CN208949164U

CN208949164U - A kind of system producing qinghaosu

Info

Publication number: CN208949164U
Application number: CN201821539174.5U
Authority: CN
Inventors: 张锁江; 张军平; 张梅香; 王慧; 张迎; 张永强
Original assignee: Institute of Process Engineering of CAS
Current assignee: Institute of Process Engineering of CAS
Priority date: 2018-09-19
Filing date: 2018-09-19
Publication date: 2019-06-07
Anticipated expiration: 2028-09-19

Abstract

The utility model discloses a kind of systems for producing qinghaosu, the system comprises recrystallization units, the recrystallization unit includes being sequentially connected composed filter device by pre-filter and refined filtration filter, the filter element aperture of the pre-filter is 1-10 μm, and the filter element aperture of the refined filtration filter is 0.1-1 μm.The system qinghaosu product recovery rate produced of production qinghaosu provided by the utility model is high, high-quality, and production procedure is simple, low energy consumption, production capacity is high, to enhance the competitiveness of enterprise.

Description

A kind of system producing qinghaosu

Technical field

The utility model belongs to substance extractive technique field, is related to a kind of system for producing qinghaosu.

Background technique

Qinghaosu is a kind of colourless acicular crystal extracted from compound inflorescence plant Artemisia annua, molecular formula C₁₅H₂₂O₅, It is a kind of sesquiterpene lactone containing peroxy-radical, is that World Health Organization's clear stipulaties replace the anti-malarial of quinine former Expect medicine.

Industrial production qinghaosu mainly extracts chrysanthemum mugwort with organic solvent at present, is separated by solid-liquid separation artemisia annua residue and obtains Extracting solution；Using macroreticular resin or the isolated qinghaosu product of silicagel column.The simple process is mature, and major defect is to mention It takes time length, low efficiency, energy consumption high, macroreticular resin or silicagel column is not reproducible utilizes.

103664988 A of CN discloses a kind of extraction separation method of qinghaosu, and this method includes (1) by raw medicinal material Chrysanthemum mugwort crushed after being dried；(2) reflux is carried out to material as solvent using the mixture of petroleum ether or industrial naptha or both to mention It takes twice, the volume mass ratio of solvent and material is 2:1-15:1 when extraction, extraction time 1-10 hour, to mentioning in extraction process Take tank carry out it is intermittent vacuumize and vacuum breaker, merge extracting solution twice and be concentrated, it is spare；(3) by the qinghaosu after concentration Extracting solution carries out silica gel column chromatography, is then eluted with the mixture of n-hexane and ether, and eluent is concentrated, decoloration, does Up to qinghaosu product after dry and crystallization.The problem of this method is primarily present includes: to be mentioned in extraction process using vacuum impulse formula It takes, operating process is complicated, and equipment cost is high, and vacuum energy consumption is high；Merge the quantity of solvent evaporated needed for extracting solution is concentrated twice Greatly, concentration section energy consumption is high, time-consuming；Silica gel column chromatography is assisted using ultrasonic wave in qinghaosu purification process, silicagel column can not Regeneration, ultrasonic wave operating cost are high.

104327092 A of CN discloses the method that qinghaosu is extracted from chrysanthemum wormwood, and this method utilizes supercritical CO₂ There is good dissolubility to qinghaosu, CO₂It is mixed in extractor with chrysanthemum wormwood, increases pressure and temperature to CO₂Liquid Change, extracts, qinghaosu dissolves in CO₂In, the CO containing qinghaosu₂Enter knockout drum after decompression, qinghaosu (and impurity) is dividing It separates and is precipitated from tank, CO₂It is sent into compressor cycle to use, extract carries out simple separation and purification and obtains qinghaosu sterling. But the procedure extraction tank operating pressure reaches 20MPa, and equipment investment is big, operating cost is high, production capacity is low.

101597296 A of CN discloses a kind of new method of efficiently extracting and producing artemisinin by ionic liquid, this method be by Artemisia annua raw material crushes, with the ultrasound-enhanced extraction of the mixed liquor of glyoxaline ion liquid halide salts and water, after solid-liquor separation Qinghaosu extracting solution；Extracting solution is extracted through organic extractant, obtains the extract liquor of enrichment qinghaosu；Evaporation recycling organic extraction Agent obtains qinghaosu crude product；High-purity qinghaosu is obtained by column chromatography, recrystallization etc. after the redissolution of qinghaosu crude product.Ionic liquid Body extracting solution is recycled, and is repeatedly regenerated after circulation with macroreticular resin.The problem of this method is primarily present includes: extraction process institute High-purity qinghaosu is obtained by column chromatography, recrystallization etc. after, qinghaosu crude product redissolution at high cost using ionic liquid, process is multiple Miscellaneous, the operation cycle is long, at high cost, there is solid waste generation.

1740176 A of CN disclose it is a kind of from sweet wormwood plant extract separation qinghaosu method, this method include with Lower process: the cauline leaf of sweet wormwood plant is crushed through pulverizer, 60-80 mesh powder of being sieved to obtain, in 40-60 DEG C of drying；It is dry Powder afterwards, it is 30-60 DEG C of petroleum ether that fraction, which is added, in the ratio of 50-70mL/g, 20-35 DEG C immersion 3-4 hours, Zhi Hou 48-52 DEG C of constant temperature and under the conditions of being 800-1000r/min agitating and heating with mixing speed, obtains extracting solution, and extracting solution is cooling To room temperature, filtering；Filtrate is subjected to alkali cleaning with 1.8-2.5wt%NaOH solution, and discards lower layer's lye, then wash with deionization To neutrality；Extracting solution after washing rotary evaporation under the conditions of 48-50 DEG C, obtains qinghaosu medicinal extract, the recycled solvent steamed. Need to carry out first extracting solution cooling in this method, alkali cleaning, washing obtain extracting solution, then obtain medicinal extract, process through rotary evaporation Complexity, unit capacity is small, waste liquid (spent lye and waste water) discharge amount is big.

Utility model content

In view of the deficienciess of the prior art, the purpose of this utility model is to provide a kind of system for producing qinghaosu and Method, the system equipment is at low cost, and production procedure is simple and strong operability, passes through using the method for the system production qinghaosu Impurity contained by high efficiency of helping and the qinghaosu product of production is few, with high purity.

For this purpose, the utility model uses following technical scheme:

A kind of system producing qinghaosu, including recrystallization unit, the recrystallization each unit includes filter device, described Filter device includes pre-filter and the refined filtration filter connecting with pre-filter.

Pre-filter and refined filtration filter fits can remove the impurity after dissolution qinghaosu crude product in acquired solution, Solves the problems, such as impurity effect product quality.

The filter element aperture of the pre-filter is 1-10 μm, such as can be 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μ M, 8 μm or 9 μm etc., preferably 2-6 μm.

If the filter element aperture of pre-filter is excessive, obtained by cannot effectively removing after dissolution qinghaosu crude product Impurity in solution will appear the phenomenon that filter element is easy blocking if the filter element aperture of pre-filter is too small, Therefore the filter element aperture for the pre-filter that the utility model uses is 1-10 μm.

The filter element aperture of the refined filtration filter is 0.1-1 μm, such as can be 0.2 μm, 0.3 μm, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm or 0.9 μm etc., preferably 0.2-0.6 μm.

If the filter element aperture of refined filtration filter is excessive, obtained by cannot effectively removing after dissolution qinghaosu crude product Impurity in solution will appear the phenomenon that filter element is easy blocking if the filter element aperture of refined filtration filter is too small, Therefore the filter element aperture for the refined filtration filter that the utility model uses is 0.1-1 μm.

The pre-filter and refined filtration filter independently include candle filter and/or bag filter, this field Technical staff it is to be understood that filter element reaches the pre-filter that above-mentioned technique requires and refined filtration filter is included in this In the technical proposal scope of utility model.

Preferably, the number of the pre-filter is 1-3, such as can be 1,2 or 3, preferably 1, Multiple pre-filters can be improved the rejection of impurity in acquired solution after dissolution qinghaosu crude product, but will increase equipment at This, is unfavorable for industrial application, therefore the utility model uses the number of the pre-filter a for 1-3, the technology of this field Personnel can reasonably be selected in the range of technical solution provided by the utility model.

Preferably, the number of the refined filtration filter is 1-3, such as can be 1,2 or 3, preferably 1, Multiple refined filtration filters can be improved the rejection of impurity in acquired solution after dissolution qinghaosu crude product, but will increase equipment at This, is unfavorable for industrial application, therefore the utility model uses the number of the refined filtration filter a for 1-3, the technology of this field Personnel can reasonably be selected in the range of technical solution provided by the utility model.

Preferably, the recrystallization unit further includes dissolver and the first crystallization apparatus, the dissolver, filtering dress It sets and is sequentially connected with the first crystallization apparatus.

Preferably, the recrystallization unit further includes recrystallization solvent recyclable device, the recrystallization solvent recyclable device Inlet be connected with the liquid outlet of the first crystallization apparatus, the outlet of the recrystallization solvent of the recrystallization solvent recyclable device with it is molten The feed inlet for solving device is connected.Recrystallization solvent after the recovery returns to dissolution equipment, recycles, so that it is molten to improve recrystallization The utilization rate of agent, has saved cost, improves economic benefit.

Preferably, the dissolver, the first crystallization apparatus and recrystallization solvent recyclable device have been provided independently from stirring Module and/or heating module, mass transport process can be accelerated by stirring module and/or heating module, shortened the operating time, improved production Efficiency, those skilled in the art can reasonably be selected according to process requirement.

Preferably, first crystallization apparatus includes the first crystallizer and the first solid-liquid separator.

Preferably, first crystallizer includes crystallization kettle.

Preferably, first solid-liquid separator includes centrifuge, and centrifuge can be rapidly separated by solid-liquid separation, and is reduced The residual of qinghaosu product surface recrystallization solvent improves the purity of qinghaosu product.

The system of the production qinghaosu further includes extraction unit, upgrading unit, extraction cells and crystalline element；It is described to mention Unit, upgrading unit, extraction cells, crystalline element and recrystallization unit is taken to be sequentially connected.

Preferably, the discharge port of the extraction unit is also connected with the feed inlet of extraction unit.

Preferably, the extraction unit includes the extraction element for being provided with blender and/or external liquid circulation, the setting There is the extraction element of blender and/or external liquid circulation to can be improved mass transfer velocity, shorten the time of extraction, improves the effect of extraction Rate.

Preferably, the upgrading unit includes primary concentration device and the secondary concentration connecting with primary concentration device dress It sets；

Preferably, the steam (vapor) outlet of the upgrading unit is connected with the feed inlet of the extraction element, upgrading unit concentration The first extractant can return to extraction element, for extracting the qinghaosu in qinghaosu raw material, to improve the first extraction The utilization rate of agent, has achieved the purpose that energy-saving and emission-reduction, improves economic benefit.

Preferably, the discharge port of the extraction cells is also connected with the feed inlet of extraction cells.

Preferably, the extraction cells include extraction equipment.

Preferably, the crystalline element includes the second crystallizer and the second solid-liquid separator for connecting with the second crystallizer.

Preferably, second crystallizer includes equipment of crystallisation by cooling.

Preferably, second solid-liquid separator includes the solid-liquid separating equipment with driving force, preferably centrifuge, Make to improve artemislnin content in crude product in solid qinghaosu and the wax oil split-phase in liquid under the action of centrifugal force, Recrystallization number is reduced, the operation cycle is shortened, saves consumption.It solves during typical filter separates solid-liquid and (such as uses vacuum Suction filtration machine, filter press etc.) wax oil the problem of being easily coated on qinghaosu surface and reducing artemislnin content in crude product.

Preferably, the system of the production qinghaosu further includes disposing mother liquor unit, the feed inlet of disposing mother liquor unit with The liquid outlet of crystalline element is connected.

Preferably, the disposing mother liquor unit includes mixing arrangement, extractant recyclable device and extracting agent recovery device；Institute The arrival end of the arrival end and extracting agent recovery device of stating extractant recyclable device is connect with the outlet end of the mixing arrangement.

Preferably, the outlet end of the extractant recyclable device is connect with the arrival end of the mixing arrangement, therefore, is extracted The extractant recycled in agent recyclable device can return in mixing arrangement the recycling for being used for qinghaosu crude product mother solution, to improve The utilization rate of second extractant.

Preferably, the extractant recyclable device further includes the by-product output that extractant recyclable device bottom is arranged in End.

Preferably, the outlet end of the extracting agent recovery device is connect with the arrival end of the extraction equipment, therefore, extraction The extractant recycled in agent recyclable device can return in extraction equipment the extraction for being used for the extract containing qinghaosu, to improve The utilization rate of extractant.

Preferably, the outlet end of the extractant recyclable device and the outlet end of extracting agent recovery device are separately set It sets at the top of the extractant recyclable device and extracting agent recovery device.

Preferably, the mixing arrangement, extractant recyclable device and extracting agent recovery device have been provided independently from stirring mould Block and/or heating module, those skilled in the art is it is to be understood that stirring module and/or heating module can be improved mass transfer speed Degree reduces the operating time, improves production efficiency.

Preferably, upgrading unit is set between the extraction unit and extraction cells of the system of the production qinghaosu.

Preferably, the primary concentration device includes thin film evaporator, thin film evaporator big, heat transfer efficiency with treating capacity The high, advantages such as evaporation rate is fast, residence time of material is short, the utility model is using thin film evaporator as primary concentration device energy Enough total times for shortening concentration.

Preferably, the thin film evaporator includes falling film evaporator or luwa evaporator, preferably luwa evaporator, ability The technical staff in domain is it is to be understood that there may be artemisia annua particle in the extract containing qinghaosu, common thin film evaporator holds Easily there is particle wall sticking phenomenon and influence evaporation efficiency, and luwa evaporator can be avoided particle and glue wall to improve concentration effect Rate.

Preferably, the quantity of the primary concentration device is 1-3, such as can be 1,2 or 3, preferably 1 A, multiple primary concentration devices can be improved the speed of concentration, but will increase equipment cost, therefore the utility model uses The number of primary concentration device be 1-3, those skilled in the art can be in technical solution provided by the utility model It is reasonably selected in range.

Preferably, the secondary concentration device includes concentration kettle or Rotary Evaporators, preferably concentration kettle, and concentration kettle has The first extractant for not having concentration in primary concentration device can be carried out concentration and recovery by general applicability.

Preferably, the quantity of the secondary concentration device is 1-3, such as can be 1,2 or 3, preferably 1 A, multiple secondary concentration devices can be improved the speed of concentration, but will increase equipment cost, therefore the utility model uses The number of primary concentration device is 1-3, and those skilled in the art can be in the model of technical solution provided by the utility model It encloses and interior is reasonably selected.

It is excellent that the setting of upgrading unit described in the utility model has that high production efficiency, treating capacity are big and the operating time is short etc. Gesture.

It is described production qinghaosu system production qinghaosu method the following steps are included:

(1) qinghaosu in qinghaosu raw material is extracted using the first extractant, obtains the extract containing qinghaosu；

(2) extracting solution containing qinghaosu is concentrated, obtains medicinal extract；

(3) qinghaosu in extract is extracted, the extract liquor containing qinghaosu is obtained；

(4) it by extract liquor crystallisation by cooling, is separated by solid-liquid separation, obtains qinghaosu crude product and qinghaosu crude product mother solution；

(5) the qinghaosu crude product is dissolved, filtering, recrystallization and separation of solid and liquid obtain qinghaosu product and recrystallization Mother liquor.

Wherein, the filtering includes by-pass filtration processing and secondary filtration processing, and by-pass filtration handles filter device therefor Filter element aperture is 1-10 μm, such as can be 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm or 9 μm etc., preferably 2-6 μ M, secondary filtration handle filter device therefor filter element aperture be 0.1-1 μm, such as can be 0.2 μm, 0.3 μm, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm or 0.9 μm etc., preferably 0.2-0.6 μm.

If the filter element aperture of pre-filter is excessive, obtained by cannot effectively removing after dissolution qinghaosu crude product Impurity in solution will appear the phenomenon that filter element is easy blocking if the filter element aperture of pre-filter is too small, Therefore the filter element aperture for the pre-filter that the utility model uses is 1-10 μm.If the filter element of refined filtration filter Aperture is excessive, the impurity after dissolving qinghaosu crude product in acquired solution cannot be effectively removed, if the mistake of refined filtration filter It is too small to filter component aperture, then will appear the phenomenon that filter element is easy blocking, therefore the refined filtration filter that the utility model uses Filter element aperture be 0.1-1 μm.

Step (1) the qinghaosu raw material is selected from artemisia annua, preferably artemisia annua powder.

Preferably, the granularity of the artemisia annua powder is 10-80 mesh, such as can be 20 mesh, 30 mesh, 40 mesh, 50 mesh, 60 Mesh or 70 mesh etc., preferably 20-60 mesh.

Preferably, the water content of the artemisia annua powder be less than 1wt ‰, such as can be 0.1wt ‰, 0.2wt ‰, 0.4wt ‰, 0.6wt ‰, 0.8wt ‰ or 0.9wt ‰ etc..

Preferably, in the artemisia annua powder qinghaosu content be 0.8-1.6wt%, such as can be 1.0wt%, 1.2wt% or 1.4wt% etc., preferably 1.0-1.4wt%.

Those skilled in the art is it is to be understood that any qinghaosu raw material that can extract qinghaosu is included in this technology In the range of scheme.

Preferably, step (1) first extractant includes any in methanol, ethyl alcohol, ether, petroleum ether or isohexane It is a kind of or at least two combination, typical but non-limiting group is combined into methanol and ethyl alcohol, methanol and ether, ethyl alcohol and ether, Ethyl alcohol and petroleum ether, ethyl alcohol, ether and isohexane, methanol, ethyl alcohol, ether, petroleum ether and isohexane, those skilled in the art It is to be understood that technical solution provided by the utility model is not limited to above-mentioned solvent, it can be to the solvent that qinghaosu extracts all It is included in the range of technical solution provided by the utility model.

Preferably, the volume mass ratio of step (1) first extractant and qinghaosu raw material is 5-30mL/g, such as can To be 10mL/g, 15mL/g, 20mL/g or 25mL/g etc., preferably 10-20mL/g.When the dosage of first extractant is lower, nothing Method sufficiently extracts the qinghaosu in qinghaosu raw material, when the dosage of the first extractant is higher, will increase the place of subsequent process steps Cost is managed, therefore the utility model uses the volume mass ratio of the first extractant and qinghaosu raw material for 5-30mL/g, this field Technical staff can reasonably be selected according to process requirement.

Preferably, the number of step (1) described extraction is 1-5 times, such as to can be 2 times, 3 times or 4 inferior, preferably 3 It is secondary.

Preferably, the specific steps of the extraction include: and extract the obtained extracting solution containing qinghaosu for the first time to carry out It operates in next step, the qinghaosu raw material after being extracted using the first new extractant to first time carries out second obtaining after extracting Extracting solution containing qinghaosu return to extraction step, the utilization rate of the first extractant can be improved in this way, increase economic efficiency.

Preferably, the temperature of step (1) described extraction be 40-70 DEG C, such as can be 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C or 65 DEG C etc., preferably 45-60 DEG C, when temperature is lower, the first extractant extract qinghaosu raw material in qinghaosu spend the time compared with It is long, it is unfavorable for shortening the production cycle, and qinghaosu is heat-sensitive substance, in order to guarantee product quality, sweet wormwood when should ensure that extraction The operation temperature of plain raw material is lower than 70 DEG C, therefore the temperature of extraction that uses of the utility model is 40-70 DEG C, the technology of this field Personnel can reasonably be selected according to process requirement.

Preferably, step (1) can also obtain the sweet wormwood slag not dissolved by the first extractant, and the sweet wormwood slag can be used as solid Fluid fuel or animal feed, to improve the economic benefit of enterprise.

Preferably, the first extractant obtained after the extracting solution concentration containing qinghaosu is used for by step (2) concentration The qinghaosu extracted in artemisia annua powder has saved cost to improve the utilization rate of the first extractant, improves economic effect Benefit.

Preferably, step (3) extractant used that extracts includes methanol aqueous solution and/or ethanol water.

Preferably, the water content of the extractant be 20-50wt%, such as can be 25wt%, 30wt%, 35wt%, 40wt% or 45wt% etc., preferably 30-40wt%.

Preferably, the volume mass ratio of the extractant and extract of step (3) described extraction is 3-20mL/g, such as can be with It is 5mL/g, 8mL/g, 10mL/g, 12mL/g, 15mL/g or 18mL/g etc., preferably 10-20mL/g, the dosage of extractant is lower When, it is unable to fully extract the extract containing qinghaosu, when the dosage of extractant is higher, will increase being processed into for subsequent process steps This, therefore the volume mass ratio of the extractant that uses of the utility model and the extract containing qinghaosu is 3-20mL/g, this field Technical staff can reasonably be selected according to process requirement.

Preferably, the temperature of step (3) described extraction be 40-70 DEG C, such as can be 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C or 65 DEG C etc., preferably 50-60 DEG C, when temperature is lower, the qinghaosu in extractant extracting artemisine raw material spends the time longer, no Conducive to the shortening production cycle, and qinghaosu is heat-sensitive substance, in order to guarantee product quality, qinghaosu raw material when should ensure that extraction Operation temperature be lower than 70 DEG C, therefore the temperature of extraction that the utility model uses is 40-70 DEG C, those skilled in the art can Reasonably to be selected according to process requirement.

Preferably, the time of step (3) described extraction be 10-60min, such as can be 20min, 30min, 40min or 50min etc., preferably 30-50min, when extraction time is shorter, extractant can not sufficiently extract from the extract containing qinghaosu Qinghaosu is taken, when extraction time is longer, the extraction yield of qinghaosu is increased speed slowly, it is unfavorable for shortening the production cycle, because The time for the extraction that this utility model uses, those skilled in the art can close according to process requirement for 10-60min The selection of reason ground.

Preferably, the number of step (3) described extraction is 1-5 times, such as can be 2 times, 3 times or 4 times, preferably 3 times.

Preferably, the specific steps of the extraction are as follows: the extract liquor containing qinghaosu being obtained by extraction for the first time carries out down Single stepping contains qinghaosu to what medicinal extract extracted for the first time carried out second obtaining after extracting using new extractant Extracting solution return to extraction step and be used to extract qinghaosu in medicinal extract, improve the utilization rate of extractant in this way, reduce cost, It increases economic efficiency, to improve enterprise competitiveness.

Preferably, step (3) extraction is not extracted the extract remainder of agent dissolution also, and the extract remainder is used to prepare Veterinary drug improves economic benefit.

Preferably, step (4) crystallization includes crystallisation by cooling, and the temperature of the crystallisation by cooling is preferably 3-30 DEG C, example It such as can be 5 DEG C, 10 DEG C, 15 DEG C, 20 DEG C or 25 DEG C, further preferably 5-15 DEG C, when the temperature of crystallisation by cooling is lower, tie The crystal quality of brilliant gained qinghaosu crude product is bad, it is also possible to include impurity；When the temperature of crystallisation by cooling is higher, crystallization Time can accordingly extend, be unfavorable for shorten the production cycle, therefore the utility model use the 3-30 DEG C of temperature as crystallisation by cooling Degree, those skilled in the art can reasonably be selected according to the technological requirements.

Preferably, the time of step (4) described crystallization is 1-8h, such as can be 2h, 3h, 4h, 5h, 6h or 7h, preferably For 3-6h, when the time of crystallization is shorter, qinghaosu crude product can not fully be crystallized out from the extract liquor containing qinghaosu, In the time of crystallization provided by the utility model, qinghaosu can obtain more fully crystallizing, and the time for extending crystallization will not Significantly improve the extraction yield of qinghaosu, thus time of crystallization that the utility model uses for 1-8h, those skilled in the art It can reasonably be selected according to process requirement.

Preferably, step (4) separation of solid and liquid carries out on centrifuge, and the revolving speed of the centrifuge is 2000- 15000r/min, such as can be 2000r/min, 3000r/min, 4000r/min, 5000r/min, 6000r/min, 7000r/ min、8000r/min、9000r/min、10000r/min、11000r/min、12000r/min、13000r/min、14000r/ Min or 15000r/min, preferably 4000-12000r/min.

For those skilled in the art it is to be understood that the revolving speed of centrifuge is faster, the effect of separation of solid and liquid is better, it is possible to reduce The number of recrystallization, but the equipment cost of high speed centrifuge is high, is unfavorable for economic benefit.The utility model selects centrifuge to make For the technical solution of separation of solid and liquid, overcomes and uses silica gel post separation bring problem of environmental pollution in state of the art, It is environmentally protective.

Preferably, the time of step (4) described separation of solid and liquid is 2-10min, preferably 4-6min.

The revolving speed for the centrifuge that the utility model is selected and the time of separation of solid and liquid cooperate, and can not only reach solid-liquid point From technical effect, additionally it is possible to save the cost reduces the number of recrystallization, improves production efficiency.

Preferably, step (5) solvent used that dissolves includes anhydrous methanol and/or dehydrated alcohol.

Preferably, the temperature of step (5) described dissolution is 20-70 DEG C, such as can be 30 DEG C, 40 DEG C, 50 DEG C or 60 DEG C Deng, preferably 30-60 DEG C, when temperature is lower, the dissolution time of qinghaosu crude product is longer, it is unfavorable for shortening the production cycle, and it is green Artemisin is heat-sensitive substance, and in order to guarantee product quality, the operation temperature of qinghaosu raw material is lower than 70 DEG C when should ensure that extraction, because For 20-70 DEG C, those skilled in the art can close the temperature for the dissolution that this utility model uses according to process requirement The selection of reason ground.

Preferably, steam or hot water heating are used when step (5) described dissolution, external heat source can accelerate the speed of dissolution Degree improves production efficiency.

Preferably, the volume mass ratio of step (5) recrystallization solvent and qinghaosu crude product is 5-50mL/g, such as can To be 10mL/g, 15mL/g, 20mL/g, 25mL/g, 30mL/g, 35mL/g, 40mL/g or 45mL/g etc., preferably 10-40mL/ g.When the dosage of recrystallization solvent is lower, it is unable to fully dissolution qinghaosu crude product, when the dosage of recrystallization solvent is higher, will increase The processing cost of subsequent process steps, thus the utility model use the volume mass ratio of recrystallization solvent and qinghaosu crude product for 5-30mL/g, those skilled in the art can reasonably be selected according to process requirement.

Preferably, the temperature of step (5) described recrystallization be 3-30 DEG C, such as can be 5 DEG C, 10 DEG C, 15 DEG C, 20 DEG C or 25 DEG C, preferably 5-15 DEG C.When the temperature of recrystallization is lower, the crystal quality of recrystallization gained qinghaosu product is bad, It may include the impurity that other are dissolved in recrystallization solvent；When increasing the temperature of recrystallization, the time meeting of recrystallization It is corresponding to extend, it is unfavorable for shortening the production cycle, therefore the utility model uses the 3-30 DEG C of temperature as recrystallization, this field Technical staff can reasonably be selected according to the technological requirements.

Preferably, the time of step (5) described recrystallization is 1-8h, such as can be 2h, 3h, 4h, 5h, 6h or 7h, excellent It is selected as 3-6h.When the time of recrystallization is shorter, what qinghaosu product was unable to fully ties from the recrystallization solution containing qinghaosu Crystalline substance comes out, and within the time of recrystallization provided by the utility model, qinghaosu product can obtain more adequately crystallizing, and extends The time of recrystallization will not significantly improve the extraction yield of qinghaosu, therefore time of recrystallization that the utility model uses is 1- 8h, those skilled in the art can reasonably be selected according to process requirement.

Preferably, the method for the production qinghaosu further includes the steps that carrying out (c) after step (5): recycling recrystallization Solvent in mother liquor.

Preferably, the solvent in recrystallization mother liquor is recycled by the way of evaporation, the temperature of the evaporation is 40-70 DEG C, Such as can be 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C or 65 DEG C etc., preferably 50-70 DEG C.When the temperature of evaporation is lower, recrystallization The recovery time of solvent in mother liquor can be longer, is unfavorable for improving operating efficiency, shortens the production cycle；When the temperature of evaporation is higher When, it is unfavorable for recycling for the recrystallization solvent of recycling, therefore the utility model takes the 40-70 DEG C of temperature as evaporation, Those skilled in the art, which can according to need, reasonably to be selected.

Preferably, it is molten to improve recrystallization for dissolving qinghaosu crude product for the solvent in the recrystallization mother liquor of the recycling The utilization rate of agent, improves economic benefit.

Step (2) concentration includes heating concentration.Heating concentration can shorten the time of concentration, shorten the production cycle, It increases economic efficiency.

Preferably, step (2) concentration includes primary concentration processing and secondary concentration processing, the primary concentration processing It is carried out on thin film evaporator, the secondary concentration processing carries out in concentration kettle and/or Rotary Evaporators, is preferably concentrated Kettle.

Thin film evaporator has the advantages such as treating capacity is big, heat transfer efficiency is high, evaporation rate is fast, residence time of material is short, this Utility model can shorten the total time of concentration using thin film evaporator as primary concentration device；Concentration kettle and/or rotation are steamed Sending out instrument has general applicability, the first extractant for not having concentration in primary concentration device can be carried out concentration and recovery, ability The technical staff in domain can reasonably be selected according to the technological requirements.

Preferably, in extracting solution of the primary concentration processing removal containing qinghaosu 40-90% extractant, such as can be with It is 50%, 60%, 70% or 80%, preferably 60-90%；Secondary concentration is handled the extractant in the extracting solution containing qinghaosu Evaporating completely.

Preferably, step (2) thickening temperature is 40-70 DEG C, such as can be 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C or 65 DEG C, preferably 50-60 DEG C.When thickening temperature is lower, the time of concentration is longer, is unfavorable for improving operating efficiency, shortens production Period；When thickening temperature is higher, the quality of qinghaosu product can be destroyed, therefore 40-70 DEG C of the utility model selection is as dense Contracting temperature, those skilled in the art can reasonably be selected according to process requirement.

Preferably, the extractant recycling that the primary concentration device and the concentration of secondary concentration device are fallen is in step (1) Extraction, this improves the utilization rate of the first extractant, improves economic benefit.

The method of the production qinghaosu further includes the steps that after step (4) (b): in recycling qinghaosu crude product mother solution Extractant.

Preferably, the extractant that recycling qinghaosu promotees in product mother liquor specifically includes: extracting the blueness using the second extractant Artemisin crude product mother solution, separation, obtains the second extractant containing wax oil and the extractant containing extract, and second containing wax oil Extractant isolates the second extractant and by-product wax oil through evaporation, and the extractant containing extract isolates extraction through distillation Agent.

Preferably, second extractant include in methanol, ethyl alcohol, ether, petroleum ether or isohexane any one or At least two combination, typical but non-limiting group is combined into methanol and ethyl alcohol, methanol and ether, ethyl alcohol and ether, ethyl alcohol and Petroleum ether, ethyl alcohol, ether and isohexane, methanol, ethyl alcohol, ether, petroleum ether and isohexane, those skilled in the art should know Dawn, technical solution provided by the utility model are not limited to above-mentioned solvent.

Preferably, the volume ratio of second extractant and qinghaosu crude product mother solution is 1:(0.5-3), such as can be 1: 1,1:1.5,1:2 or 1:2.5 etc., preferably 1:(1-2), when the dosage of the second extractant is less, the second extractant cannot have The wax oil that effect ground extracts in qinghaosu crude product mother solution will increase the processing of subsequent technique when the dosage of the second extractant is too many Cost, therefore the utility model uses the volume ratio of the second extractant and qinghaosu crude product mother solution for 1:(0.5-3), this field Technical staff can reasonably be selected according to process requirement.

Preferably, the extractant return step (3) isolated of distilling is used to extract the qinghaosu in extract, in this way The utilization rate for improving extractant, reduces production cost, improves economic benefit.

Preferably, the second obtained extractant that evaporates improves second for recycling qinghaosu crude product mother solution in this way The utilization rate of extractant, reduces production cost, improves economic benefit.

As the optimal technical scheme of the utility model, the utility model provides the system using the production qinghaosu The method for producing qinghaosu, described method includes following steps:

(1) under the conditions of 40-70 DEG C, the qinghaosu in artemisia annua powder is extracted using the first extractant, is obtained containing qinghaosu Extracting solution, the content of qinghaosu is 0.8-1.6wt% in the artemisia annua powder, and the granularity of artemisia annua powder is 10-80 mesh, Water content is less than 1wt ‰, and the volume mass ratio of the first extractant and artemisia annua powder is 5-30mL/g；The number of the extraction is extremely It is 2 times less, and extracts the obtained extract containing qinghaosu for the first time and carry out next step operation, is obtained after second of extraction Extract containing qinghaosu return to extraction step；

(2) under the conditions of 40-70 DEG C, the extractant of 40-90% in extracting solution of the removal containing qinghaosu is handled through primary concentration, Later under the conditions of 40-70 DEG C, handles through secondary concentration by extractant evaporating completely remaining in the extracting solution containing qinghaosu, obtain To medicinal extract, the extractant that the primary concentration processing is fallen with secondary concentration processing concentration is used for step (1) described extraction artemisia annua Qinghaosu in powder；

(3) under the conditions of 40-70 DEG C, the methanol aqueous solution for being 20-50wt% with water content and/or ethanol water extraction are soaked Cream obtains the extract liquor and extract remainder containing qinghaosu, the volume mass of the methanol aqueous solution and/or ethanol water and medicinal extract Than for 3-20mL/g, extraction time 10-60min；The number of the extraction is at least 2 times, and what is be obtained by extraction for the first time contains There is the extract liquor of qinghaosu to carry out next step operation, the extract liquor containing qinghaosu obtained after second of extraction is for extracting Qinghaosu in extract；

(4) extract liquor containing qinghaosu is crystallized into 1-8h under the conditions of 3-30 DEG C, be separated by solid-liquid separation, obtain qinghaosu crude product and Qinghaosu crude product mother solution；

(5) the qinghaosu crude product mother solution is extracted using the second extractant, separation obtains the second extractant containing wax oil With the extractant containing extract, the second extractant containing wax oil isolates the second extractant through evaporation, contains extract Extractant obtains extractant through distillation；The extractant return step (2) isolated of distilling is used to extract the blueness in extract Artemisin；The second obtained extractant that evaporates is for recycling qinghaosu crude product mother solution；

(6) qinghaosu crude product is dissolved using methanol and/or ethyl alcohol, the solution after making dissolution qinghaosu crude product passed sequentially through The pre-filter that component aperture is 1-10 μm and the refined filtration filter that filter element aperture is 0.1-1 μm are filtered, filtrate is obtained, it Filtrate is recrystallized under conditions of 3-30 DEG C afterwards, is separated by solid-liquid separation, obtains qinghaosu product and recrystallization mother liquor, the recrystallization Time is 1-8h, and the volume mass ratio of methanol and/or ethyl alcohol and qinghaosu crude product is 5-50mL/g；

(7) recrystallization mother liquor is evaporated under the conditions of 40-70 DEG C, the Steam Recovery that will be obtained；After the steam condensation of the recycling Dissolution for qinghaosu crude product；

Wherein, step (5) and step (6) are without sequencing.

System described in the utility model refers to apparatus system, is the set of each device or equipment.

Compared with prior art, the utility model has the following beneficial effects:

(1) the qinghaosu product purity that the system of production qinghaosu provided by the utility model obtains is higher than 99%, and again Crystallisation times are low, simple production process, improve the rate of recovery of qinghaosu, reduce production cost, improve the competition of enterprise Power；

(2) the disposing mother liquor unit in the system of production qinghaosu provided by the utility model can obtain byproduct wax Oil, the raffinate phase that extraction cells obtain may be used as veterinary drug, and the sweet wormwood slag that extraction unit obtains can be used for solid fuel or dynamic Object feed, this all improves the utilization rate of the qinghaosu raw material, improves the economic benefit of enterprise；

(3) system of production qinghaosu provided by the utility model improves extractant, extractant and recrystallization solvent Utilization rate, it is environmentally protective, reduce production cost.

Detailed description of the invention

Fig. 1 is the qinghaosu product manufacturing process schematic diagram of the utility model.

Wherein: 1, extraction element；2, primary concentration device；3, secondary concentration device；4, extraction equipment；5, the second crystallization Device；6, the second solid-liquid separator；7, mixing arrangement；8, extractant recyclable device；9, extracting agent recovery device, 10, dissolver； 11, filter device；12, the first crystallizer；13, the first solid-liquid separator；14, recrystallization solvent recyclable device；15, extractant； 16, extractant；17, recrystallization solvent；18, qinghaosu product；19, wax oil.

Specific embodiment

The technical solution of the utility model is further illustrated below by specific embodiment.

The utility model is illustrated with following embodiment, but the utility model is not limited to following embodiments, before not departing from Afterwards under the range of the objective, change is included in the technical scope of the utility model.

Embodiment 1

A kind of system producing qinghaosu, including extraction unit, upgrading unit, extraction cells, crystalline element and recrystallization Unit；

The liquid outlet of extraction unit is connected with the feed inlet of upgrading unit, the discharge port of upgrading unit and extraction cells Feed inlet is connected, and the steam (vapor) outlet of upgrading unit is connected with the feed inlet of extraction unit, the extract liquor outlet of extraction cells and knot The feed inlet of brilliant unit is connected, and the crystal discharge port of crystalline element is connected with the feed inlet of recrystallization unit, wherein described to mention The liquid outlet of unit is taken also to be connected with the feed inlet of extraction unit；The raffinate outlet of the extraction cells also with extraction cells Feed inlet be connected；

The extraction unit includes the extraction element 1 for being provided with blender and external liquid circulation；

The upgrading unit includes primary concentration device 2 and the secondary concentration device 3 connecting with primary concentration device 2；Institute Stating primary concentration device 2 is 1-3 falling film evaporator and/or luwa evaporator, and the secondary concentration device 3 is 1-3 concentration Kettle and/or Rotary Evaporators；

The extraction cells include extraction equipment 4；

The crystalline element includes the second crystallizer 5 and the second solid-liquid separator 6 for connecting with the second crystallizer 5；

The recrystallization unit includes sequentially connected dissolver 10, filter device 11, the first crystallization apparatus and ties again The inlet of brilliant solvent recovery unit 14, the recrystallization solvent recyclable device 14 is connected with the liquid outlet of the first crystallization apparatus, The recrystallization solvent outlet of the recrystallization solvent recyclable device 14 is connected with the feed inlet of dissolver 10；The filter device 11 include pre-filter and the refined filtration filter connecting with pre-filter；The filter component aperture that the pre-filter is is 1-10 μm, the number of the pre-filter is 1-3；The filter element aperture of the refined filtration filter is 0.1-1 μm, described The number of refined filtration filter is 1-3；The pre-filter and refined filtration filter independently include candle filter or pocket type Filter；The dissolver 10, the first crystallization apparatus and recrystallization solvent recyclable device 14 have been provided independently from stirring module And heating module；First crystallization apparatus includes the first crystallizer 12 and the first separation of solid and liquid connecting with the first crystallizer 12 Device 13；First crystallizer 12 and the second crystallizer 5 independently include crystallization kettle, first solid-liquid separator 13 and second Solid-liquid separator 6 independently includes centrifuge.

Method using the system production qinghaosu includes the following steps:

(1) qinghaosu in qinghaosu raw material is extracted using the first extractant 16, obtains the extracting solution containing qinghaosu；

(2) extracting solution containing qinghaosu is concentrated, obtains medicinal extract, the extractant 16 after concentration is used for extraction step (1) institute State the qinghaosu extracted in qinghaosu raw material；

(3) qinghaosu in medicinal extract is extracted, extract liquor and extract remainder containing qinghaosu are obtained；

(5) recrystallization solvent 17 dissolves the qinghaosu crude product, filtering, and recrystallization and separation of solid and liquid obtain qinghaosu production Product 18 and recrystallization mother liquor, recrystallization mother liquor obtain the recrystallization for dissolving step (4) described qinghaosu crude product by recycling Solvent 17.

Embodiment 2

A kind of system producing qinghaosu, as shown in Figure 1, including extraction unit, upgrading unit, extraction cells, crystallization list Member, disposing mother liquor unit and recrystallization unit；

The liquid outlet of extraction unit is connected with the feed inlet of upgrading unit, the discharge port of upgrading unit and extraction cells Feed inlet is connected, and the steam (vapor) outlet of upgrading unit is connected with the feed inlet of extraction unit, the extract liquor outlet of extraction cells and knot The feed inlet of brilliant unit is connected, and the crystal discharge port of crystalline element is connected with the feed inlet of recrystallization unit, wherein crystallization is single The mother liquor outlet of member is connected with the feed inlet of disposing mother liquor unit；The liquid outlet of the extraction unit also with extraction unit into Material mouth is connected；The raffinate outlet of the extraction cells is also connected with the feed inlet of extraction cells；

The extraction cells include extraction equipment 4；

The disposing mother liquor unit includes mixing arrangement 7, extractant recyclable device 8 and extracting agent recovery device 9, described to mention The arrival end of agent recyclable device 8 is taken to connect with the outlet end of the mixing arrangement 7 with the arrival end of extracting agent recovery device 9； The outlet end of the extractant recyclable device 8 is connect with the arrival end of the mixing arrangement 7；The extracting agent recovery device 9 Outlet end is connect with the arrival end of the extraction equipment 4；The outlet end of the extractant recyclable device 8 and extracting agent recovery device The top of the extractant recyclable device 8 and extracting agent recovery device 9 is separately arranged in 9 outlet end；The mixing Device 7, extractant recyclable device 8 and extractant recycling, which fill 9, sets and has been provided independently from stirring module and heating module；The extraction Agent recyclable device 8 further includes the by-product output end that 8 bottom of extractant recyclable device is arranged in；The mixing arrangement 7 includes extraction Take tank；

Method using the system production qinghaosu includes the following steps:

(5) recrystallization solvent 17 dissolves the qinghaosu crude product, filtering, and recrystallization and separation of solid and liquid obtain qinghaosu production Product 18 and recrystallization mother liquor, recrystallization mother liquor obtain the recrystallization for dissolving step (4) described qinghaosu crude product by recycling Solvent 17；

(6) second extractants 16 recycle qinghaosu crude product mother solution, and for extracting medicinal extract, recycling mentions the extractant 15 of recycling It takes agent 16 for recycling qinghaosu crude product mother solution, obtains by-product wax oil 19 when recycling extractant.

The step (5) and step (6) are without sequencing.

Embodiment 3

The method that the system production qinghaosu of qinghaosu is produced described in Application Example 2 includes the following steps:

With 20 mesh artemisia annua powder, extractant 16 (petroleum ether), extractant 15 (methanol aqueous solution) and recrystallization solvent 17 (methanol) is raw material, produces qinghaosu product 18, which is 300kg.

The primary concentration device 2 is 1 falling film evaporator, and the secondary concentration device is 1 concentration kettle, the filtering Device 11 includes 1 pre-filter and 1 refined filtration filter, and the filter element aperture of the pre-filter is 4 μm, described The filter element aperture of refined filtration filter is 0.4 μm.

(1) extraction step

Chrysanthemum mugwort is extracted twice.

Artemisia annua powder, the 3m that 300kg granule size is 20 mesh are added in extraction element 1³Petroleum ether, after impregnating 1h, It is heated with the steam of 0.2MPaG, the temperature of extraction is 55 ± 2 DEG C, stirs 1h.After extraction, the extracting solution containing qinghaosu Go to thin film evaporator.3m is added into extraction element 1³Petroleum ether, heated with the steam of 0.2MPaG, control extraction Temperature is 55 ± 2 DEG C, stirs 1h, first time extracting solution of second of extracting solution extracted as next batch artemisia annua powder. The solid sweet wormwood slag about 279kg of extraction element 1 is discharged, can be used as solid fuel.

(2) it is concentrated and separated step

Extracting solution containing qinghaosu be concentrated in falling film evaporator fall 80% the first extractant 16, be concentrated in concentration kettle Fall remaining extractant 16, obtain medicinal extract (21kg), returns to extraction element after 16 condensing recovery of the first extractant being concentrated For extracting the qinghaosu in artemisia annua powder.

Thickening temperature in falling film evaporator and concentration kettle is 58 DEG C, and concentration time amounts to 1h.

(3) extraction step

Medicinal extract extracts 2 times.

In extraction equipment 4, the methanol aqueous solution (0.21m for being 80wt% with water content³) dissolve medicinal extract, the blueness in medicinal extract Artemisin is enriched in methanol aqueous solution, which goes to the second crystallizer 5；Adding water content into extraction equipment 4 is Methanol aqueous solution (the 0.21m of 80wt%³) dissolve remaining extract remainder, after extraction, the solution as next group medicinal extract the Single extraction agent 15；Undissolved extract remainder (about 4.1kg) is discharged from the bottom of extraction equipment 4, which can be used as veterinary drug.

The temperature of extraction is 60 DEG C, and each extraction time is 2h.

(4) crystallisation step

In the second crystallizer 5, the crystallisation by cooling 3h at 15 DEG C of the extraction agent solution containing qinghaosu, magma is consolidated second It is separated, is obtained qinghaosu crude product (about 3.3kg, artemislnin content 81.5wt%) in liquid/gas separator 6, qinghaosu crude product is female Liquid goes to mixing arrangement 7.

(5) extractant 15 recycles circulation step

In mixing arrangement 7, qinghaosu crude product mother solution and petroleum ether (0.2m³) mixing, stirring, standing, layering；Heavy phase is Methanol water layer, light phase are petroleum ether layer；Heavy phase is transferred to extracting agent recovery device 9, is distilled the methanol aqueous solution isolated and followed Ring is to extraction equipment 4；Light phase is transferred to extractant recyclable device 8, isolates petroleum ether through evaporation and is recycled to mixing arrangement 7, residual Remaining recombination is divided into wax oil 19 (13.6kg).

7 operating condition of mixing arrangement is room temperature；The operation temperature of extractant recyclable device 8 is 60 DEG C；Extractant recycling dress The operating time for setting 9 is 2h, and the operation temperature of extracting agent recovery device 9 is 65 DEG C.

(6) re-crystallization step

In dissolver 10,17 methanol (0.033m of recrystallization solvent³) dissolution qinghaosu crude product, methanol solution is through filtering (level-one is initial filter to device 11, and the aperture of pre-filter filter element is 1 μm, and second level is refined filtration, refined filtration filter filter element Aperture be 0.3 μm) removal impurity, (temperature of recrystallization is 15 DEG C), the first solid-liquid separator are crystallized in the first crystallizer 12 Solid obtained after separation is qinghaosu product 18 (2.7kg, artemislnin content 99.7wt%) in 13, and mother liquor is molten through recrystallizing Agent recyclable device 14 recycles recrystallization solvent 17, recycles.

The operation temperature of dissolver 10 is room temperature, and the time of recrystallization is 4h；The behaviour of recrystallization solvent recyclable device 14 Making temperature is 60 DEG C.

Embodiment 4

Primary concentration device 2 in the system of the production qinghaosu is 1 luwa evaporator, the secondary concentration device For 1 concentration kettle, the filter device 11 includes 1 pre-filter and 3 refined filtration filters, the pre-filter were The candle filter that component aperture is 4 μm is filtered, the refined filtration filter is the candle filter that filter element aperture is 0.4 μm.

Under the conditions of (1) 50 DEG C, the qinghaosu in artemisia annua powder is extracted using ethyl alcohol in extraction element 1, is obtained containing blueness The extracting solution of artemisin, the content of qinghaosu is 1.2wt% in the artemisia annua powder, and the granularity of artemisia annua powder is 40 mesh, is contained Water is less than 0.6wt ‰, and the volume mass ratio of ethyl alcohol and artemisia annua powder is 15mL/g；The number of the extraction is 3 times, and the Extract obtained extract containing qinghaosu for 1 time and carry out next step operation, the 2nd time with extract for the 3rd time it is later obtain contain The extract of qinghaosu returns to extraction step；

Under the conditions of (2) 55 DEG C, handled 70% in extracting solution of the removal containing qinghaosu in luwa evaporator through primary concentration Ethyl alcohol, later under the conditions of 55 DEG C, in concentration kettle through secondary concentration handle will contain remaining ethyl alcohol in qinghaosu extracting solution Evaporating completely obtains medicinal extract, and the ethyl alcohol that the primary concentration processing is fallen with secondary concentration processing concentration described in step (1) for mentioning Take the qinghaosu in artemisia annua powder；

Under the conditions of (3) 55 DEG C, in extraction equipment 4, medicinal extract is extracted with the ethanol water that water content is 35wt%, is obtained The volume mass ratio of extract liquor and extract remainder containing qinghaosu, the ethanol water and medicinal extract is 15mL/g, and extraction time is 40min；The number of the extraction is 3 times, and the extract liquor containing qinghaosu being obtained by extraction for the 1st time carries out next step operation, 2nd time, the obtained extract liquor containing qinghaosu is used to extract the qinghaosu in extract, the raffinate after the 3rd extraction Object can do veterinary drug；

In (4) second crystallizers 5, the extract liquor containing qinghaosu is crystallized into 4h under the conditions of 10 DEG C, is separated by solid-liquid separation second It is separated by solid-liquid separation in device 6, obtains qinghaosu crude product and qinghaosu crude product mother solution；

(5) the qinghaosu crude product mother solution is extracted using ethyl alcohol in mixing arrangement 7, separation obtains the containing wax oil 19 Two extractants 16 and extractant 15 containing extract, by the second extractant containing wax oil 19 in extractant recyclable device 8 16 isolate ethyl alcohol through evaporation, and the extractant 15 containing extract is obtained ethyl alcohol through distillation in extracting agent recovery device 9；Institute The volume ratio for stating ethyl alcohol and qinghaosu crude product mother solution is 1:1.5；The ethyl alcohol return step (2) isolated of distilling is for extracting Qinghaosu in extract；The obtained ethyl alcohol that evaporates is for recycling qinghaosu crude product mother solution；

Under the conditions of (6) 50 DEG C, qinghaosu crude product is dissolved using ethyl alcohol in the dissolver 10 that steam is heat source, makes to dissolve Solution after qinghaosu crude product passes sequentially through the candle filter that filter element aperture is 4 μm and filter element aperture is 0.4 μm Candle filter, obtain filtrate, later recrystallize filtrate under conditions of 10 DEG C in the first crystallizer 12, in the first solid-liquid It is separated by solid-liquid separation in separator 13, obtains qinghaosu product 18 and recrystallization mother liquor, the recrystallization time is 4h, methanol and sweet wormwood The volume mass ratio of plain crude product is 25mL/g；

(7) in recrystallization solvent recyclable device 14, recrystallization mother liquor is evaporated under the conditions of 55 DEG C, obtained alcohol vapour is returned It receives；It is recycled to dissolver 10 after the alcohol vapour condensation of the recycling, the dissolution for qinghaosu crude product；

Wherein, step (5) and step (6) are without sequencing.

Embodiment 5

Primary concentration device 2 in the system of the production qinghaosu is 2 falling film evaporators, the secondary concentration device For 1 concentration kettle, the filter device 11 includes 2 pre-filters and 1 refined filtration filter, the pre-filter were The bag filter that component aperture is 6 μm is filtered, the refined filtration filter is the candle filter that filter element aperture is 0.6 μm.

Under the conditions of (1) 60 DEG C, in the extraction element 1 for being provided with external liquid circulation, extracted by ether artemisia annua powder is used In qinghaosu, obtain the extracting solution containing qinghaosu, in the artemisia annua powder content of qinghaosu be 1.4wt%, artemisia annua The granularity of powder is 60 mesh, and water content is less than 0.8wt ‰, and the volume mass ratio of ether and artemisia annua powder is 20mL/g；It is described The number of extraction is 4 times, and extracts the obtained extract progress next step operation containing qinghaosu for the 1st time, the 2nd time, the 3rd time The extract containing qinghaosu obtained after extracting with the 4th returns to extraction step；

Under the conditions of (2) 60 DEG C, handled 80% in extracting solution of the removal containing qinghaosu in falling film evaporator through primary concentration Ether, later under the conditions of 60 DEG C, in concentration kettle through secondary concentration handle will contain remaining ether in qinghaosu extracting solution Evaporating completely obtains medicinal extract, and the ether that the primary concentration processing is fallen with secondary concentration processing concentration described in step (1) for mentioning Take the qinghaosu in artemisia annua powder；

Under the conditions of (3) 60 DEG C, in extraction equipment 4, medicinal extract is extracted with the methanol aqueous solution that water content is 40wt%, is obtained The volume mass ratio of extract liquor and extract remainder containing qinghaosu, the methanol aqueous solution and medicinal extract is 18mL/g, and extraction time is 50min；The number of the extraction is 4 times, and the extract liquor containing qinghaosu being obtained by extraction for the 1st time carries out next step operation, The obtained extract liquor containing qinghaosu is used to extract the qinghaosu in extract, institute after 2nd time, the 3rd time and the 4th extraction Veterinary drug can be done by stating extract remainder；

Extract liquor containing qinghaosu is crystallized 6h under the conditions of 15 DEG C by 5 device of (4) second crystallizer, in the second solid-liquid point From being separated by solid-liquid separation in device 6, qinghaosu crude product and qinghaosu crude product mother solution are obtained；

(5) using qinghaosu crude product mother solution described in petroleum ether extraction in mixing arrangement 7, separation is obtained containing wax oil 19 Second extractant 16 and extractant 15 containing extract extract second containing wax oil 19 in extractant recyclable device 8 Agent 16 isolates petroleum ether through evaporation, and the extractant 15 containing extract is obtained first through distillation in extracting agent recovery device 9 Alcohol；The volume ratio of the petroleum ether and qinghaosu crude product mother solution is 1:2；The methanol return step (2) isolated of distilling is used Qinghaosu in extraction extract；The obtained petroleum ether that evaporates is for recycling qinghaosu crude product mother solution；

Under the conditions of (6) 60 DEG C, qinghaosu crude product is dissolved using methanol in using the dissolver 10 that steam is heat source, is made Solution after dissolution qinghaosu crude product passes sequentially through the bag filter that filter element aperture is 6 μm and filter element aperture is 1 μ The candle filter of m obtains filtrate, later recrystallizes filtrate under conditions of 15 DEG C in the first crystallization apparatus, in centrifuge It is separated by solid-liquid separation, obtains qinghaosu product 18 and recrystallization mother liquor, the recrystallization time is 6h, the body of methanol and qinghaosu crude product Product mass ratio is 40mL/g；

(7) in recrystallization solvent recyclable device 14, recrystallization mother liquor is evaporated under the conditions of 60 DEG C, obtained methanol steam is returned It receives；It is recycled to dissolver 10 after the methanol steam condensation of the recycling, the dissolution for qinghaosu crude product；

Wherein, step (5) and step (6) are without sequencing.

Embodiment 6

Primary concentration device 2 in the system of the production qinghaosu is 3 falling film evaporators, the secondary concentration device For 2 Rotary Evaporators, the filter device 11 includes 3 pre-filters and 2 refined filtration filters, the pre-filter The candle filter for being 2 μm for filter element aperture, the refined filtration filter are the filter element filtering that filter element aperture is 0.1 μm Device.

Under the conditions of (1) 45 DEG C, in the extraction element 1 for being provided with blender and external liquid circulation, extracted using isohexane Qinghaosu in artemisia annua powder obtains the extracting solution containing qinghaosu, and the content of qinghaosu is in the artemisia annua powder 1wt%, the granularity of artemisia annua powder are 20 mesh, and water content is less than 0.4wt ‰, the volume of the first extractant 16 and artemisia annua powder Mass ratio is 10mL/g；The number of the extraction is 2 times, and extracts the obtained extract containing qinghaosu for the 1st time and carry out down Single stepping, the extract containing qinghaosu obtained after the 2nd extraction return to extraction step；

Under the conditions of (2) 50 DEG C, handled 60% in extracting solution of the removal containing qinghaosu in falling film evaporator through primary concentration Isohexane, later under the conditions of 50 DEG C, handle in Rotary Evaporators through secondary concentration will contain in qinghaosu extracting solution it is remaining Isohexane evaporating completely, obtain medicinal extract, the isohexane that the primary concentration processing is fallen with secondary concentration processing concentration is used to walk Suddenly (1) qinghaosu extracted in artemisia annua powder；

Under the conditions of (3) 50 DEG C, in extraction equipment 4, medicinal extract is extracted with the methanol aqueous solution that water content is 30wt%, is obtained The volume mass ratio of extract liquor and extract remainder containing qinghaosu, the methanol aqueous solution and medicinal extract is 10mL/g, and extraction time is 30min；The number of the extraction is 2 times, and the extract liquor containing qinghaosu being obtained by extraction for the 1st time carries out next step operation, The extract liquor containing qinghaosu obtained after 2nd extraction is used to extract the qinghaosu in extract, and the extract remainder can be done Veterinary drug；

In (4) second crystallizers 5, the extract liquor containing qinghaosu is crystallized into 3h under the conditions of 5 DEG C, is consolidated in centrifuge Liquid separation, obtains qinghaosu crude product and qinghaosu crude product mother solution；

(5) in mixing arrangement 7 using qinghaosu crude product mother solution described in methanol extraction, separation obtains the containing wax oil 19 Two extractants 16 and the extractant containing extract, by the second extractant 16 containing wax oil 19 in extractant recyclable device 8 Methanol is isolated through evaporation, the extractant 15 containing extract is obtained into methanol through distillation in extracting agent recovery device 9；It is described It is 1:1 as the methanol of extractant 15 and the volume ratio of qinghaosu crude product mother solution；It is described to distill the methanol return step isolated (2) for extracting the qinghaosu in extract；The obtained petroleum ether that evaporates is for recycling qinghaosu crude product mother solution；

Under the conditions of (6) 30 DEG C, qinghaosu crude product is dissolved using methanol in using the dissolver 10 that hot water is heat source, is made Solution after dissolution qinghaosu crude product passes sequentially through the candle filter that filter element aperture is 2 μm and is with filter element aperture 0.1 μm of candle filter obtains filtrate, later recrystallizes filtrate under conditions of 5 DEG C in the first crystallizer 12, and first is solid It is separated by solid-liquid separation in liquid/gas separator 13, obtains qinghaosu product 18 and recrystallization mother liquor, the recrystallization time is 3h, methanol Volume mass ratio with qinghaosu crude product is 10mL/g；

(7) in recrystallization solvent recyclable device 14, recrystallization mother liquor is evaporated under the conditions of 50 DEG C, obtained methanol steam is returned It receives；It is recycled to dissolver 10 after the methanol steam condensation of the recycling, the dissolution for qinghaosu crude product；

Wherein, step (5) and step (6) are without sequencing.

Embodiment 7

A kind of system producing qinghaosu, in addition to being not provided with primary concentration device, remaining is same as Example 2.

Upgrading unit in the system of the production qinghaosu includes 3 concentration kettles, at the beginning of the filter device 11 includes 1 It filters filter and 1 refined filtration filter, the pre-filter is the candle filter that filter element aperture is 10 μm, the essence Filtration filter is the candle filter that filter element aperture is 0.6 μm.

Method using the system production qinghaosu of the production qinghaosu includes the following steps:

Under the conditions of (1) 70 DEG C, in the extraction element 1 for being provided with blender, using in petroleum ether extracted yellow flower wormwood artemisia powder Qinghaosu, obtain the extracting solution containing qinghaosu, in the artemisia annua powder content of qinghaosu be 1.6wt%, artemisia annua powder The granularity at end is 80 mesh, and water content is less than 1.0wt ‰, and the volume mass ratio of the first extractant 16 and artemisia annua powder is 30mL/ g；The number of the extraction is 5 times, and extracts the obtained extract progress next step operation containing qinghaosu for the 1st time, the 2nd It is secondary, the 3rd time, the extract containing qinghaosu that is obtained after extracting of the 4th and the 5th return to extraction step；After extracting The extract containing qinghaosu arrived returns to extraction step；

(2) under the conditions of 70 DEG C, concentrated processing steams the petroleum ether in extracting solution containing qinghaosu completely in concentration kettle Hair obtains medicinal extract, and the petroleum ether that the concentration concentration is fallen is for step (1) sweet wormwood extracted in artemisia annua powder Element；

Under the conditions of (3) 70 DEG C, in extraction equipment 4, medicinal extract is extracted with the methanol aqueous solution that water content is 50wt%, is obtained The volume mass ratio of extract liquor and extract remainder containing qinghaosu, the methanol aqueous solution and medicinal extract is 20mL/g, and extraction time is 60min；The number of the extraction is 5 times, and the extract liquor containing qinghaosu being obtained by extraction for the 1st time carries out next step operation, The extract liquor containing qinghaosu obtained after 2nd time, the 3rd time, the 4th and the 5th extraction returns to extraction step；The raffinate Object can do veterinary drug；

In (4) second crystallizers 5, the extract liquor containing qinghaosu is crystallized into 8h under the conditions of 30 DEG C, is separated by solid-liquid separation second It is separated by solid-liquid separation in device 6, obtains qinghaosu crude product and qinghaosu crude product mother solution；

(5) the qinghaosu crude product mother solution is extracted using ether in mixing arrangement 7, separation obtains the containing wax oil 19 Two extractants 16 and extractant 15 containing extract, by the second extractant containing wax oil 19 in extractant recyclable device 8 16 isolate ether through evaporation, and the extractant 15 containing extract is obtained methanol through distillation in extracting agent recovery device 9；Institute The volume ratio for stating ether and qinghaosu crude product mother solution is 1:0.5；The methanol return step (2) isolated of distilling is for extracting Qinghaosu in extract；The obtained ether that evaporates is for recycling qinghaosu crude product mother solution；

Under the conditions of (6) 70 DEG C, qinghaosu crude product is dissolved using methanol in using the dissolver 10 that steam is heat source, is made Solution after dissolution qinghaosu crude product passes sequentially through the candle filter that filter element aperture is 10 μm and is with filter element aperture 0.6 μm of candle filter obtains filtrate, later recrystallizes filtrate under conditions of 30 DEG C in the first crystallizer 12, It is separated by solid-liquid separation in one solid-liquid separator 13, obtains qinghaosu product 18 and recrystallization mother liquor, the recrystallization time is 8h, methanol Volume mass ratio with qinghaosu crude product is 50mL/g；

(7) in recrystallization solvent recyclable device 14, recrystallization mother liquor is evaporated under the conditions of 70 DEG C, obtained methanol steam is returned It receives；It is recycled to dissolver 10 after the alcohol vapour condensation of the recycling, the dissolution for qinghaosu crude product；

Wherein, step (5) and step (6) are without sequencing.

Embodiment 8

A kind of system producing qinghaosu, except by obtained qinghaosu product embodiment 2 the step of (6) described condition Under recrystallized again outside, remaining is identical as embodiment (2).

Comparative example 1

A kind of system producing qinghaosu, in addition to not including refined filtration filter, remaining structure and production as described in example 2 The system of qinghaosu is identical.

Primary concentration device 2 in the system of the production qinghaosu is 1 luwa evaporator, the secondary concentration device For 1 concentration kettle, the filter device 11 includes 1 pre-filter, and the pre-filter is that filter element aperture is 4 μm Candle filter.

(6) qinghaosu crude product is dissolved using ethyl alcohol in the dissolver 10 that steam is heat source, makes to dissolve qinghaosu crude product The candle filter that solution afterwards is 4 μm by filter element aperture, obtains filtrate, later at 10 DEG C in the first crystallizer 12 Under the conditions of filtrate is recrystallized, be separated by solid-liquid separation in the first solid-liquid separator 13, obtain qinghaosu product 18 and recrystallization mother liquor, The recrystallization time is 4h, and the volume mass ratio of methanol and qinghaosu crude product is 25mL/g；

Wherein, step (5) and step (6) are without sequencing.

Comparative example 2

A kind of system producing qinghaosu, in addition to not including pre-filter, remaining structure and production as described in example 2 The system of qinghaosu is identical.

Primary concentration device 2 in the system of the production qinghaosu is 1 luwa evaporator, the secondary concentration device For 1 concentration kettle, the filter device 11 includes 1 refined filtration filter, and it is 0.6 that the refined filtration filter, which is filter element aperture, μm bag filter.

(6) qinghaosu crude product is dissolved using ethyl alcohol in the dissolver 10 that steam is heat source, makes to dissolve qinghaosu crude product The bag filter that solution afterwards is 0.6 μm by filter element aperture, obtains filtrate, later at 10 DEG C in the first crystallizer 12 Under conditions of filtrate is recrystallized, be separated by solid-liquid separation in centrifuge, obtain qinghaosu product 18 and recrystallization mother liquor, the recrystallization Time is 4h, and the volume mass ratio of methanol and qinghaosu crude product is 25mL/g；

Wherein, step (5) and step (6) are without sequencing.

Comparative example 3

A kind of system producing qinghaosu, in addition to not including filter device 11, remaining structure and production as described in example 2 The system of qinghaosu is identical.

Primary concentration device 2 in the system of the production qinghaosu is 1 luwa evaporator, the secondary concentration device For 1 concentration kettle.

(6) qinghaosu crude product is dissolved using ethyl alcohol in the dissolver 10 that steam is heat source, in the first crystallizer 12 Filtrate is recrystallized under conditions of 10 DEG C, is separated by solid-liquid separation in the first solid-liquid separator 13, qinghaosu product 18 is obtained and ties again Brilliant mother liquor, the recrystallization time are 4h, and the volume mass ratio of methanol and qinghaosu crude product is 25mL/g；

Wherein, step (5) and step (6) are without sequencing.

Comparative example 4

A kind of system producing qinghaosu, in addition to the filter element aperture of pre-filter is 15 μm, remaining structure and reality The system for applying production qinghaosu described in example 4 is identical, and the method using the system production qinghaosu is also same as Example 4.

Comparative example 5

A kind of system producing qinghaosu, in addition to the filter element aperture of refined filtration filter is 2 μm, remaining structure and implementation The system that qinghaosu is produced described in example 4 is identical, and the method using the system production qinghaosu is also same as Example 4.

Comparative example 6

A kind of system producing qinghaosu, in addition to the filter element aperture of pre-filter is 0.5 μm, remaining structure and reality The system for applying production qinghaosu described in example 4 is identical, and the method using the system production qinghaosu is also same as Example 4.

The qinghaosu product that the qinghaosu product of embodiment provided by the utility model production is produced with comparative example it is pure It spends as shown in table 1 with rate of recovery situation:

Table 1

Compare comparative example 1-3 and embodiment 2 it is found that filter device can significantly improve the purity of qinghaosu product；Compare Embodiment 8 and embodiment 2 it is found that when increasing the number of recrystallization in the case where being provided with filter device, qinghaosu product Purity is not promoted, therefore setting filter device can reduce the number of recrystallization；Refined filtration filter is only provided in comparative example 2 When, it still is able to obtain the qinghaosu product of purity is high, but refined filtration filter is easy blocking, is unfavorable for the production qinghaosu The stable operation of system；The filter element aperture for the pre-filter being arranged in comparative example 4 is larger, and pre-filter does not have just The effect of filtering is walked, is easy blocking refined filtration filter in this way；The filter element aperture for the refined filtration filter being arranged in comparative example 5 compared with Greatly, it is unfavorable for the progress of filtering, the purity of qinghaosu product can not be effectively improved；The pre-filter being arranged in comparative example 6 Filter element aperture is smaller, although the qinghaosu product of purity is high can be obtained, pre-filter is easy blocking, is unfavorable for institute State the stable operation of the system of production qinghaosu.

To sum up, it can reduce being produced into for qinghaosu using the system and method for production qinghaosu provided by the utility model This, shortens the production cycle of qinghaosu, the purity of qinghaosu product is improved, to promote the competitiveness of qinghaosu manufacturing enterprise.

The Applicant declares that the utility model illustrates the method detailed of the utility model, but this reality through the foregoing embodiment It is not limited to above-mentioned method detailed with novel, that is, it is real not mean that the utility model must rely on above-mentioned method detailed ability It applies.It should be clear to those skilled in the art, any improvement to the utility model, to each original of the utility model product The equivalence replacement of material and addition, the selection of concrete mode of auxiliary element etc., all fall within the protection scope of the utility model and public affairs Within the scope of opening.

Claims

1. a kind of system for producing qinghaosu, including recrystallization unit, the recrystallization each unit includes filter device (11), It is characterized in that, the filter device (11) includes pre-filter and the refined filtration filter connecting with pre-filter；

The pre-filter includes the filter element that aperture is 1-10 μm；

The refined filtration filter includes the filter element that aperture is 0.1-1 μm.

2. the system of production qinghaosu according to claim 1, which is characterized in that the pre-filter and refined filtration filtering Device independently includes candle filter and/or bag filter；

The pre-filter includes the filter element that aperture is 2-6 μm；

The number of the pre-filter is 1-3；

The refined filtration filter includes the filter element that aperture is 0.2-0.6 μm；

The number of the refined filtration filter is 1-3.

3. the system of production qinghaosu according to claim 1, which is characterized in that the recrystallization unit further includes dissolution Device (10), the first crystallization apparatus and recrystallization solvent recyclable device (14), the dissolver (10), filter device (11), First crystallization apparatus and recrystallization solvent recyclable device (14) are sequentially connected；

The inlet of the recrystallization solvent recyclable device (14) is connected with the liquid outlet of the first crystallization apparatus, and the recrystallization is molten The recrystallization solvent outlet of agent recyclable device (14) is connected with the feed inlet of dissolver (10).

4. the system of production qinghaosu according to claim 3, which is characterized in that first crystallization apparatus includes first Crystallizer (12) and the first solid-liquid separator (13)；

First crystallizer (12) includes crystallization kettle；

First solid-liquid separator (13) includes centrifuge.

5. the system of production qinghaosu according to claim 3, which is characterized in that the system of the production qinghaosu is also wrapped Extraction unit, upgrading unit, extraction cells and crystalline element are included, the extraction unit, upgrading unit, extraction cells, crystallization are single Member and recrystallization unit are sequentially connected；

The extraction unit includes the extraction element (1) for being provided with blender and/or external liquid circulation；

The discharge port of the extraction unit is also connected with the feed inlet of extraction unit；

The steam (vapor) outlet of the upgrading unit is connected with the feed inlet of extraction element (1)；

The discharge port of the extraction cells is also connected with the feed inlet of extraction cells；

The extraction cells include extraction equipment (4).

6. the system of production qinghaosu according to claim 5, which is characterized in that the crystalline element includes the second crystallization Device (5) and the second solid-liquid separator (6) being connect with the second crystallizer (5)；

Second crystallizer (5) includes equipment of crystallisation by cooling；

Second solid-liquid separator (6) includes centrifuge.

7. the system of production qinghaosu according to claim 5, which is characterized in that the upgrading unit includes primary concentration Device (2) and the secondary concentration device (3) being connect with primary concentration device (2)；

The primary concentration device (2) includes falling film evaporator or luwa evaporator；

The quantity of the primary concentration device (2) is 1-3；

The secondary concentration device (3) includes concentration kettle or Rotary Evaporators；

The quantity of the secondary concentration device (3) is 1-3.

8. the system of production qinghaosu according to claim 5, which is characterized in that the system of the production qinghaosu is also wrapped Disposing mother liquor unit is included, the feed inlet of disposing mother liquor unit is connected with the liquid outlet of crystalline element.

9. the system of production qinghaosu according to claim 8, which is characterized in that the disposing mother liquor unit includes mixing Device (7), extractant recyclable device (8) and extracting agent recovery device (9)；

The arrival end of the extractant recyclable device (8) and the arrival end of extracting agent recovery device (9) with the mixing arrangement (7) outlet end connection；

The outlet end of the extractant recyclable device (8) is connect with the arrival end of the mixing arrangement (7)；

The extractant recyclable device (8) further includes by-product output end of the setting in extractant recyclable device (8) bottom；

The outlet end of the extracting agent recovery device (9) is connect with the arrival end of the extraction equipment (4)；

The outlet end of the extractant recyclable device (8) and the outlet end of extracting agent recovery device (9) are separately arranged in The top of the extractant recyclable device (8) and extracting agent recovery device (9).

10. the system of production qinghaosu according to claim 3, which is characterized in that the dissolver (10), the first knot Brilliant device, recrystallization solvent recyclable device (14), mixing arrangement (7), extractant recyclable device (8) and extracting agent recovery device (9) stirring module and/or heating module have been provided independently from.