer repeated description.
Embodiment three:
The present embodiment technical process is identical with embodiment one, and only some processes parameter is different, Green extraction process for artemisinin of the present invention, and this extraction process comprises the following steps:
(1) raw material drying process: sweet wormwood raw material is put in microwave energy saving drying plant and carries out drying treatment, in drying process, the temperature of microwave energy saving drying plant is set to 65 DEG C, the drying treatment time is 25 minutes, when reducing to 5% to sweet wormwood raw material moisture, take out the pack of sweet wormwood raw material, warehouse-in is preserved;
(2) the first system of Artemisinin: the sweet wormwood raw material l000kg in (1) after drying treatment puts in extractor, close the dog-house of extractor, the fuel charging valve opening extractor adds sherwood oil in extractor, heating countercurrent extraction, it is 60 DEG C that temperature controls, in the present embodiment, heating countercurrent extraction need carry out 3 times, extraction time first time is 2 hours, second time extraction time is 1.5 hours, extraction time third time is 0.5 hour, after countercurrent extraction liquid and solvent oil being released extractor after countercurrent extraction completes, countercurrent extraction liquid is left standstill, after countercurrent extraction liquid and solvent oil are released extractor, close oil drain valve simultaneously, the steaming valve that rushes opening extractor carries out punching steaming to sweet wormwood slag, after the sherwood oil in sweet wormwood slag volatilizees recovery completely, sweet wormwood slag is discharged outside extractor, treat that the impurity in countercurrent extraction liquid (is mainly wax, moisture etc.) get supernatant liquor and make it pass through silicagel column after precipitation, flow out stream part of silicagel column, part free from foreign meter direct back dissolving agent stock use again, impure part is by after concentration and recovery sherwood oil, gained concentrated solution is the material A containing Herba Artemisiae Annuae oil and sweet wormwood wax, material A stays subsequent handling for subsequent use, sherwood oil eluting silica gel post is used again after silicagel column is saturated, sherwood oil in the present embodiment for eluting silica gel post contains 4% ethyl acetate, collect from silicagel column de-come out containing Artemisinin stream part, be put in concentration tank concentrated by what collect containing Artemisinin stream part, when having crystal to separate out to concentration tank, again concentrated solution to be put to crystallizer crystallization 20 hours, during crystallization, crystallizer water coolant forces cooling to keep Tc to control at 30 DEG C, obtain crystal after being fallen by mother liquor suction filtration in concentration tank after crystallization completes, crystal is drying to obtain Artemisinin crude product, also collect in eluting silica gel post process flow out from silicagel column impure, not containing part stream part of Artemisinin composition, after concentration and recovery sherwood oil, gained concentrated solution is the material B containing Herba Artemisiae Annuae oil and sweet wormwood wax, and material B stays subsequent handling for subsequent use, after above-mentioned sherwood oil eluting silica gel post, also comprise the technique with the hot water cleaning silicagel column reclaimed, have partial impurities not clean up, can be burnt completely by the impurity do not washed clean during silica gel activating with water cleaning silicagel column,
(3) Artemisinin is refining: the Artemisinin crude product obtained in step (2) is placed in Alcohol-settling tank and leaves standstill with after 75 times of 94% dissolve with ethanol, get supernatant liquor secondary filter, filtrate be placed in concentration tank be concentrated into original volume 1/3 after, standing spontaneous nucleation at normal temperatures 20 hours, crystal is obtained after being filtered by mother liquor after crystallization completes, crystal obtains Artemisinin fine work 5.45kg after vacuum drying treatment, (European Pharmacopoeia HPLC method is adopted to detect) after testing, in Artemisinin fine work, artemislnin content is 99.6%, related substances and clarity qualified, Artemisinin extraction yield is 88%, after the mother liquor that suction filtration goes out is concentrated into 1/3 of its volume again, standing spontaneous nucleation at normal temperatures 20 hours again, same method process mother liquor three to four times, gained crystal is Artemisinin crude product, Artemisinin crude product again in repeating step (3) the extracting method process of Artemisinin fine work obtain Artemisinin fine work,
(4) recovery and reuse of waste: the mother liquor that step (2) is leached and collect containing the material A of Herba Artemisiae Annuae oil and sweet wormwood wax and material B and be placed in extractor and be heated to 75 DEG C, the sherwood oil gasified is reclaimed by with the tank connected device of extraction, pure sherwood oil 25 kg free from foreign meter can be obtained, residue mother liquor (containing Herba Artemisiae Annuae oil and sweet wormwood wax) passes through steam distillation again, the Herba Artemisiae Annuae oil gasified is reclaimed by with the tank connected device of extraction, obtain Herba Artemisiae Annuae oil 1.5kg, cool and collect remaining material sweet wormwood wax in extractor, obtaining sweet wormwood wax 10kg.
The present embodiment also can reach technique effect described in embodiment one, at this no longer repeated description.
As conversion of the present invention: the present invention also can not comprise step (4), and only comprises step (1), (2), (3); Countercurrent extraction in step (2) is also not limited to comprise 3 extractions, also can suitably increase or reduce; The processing parameter of each step is also not limited to the value described in above-described embodiment, as long as conversion done within the scope of the present invention all belongs to category of the present invention.
Claims (1)
1. an extraction process for Artemisinin, is characterized in that, this extraction process comprises the following steps:
(1) raw material drying process: sweet wormwood raw material is put in microwave energy saving drying plant and carries out drying treatment, in drying process, the temperature of microwave energy saving drying plant is set to 50-70 DEG C, the drying treatment time is 30-40 minute, when reducing to 6-8% to sweet wormwood raw material moisture, take out the pack of sweet wormwood raw material, warehouse-in is preserved;
(2) the first system of Artemisinin: the sweet wormwood raw material after drying treatment in step (1) is put in extractor, close the dog-house of extractor, the fuel charging valve opening extractor adds sherwood oil in extractor, heating countercurrent extraction, temperature controls within the scope of 60-80 DEG C, after countercurrent extraction liquid is released extractor, extracting solution is left standstill, after the assorted precipitation in countercurrent extraction liquid, get supernatant liquor makes it pass through silicagel column, sherwood oil eluting silica gel post is used again after silicagel column is saturated, collection takes off and concentrates from silicagel column containing Artemisinin stream part and putting it in concentration tank of coming out, when having crystal to separate out to concentration tank, concentrated solution is put crystallization 18-24 hour to crystallizer, during crystallization, crystallizer water coolant forces cooling to keep Tc to control at 25 DEG C-35 DEG C, crystal is obtained after being filtered by mother liquor in concentration tank after crystallization completes, crystal is drying to obtain Artemisinin crude product,
(3) Artemisinin is refining: leave standstill after the Artemisinin crude product obtained in step (2) being placed in Alcohol-settling tank 60-70 times of 85-90% dissolve with ethanol, get supernatant liquor secondary filter, after filtrate is placed in concentration tank the 1/2-3/4 being concentrated into original volume, concentrated solution is put in crystallizer, leave standstill spontaneous nucleation 18-24 hour at normal temperatures, obtain crystal after being fallen by mother liquor suction filtration after crystallization completes, crystal obtains Artemisinin fine work after vacuum drying treatment.
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| CN105779129A (en) * | 2016-04-22 | 2016-07-20 | 四川蓝伯特生物科技有限责任公司 | Method for preparing Artemisia apiacea volatile oil from Artemisia apiacea waste mother liquor, method for preparing byproduct and obtained byproduct |
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| CN105779129A (en) * | 2016-04-22 | 2016-07-20 | 四川蓝伯特生物科技有限责任公司 | Method for preparing Artemisia apiacea volatile oil from Artemisia apiacea waste mother liquor, method for preparing byproduct and obtained byproduct |
| CN106496244A (en) * | 2016-08-31 | 2017-03-15 | 重庆华方武陵山制药有限公司 | A kind of method for extracting qinghaosu from the recrystallization mother liquor of production qinghaosu |
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| CN107827904A (en) * | 2017-11-17 | 2018-03-23 | 广西仙草堂制药有限责任公司 | A kind of purification process of qinghaosu |
| CN112979673A (en) * | 2021-02-26 | 2021-06-18 | 云南群优生物科技有限公司 | Extraction and purification method of artemisinin |
| CN113105947A (en) * | 2021-04-21 | 2021-07-13 | 禹州市天源生物科技有限公司 | Preparation method of sweet wormwood essential oil |
| CN114437869A (en) * | 2021-12-15 | 2022-05-06 | 河南天源药物研究有限公司 | Natural cool sweet wormwood essential oil and extraction process thereof |
| CN114231359A (en) * | 2021-12-23 | 2022-03-25 | 海南林鹏茶业有限公司 | Preparation method of agilawood extract |
| CN115466647A (en) * | 2022-08-12 | 2022-12-13 | 湖南斯依康生物科技有限公司 | Preparation method of itching-relieving essential oil |
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