CN106512467A - Economical solid-liquid transfer method - Google Patents
Economical solid-liquid transfer method Download PDFInfo
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- CN106512467A CN106512467A CN201510577064.2A CN201510577064A CN106512467A CN 106512467 A CN106512467 A CN 106512467A CN 201510577064 A CN201510577064 A CN 201510577064A CN 106512467 A CN106512467 A CN 106512467A
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Abstract
Relating to an economical solid-liquid transfer method, the invention provides an extraction method of Chinese medicinal materials, and the method is a new extraction method that gives a minimal dose of solvent capable of reaching maximum dissolution once. The method provided by the invention not only can completely extract effective components in medicinal materials, but also ensures a high medicinal material and solvent utilization rate and extraction rate. The extraction method provided by the invention has the advantages of simplified extraction operation, small solvent dosage and the like, can save a lot of cost for mass production, is beneficial to energy saving and environmental protection, and provides a new idea for the extraction process of Chinese medicinal materials.
Description
Technical field
The present invention relates to solid matter（Mushroom, microorganism, plant, animal or mineral materials, they can be natural drug, it is also possible to not be natural drug）In relevant material be transferred to liquid field, particularly to determine wherein liquid and consumption improved.
Background technology
In very long history, people have grasped the material by mushroom, microorganism, plant, animal, mineral etc., change or improve body partial function state.These are from the sporophore of Mycophyta, mycelium, spore, thalline etc., from unifacial leaf, the root of dicotyledon, rhizome, leaf, flower, fruit or herb, and mineral and the solid matter for coming from animal, have several or various be used in conjunction with, also there is a kind of exclusive use, its annual consumption is very big.It is reported that, the extract of China's Mainland outlet in 1999 is 9937 tons, and the Chinese patent medicine of outlet in 2010 is 13910 tons.At 2010 to 2013, the Chinese patent medicine yield of China's Mainland increased year by year, respectively 199.77 ten thousand tons, 238.54 ten thousand tons, 293.89 ten thousand tons, and 310.52 ten thousand tons.
These solid part composition/compositions are relevant with adjustment body function, and a part is unrelated.Therefore, before taking, it is required for doing pre-treatment.With liquid related substanceses, it is transferred out from solid, is conventional means.Relation in regard to shifting in solid-liquid between volume and solid per unit mass, always is and comments experience to be judged, this is also the emphasis of correlational study in recent years.The disclosed optimization method of the relation between volume and solid per unit mass, has single factor exploration method, orthogonal design, uniform Design, effect surface optimization at present（Three kinds of methods are designed comprising Star point design, Box.Behnken designs, Doehlert）, D- optimization designs (D-optimal design) and Projection Design (projection design) etc..The application of these methods, optimizes the relation between volume and solid masses to a certain extent.But due to, during optimization, being all to select preferably parameter in previously given scope, therefore previously given scope, directly affect the objectivity of the result of last optimization.
There is research to think, the Chinese medicine being made up of solid matters such as mushroom, microorganism, plant, animal, mineral, it is transferred in liquid to greatest extent for reaching relevant material in solid, typically now every batch solid needs to do 2 to 3 solid-liquid transfer operations, when shifting for the first time, the consumption of liquid is different according to material propertiess, probably between 8 to 18 times of raw material.Second solvent load, compared with first time, and consumption is the same or slightly few.So generally, 15,16 times to nearly 50 times in raw material of total solvent load.After the completion of transfer operation, merge transfer liquid, subsequently have the operation such as concentration.
Carrying out target substance to be transferred out in the solid of solid-liquid transfer, if in the volume of this tens times of raw materials, have raw materials quality 1 times or several times is unnecessary, the thus caused wasting of resources, will be huge.Estimated with the Chinese patent medicine yield of 2013, even if not including Chinese medicinal granule and single plant extract, it is assumed that in 310.52 ten thousand tons of Chinese patent medicines of production in 2013, need the raw material for doing solid-liquid transfer processing there are 3,000,000 tons.Assume again that this needs to do 3,000,000 tons of raw materials of solid-liquid transfer processing, liquid used is all water.If the amount of water used, when more rational many 1 times than most economical, it is exactly multiplex 3,000,000 tons of water with material quantity as radix if calculating.These water are also performed to heating, if remembered with room temperature as 25 DEG C, are heated to 100 DEG C of boilings, and 3,000,000 tons of water are accomplished by 3,000,000,000 kcal.100 DEG C of water vapor heat are 2256.8kj/kg, then per many 1 times of water（3000000 tons）, vapor is converted into from 100 DEG C of water, need 6,770,400,000,000 kj of heat energy.Plus the preparation of the most of Chinese medicinal granule promoted in some areas at present, the Chinese medicine produced with solid-liquid transfer method or granule, to solvent and the energy, it is understood that there may be greatly waste.
Above said is the waste of the good energy of the solvent caused when volume is more.Just assume volume, if conversely, total amount of liquid used, the minimum amount than reaching liquid needed for maximum transfer is little, may result in the amount that aim transference thing is transferred out not enough.And work as total amount of liquid used and reach the minimum amount phase of liquid needed for maximum transfer simultaneously as at present transfer equipment is removing transfer liquid every time, when supplementing new liq, needing to stop heating, the solid of heating and device temperature decline, and this also result in the waste of the energy.And this method so that operating process becomes loaded down with trivial details.
Even if in industrialization process, it is necessary to make volume have redundancy, in the big production of seriality, for it will do the solid of solid-liquid transfer, for the first time, for the second time, for the third time（If third time；If also multiple transfer operation, is charged to successively）In the liquid that each transfer operation is obtained, the concentration of target solids is different.Transfer equipment once feeds intake, and liquid is shifted in each time that the concentration of gained is different, after mixing, is reduced for the first time, or even second（Having for the third time, or during transfer operation more times）The concentration of transfer liquid.
For above-mentioned phenomenon, the present invention adjusts the operation after transfer operation by adjusting volume and transfer number, the transfer liquid that first time transfer operation is obtained allowed only, into next section of process operations, so as to reach solid-liquid transfer production can energy saving, resource, simplify the effect of operation.
The content of the invention
The present invention relates to solid-liquid transfer method, the method includes：
a）Conventional treatment treats solid-liquid transfer operation solid；
b）The liquid for reaching minimum amount needed for maximum transfer is added to processed conventionally solid；The minimum amount of this liquid, once uninterruptedly can add, it is also possible to which this amount is divided into two parts, first plus a part of, then plus remainder；
c）To adding the solidliquid mixture for reaching minimum amount liquid needed for maximum transfer, routinely solid-liquid transfer operation carries out operation；
d）The solid-liquid transfer liquid for obtaining enters next section of operation sequence；
e）In continuous production, transfer liquid can be removed, added and do not done in the solid that solid-liquid is shifted, as part transfer liquid to finishing the remaining solid-liquid mixing residue of a solid-liquid transfer operation, plus partially liq, mixing；Due to adding liquid to the remaining solid-liquid mixing residue for finishing a solid-liquid transfer operation, the remaining partial target material in participation thing can be made to be transferred in new liquid feeding body, therefore, accordingly, need the consumption of this partially liq of increase；This needs corresponding increased amount of liquid, can be measured by experiment, generally the 1 of amount of solid times to 5 times.
The present invention is to the liquid for needing the solid addition for doing solid-liquid transfer to reach minimum amount needed for maximum transfer, do solid-liquid transfer operation, as volume is the minimum amount that reaches liquid needed for maximum transfer, target substance transfer will not be caused incomplete because of volume deficiency；Also will not be excessive because of volume, cause to bring extra demand to heating, concentration and evaporation below.
As the present invention enters the liquid of lower one operation sequence, all it is the liquid for needing the first time solid-liquid transfer operation of the solid for doing solid-liquid transfer to obtain, aimed concn height, the saving subsequent concentration energy and the amount of labour.
To adding the solidliquid mixture for reaching minimum amount liquid needed for maximum transfer, routinely solid-liquid transfer operation carries out operation, multiple transfer operation is not carried out, reduce by several times transfer to remove during in liquid and equipment, solid adds new transfer liquid in transfer equipment, the loss of transfer equipment and solid-liquid mixed tensor, also 2 or 3 transfer operations, simplify 1 time, reduce work.
For the purpose of the present invention, term " solid " refers to the materials such as mushroom, microorganism, plant, animal, mineral, may or may not be natural drug, it is also possible to yes or no Chinese medicine.They can be the sporophore of Mycophyta, mycelium, spore, thalline etc., or unifacial leaf, the root of dicotyledon, rhizome, stem, skin, branch（It is dry）, leaf, flower, fruit or herb, or mineral, or animal tissue's organ or secretions can be one kind therein, or various mixture therein.Term " liquid " refers to liquid solvent, one or two or several mixture preferably in water, methanol, ethanol, n-butyl alcohol, 2- butanol, glycerol, Propylene Glycol, ethyl acetate, petroleum ether, benzene, chloroform, ether, dichloroethanes, halogenation 1- hexyl -3- Methylimidazole .s, supercritical carbon dioxide fluid, one or two or several mixture being optimized in water, ethanol, n-butyl alcohol, ethyl acetate, petroleum ether, halogenation 1- hexyl -3- Methylimidazole .s, supercritical carbon dioxide fluid again.After term " solid-liquid transfer " refers to solid and liquid mixing, process of the transferable thing in solid in liquid；Transferable thing in solid obtains material from solid comprising needs（Target substance）, also comprising the material that need not be obtained from solid, refer generally to the material for needing（Target substance）.
To solid plus the liquid of minimum amount needed for maximum transfer is reached, be divided into two parts, first plus a part, remaining part, can be first added in doing the material for once shifting and mix.After this mixture places a period of time, generally 15 minutes to 2 hours, liquid is taken out, is added in the mixture for having added partially liq.
1 Radix Ginseng of case determines through experiment plus 22 times of water do solid-liquid transfer processing.The transfer liquid for obtaining turns lower step operation.
2 Radix Ginseng of case determines through experiment plus 22 times of water do solid-liquid transfer processing.The transfer liquid for obtaining turns lower step operation, and remaining solidliquid mixture is designated as a0. and separately takes the Radix Ginseng for not doing solid-liquid transfer, is designated as a1, plus part water b1；To addition a1 remainder water in a0（a1*（22+2）-b1）, mixing, placement 30 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
3 Radix Salviae Miltiorrhizae of case is experimentally determined to add water 38 times, does solid-liquid transfer processing.The transfer liquid for obtaining turns lower step operation, and remaining solidliquid mixture is designated as a0. and separately takes the Radix Salviae Miltiorrhizae for not doing solid-liquid transfer, is designated as a1, plus part water b1；To addition a1 remainder water in a0（a1*（38+2）-b1）, mixing, placement 30 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
4 Radix Salviae Miltiorrhizae of case does solid-liquid transfer through the ethanol that experiment determines plus 20 times of concentration is 60%.The transfer liquid for obtaining turns lower step operation, and remaining solidliquid mixture is designated as a0. and separately takes the Radix Salviae Miltiorrhizae for not doing solid-liquid transfer, is designated as a1, plus the ethanol b1 that moiety concentrations are 60%；To the ethanol that addition a1 remainder concentration in a0 is 60%（a1*（20+1.5）-b1）, mixing, placement 30 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
5 Radix Paeoniae Alba of example determines through experiment plus 27 times of water do solid-liquid transfer.The transfer liquid for obtaining turns lower step operation.
6 Radix Paeoniae Alba of case determines through experiment plus 27 times of water do solid-liquid transfer.The transfer liquid for obtaining turns lower step operation, and remaining solidliquid mixture is designated as a0. and separately takes the Radix Paeoniae Alba for not doing solid-liquid transfer, is designated as a1, plus part water b1；To addition a1 remainder water in a0（a1*（27+2）-b1）, mixing, placement 45 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
7 Radix Puerariae of case determines through experiment plus 23 times 70% of ethanol does solid-liquid transfer.The transfer liquid for obtaining turns lower step operation.
8 Radix Puerariae of case determines through experiment plus 23 times 70% of ethanol does solid-liquid transfer.The transfer liquid for obtaining turns lower step operation, and remaining solidliquid mixture is designated as a0. and separately takes the Radix Puerariae for not doing solid-liquid transfer, is designated as a1, plus the ethanol that moiety concentrations are 70%；To the ethanol that addition a1 remainder concentration in a0 is 70%（a1*（23+1.5）-b1）, mixing, placement 45 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
9 Fructus Schisandrae Chinensis of case do solid-liquid transfer through the ethanol that experiment determines plus 21 times of concentration is 70%.The transfer liquid for obtaining turns lower step operation, and remaining solidliquid mixture is designated as a0. and separately takes the Fructus Schisandrae Chinensis for not doing solid-liquid transfer, is designated as a1, plus the ethanol that moiety concentrations are 70%；To the ethanol that addition a1 remainder concentration in a0 is 70%（a1*（21+1）-b1）, mixing, placement 30 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
10 Rhizoma Gastrodiae of case does solid-liquid transfer through the ethanol that experiment determines plus 24 times of concentration is 70%.The transfer liquid for obtaining turns lower step operation, and remaining solidliquid mixture is designated as a0. and separately takes the Rhizoma Gastrodiae for not doing solid-liquid transfer, is designated as a1, plus the ethanol that moiety concentrations are 70%；To the ethanol that addition a1 remainder concentration in a0 is 70%（a1*（21+1.5）-b1）, mixing, placement 45 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
11 Rhizoma Gastrodiae of case does solid-liquid transfer through the ethanol that experiment determines plus 24 times of concentration is 70%.The transfer liquid for obtaining turns lower step operation.
Case 12 shifts dosage 120 parts of Daphne giraldii Nitsche, 75 parts of Radix Angelicae Sinensis, 75 parts of Radix Paeoniae Rubra, 75 parts of Rhizoma Cyperi, 75 parts of Rhizoma Et Radix Notopterygii, 75 parts of Herba Asari, 75 parts of the Rhizoma Atractylodis Macrocephalae, 75 parts of Radix Saposhnikoviae, 75 parts of the Radix Angelicae Dahuricae, 75 parts of Radix Angelicae Pubescentiss, 75 parts of Semen Persicae, 75 parts of Radix Achyranthis Bidentatae, 30 parts of Ramulus Cinnamomi, 18 parts of Rhizoma Arisaematiss, 18 parts of Herba Ephedrae, 18 parts of Pheretima, 18 parts of Radix Aconiti, 25 parts of Radix Aconiti Kusnezoffii, 25 parts of Flos Carthami as a unit solid-liquid.Solid-liquid transfer is done through the ethanol that experiment determines plus 23 times of concentration is 70%.The lower step operation of the transfer liquid for obtaining turn, remaining solidliquid mixture are designated as a0. and separately take a unit solid-liquid transfer dosage portion for not doing solid-liquid transfer, are designated as a1, plus the ethanol that moiety concentrations are 70%；To the ethanol that addition a1 remainder concentration in a0 is 70%（a1*（23+1.5）-b1）, mixing, placement 60 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
13 Radix Paeoniae Alba of case determines through experiment plus 24 times of 70% ethanol does solid-liquid transfer.The transfer liquid for obtaining turns lower step operation, and remaining solidliquid mixture is designated as a0. and separately takes the Radix Paeoniae Alba for not doing solid-liquid transfer, is designated as a1, plus moiety concentrations are 70% ethanol b1；To 70% ethanol of addition a1 remainders in a0（a1*（24+1.5）-b1）, mixing, placement 45 minutes are designated as b2.The liquid in b2 is removed, is transferred in the mixture of a1+b1, is done solid-liquid transfer processing.
In above-mentioned case, the solid-liquid liquid that obtains of transfer, into next step operation when, be all the very big liquid of aim transference solid concentration, operation sequence is relatively easy, and energy saving reduces the labor intensity of next step operation, raises labour efficiency.
Claims (7)
1. a kind of economic solid-liquid transfer method, it is characterised in that comprise the steps of：
1.1 conventional treatment solids；
1.2 add the liquid for reaching minimum amount needed for maximum transfer to processed conventionally solid；The minimum amount of this liquid, once can add, it is also possible to which this amount is divided into different piece, and substep is added；
1.3 pairs add the solidliquid mixture for reaching minimum amount liquid needed for maximum transfer, and routinely solid-liquid transfer operation carries out operation；
1.4 finish the liquid that solid-liquid transfer is obtained, and do corresponding next one process operations.
2. method according to claim 1, it is characterised in that：Solid described in claim 1, refers to the material from mushroom, microorganism, plant, animal, mineral etc., may or may not be natural drug, it is also possible to yes or no Chinese medicine；They can be the sporophore of Mycophyta, mycelium, spore, thalline etc., or unifacial leaf, the root of dicotyledon, rhizome, stem, skin, branch（It is dry）, leaf, flower, fruit or herb, or mineral, or animal tissue's organ or secretions；The solid can be one kind therein, it is also possible to various mixture therein.
3. method according to claim 1, it is characterised in that：Liquid described in claim 1, refer to liquid solvent, one or two or several mixture preferably in water, methanol, ethanol, n-butyl alcohol, 2 butanol, glycerol, Propylene Glycol, ethyl acetate, petroleum ether, benzene, chloroform, ether, dichloroethanes, halogenation 1- hexyl -3- Methylimidazole .s, supercritical carbon dioxide fluid.
4. method according to claim 1, it is characterised in that：Liquid described in claim 1 can be not and do the liquid that the solid contact of solid-liquid transfer is crossed；Can also be and do after the remaining solidliquid mixture mixing after solid-liquid transfer, the liquid being transferred out.
5. method according to claim 4, it is characterised in that：After remaining solidliquid mixture that is described in claim 4 and doing after solid-liquid transfer mixes, the liquid being transferred out, because containing in remaining solidliquid mixture, the material that needs are transferred out, therefore the liquid phase ratio that consumption was not contacted with remaining solidliquid mixture, the amount of many 1 to the 6 times solids of consumption.
6. method according to claim 4, it is characterised in that：Routinely solid-liquid transfer operation described in claim 1.3 carries out the solidliquid mixture of operation, is to add in solid to reach minimum amount liquid needed for maximum transfer.
7. method according to claim 4, it is characterised in that：The liquid for entering next process operations described in claim 1.4, is the transfer liquid obtained by 1.3 operations.
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Application publication date: 20170322 |