CN104628528B - A kind of preparation method of butyl alcohol - Google Patents
A kind of preparation method of butyl alcohol Download PDFInfo
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Abstract
The preparation method that the present invention relates to a kind of high-purity butyl alcohol, comprises the following steps: step (1): take Radix Rhodiolae medical material, adopt decoct, ultrasonic, microwave, backflow, seepage, dipping or warm macerating technique are extracted; After in extracting solution, limit adds the stirring of flocculate and clarify limit, standing, filter; Filtrate after filtration crosses NF membrane, and the aperture of NF membrane is 1～2nm, and molecular cut off is 100～1000 dalton; Membrane filtration liquid crosses polymer microsphere, below microspherulite diameter 300um; Through filtrate water or the 0.5-5% ethanol elution remove impurity of polymer microsphere, 10%-25% ethanol elution, when being eluted beginning from butyl alcohol, collect eluent, merge eluent and obtain collection liquid; Concentrating under reduced pressure, the dry purity that obtains is the butyl alcohol of more than 80%. Skill operating process of the present invention is simple, is suitable for industrialized production; In extraction separation and purification process, all material all can reuse, and cost is low, and the inventive method have employed NF membrane and polymer microsphere separation purification, and dead absorption is less, and the butyl alcohol rate of transform is high.
Description
Technical field
The preparation method that the present invention relates to a kind of butyl alcohol, belongs to butyl alcohol extracting and developing purification and field of refinement in Radix Rhodiolae.
Background technology
Butyl alcohol is a kind of natural antioxidant, is one of main active in Radix Rhodiolae medical material, is a kind of derivant of phenethanol. It has extremely strong resist myocardial ischemia, reducing myocardial infarction area, reduce apoptosis of cardiac muscle number, reduce ischemia-reperfusion animal ventricular tachycardia and the incidence rate quivered in room and severity. The oxidation resistance knocking out low density lipoprotein receptor mice feeding high cholesterol diet can also be improved simultaneously, and reduce upborne cholesterolemia and triglyceride levels.
Butyl alcohol can significantly improve the superoxide dismutase in coxsackie myocarditis mouse heart and activity of glutathione peroxidase; reduce serum lactate dehydrogenase (SLD) activity and LPO; heart is had good protective effect, is mainly used in treatment cardiovascular aspect disease clinically.
Extract the method separating butyl alcohol at present mainly to have:
Rhodioside in Radix Rhodiolae, tyrosol, production technology (the Wang Huatian of coumarin, Northeast Agricultural University's Master's thesis) disclose butyl alcohol extracting method in a kind of Radix Rhodiolae, specifically: adopt the granulated slag after supercritical extraction, extract by 40% soak with ethanol, extracting solution filtering and concentrating, macroporous resin on concentrated solution, after ethanol-dichloromethane (3: 7) eluting, it is concentrated into dry, a small amount of distilled water dissolves, filter, it is concentrated into small size, vacuum freeze-drying, obtain the extract of rhodioside and butyl alcohol, wherein rhodioside and butyl alcohol content sum are about 80%, yield is 0.27%.Employing dichloromethane in a large number in the method extraction process, its toxicity is relatively big, causes that product exists potential safety hazard, and butyl alcohol yield is relatively low, wastes medical material greatly.
In olive polyphenol the composition such as butyl alcohol the research of separation purification (yellow Beichuan. Northwest University's Master's thesis) disclose a kind of butyl alcohol extraction separation method, specifically: have employed supersound extraction, extraction conditions is: temperature is 60, and the time is 20min, and solid-liquid ratio is 1: 25. Extracting solution adopts silica gel column chromatography separation butyl alcohol, and the butyl alcohol purity separated is 85.81%. It is 40% by alumina adsorption method separation butyl alcohol purity. It is adopt silica gel column chromatography to be easily separated that the method extracts butyl alcohol, extremely adsorbs more serious due to silicagel column, causes that butyl alcohol loss is more, and can use substantial amounts of organic solvent in industrialization process, and operator's health is unfavorable; The silicagel column used due to substantial amounts of use organic solvent and separation process cannot reuse, and causes in cheese preparation process relatively costly.
The preparation method research of rhodioside and Radix Rhodiolae aglycon standard substance (Ding Chaowu. analyze test journal, 1997,16 (1): 38-41) preparation method disclosing butyl alcohol standard substance, it specifically have employed supersound extraction, extracting solution adds lead acetate solution tannin-removing matter, flavone etc., using activated carbon adsorption depigmentation afterwards, be easily separated with preparative hplc post after after membrane filtration, the butyl alcohol purity obtained is 97%. The method adopts preparative hplc to be easily separated, and can only adapt to the separation of laboratory, it is impossible to realize industrialization.
Rhodioside and butyl alcohol Study on extraction (Li Chen in Radix Rhodiolae, Chen Dongsheng, Chen Juan etc. Chinese crude drug, 2006,29 (11): 1239-1241) disclosing butyl alcohol extraction process, it is to have employed 80% alcohol reflux, and solvent load is 6 times, extract 2 times, each 2 hours. The research of Extraction Technology of Rhodiola Sacra that He Meiyan, Zhang little Long. Tang Gute delivers (Chinese Journal of Modern Applied Pharmacy, 2012,29 (6): 495-497) butyl alcohol extracting method is disclosed, reflux, extract, when it is to have employed 8 times amount 50% ethanol 80 DEG C, extracts 2 times, each 1 hour. Ma Tao, Xiong Chunmei, the orthogonal experiment opening loyal grey hair table extracts the rhodioside in Rhodiola Crenulata and butyl alcohol (Kunming Normal Higher Traiing School's journal, 2006,28 (4): 14-16) extracting method of butyl alcohol is disclosed, by 90% methanol or absolute methanol supersound extraction when in fact have employed 65 DEG C, extraction time is 15 minutes, and solid-liquid ratio is 1: 20. The butyl alcohol content obtained is 0.015%. Patent name is a kind of ethanol is that the tyrosol CO2 supercritical extraction method of entrainer has opened a kind of method extracting butyl alcohol, in fact adopts the method for supercritical extraction to extract butyl alcohol, and the extraction ratio obtaining butyl alcohol is 1.637%. These methods are all preliminary extraction research, and it has been respectively adopted reflux, extract, supersound extraction and supercritical extraction, it does not have separating purification butyl alcohol further, therefore purity is all relatively low.
Patent name name is called that a kind of method of purifying tyrosol from coarse product of olive polyphenol discloses the another kind of method extracting butyl alcohol, specifically olive polyphenol coarse powder aqueous acid is dissolved, sodium chloride is added in above-mentioned olive polyphenol solution, prepare the olive polyphenol solution that Sal is saturated; It is extracted with ethyl acetate the butyl alcohol in the olive polyphenol solution that Sal is saturated; Remove extraction into ethyl acetate mutually in moisture. It is 70%-90% that liquid phase method records ethyl acetate middle butyl alcohol content mutually.The butyl alcohol purity that the method obtains is relatively low, and its described 70%-90% is for adopting areas of peak normalization method gained, and true purity should be 50%-70%.
Patent name is that butyl alcohol and butyl alcohol by-product salidroside plant extraction and preparation and purposes thereof disclose another method extracting butyl alcohol, specifically by raw material alcohol reflux, dipping or seepage are extracted, collect extracting solution, it is concentrated into without alcohol taste, add water cold preservation, go precipitation, aqueous solution acid solution adjusts PH to 2-4, cold preservation, go precipitation, low pole macroporous resin on clear liquor, first wash with water to effluent in neutrality, again with alkaline solution eluting macroporous resin, then it is washed till neutrality with deionized water again, again with acid solution eluting, it is eluted to partial neutral again with deionized water, above eluent all discards, again with 5%-30% ethanol elution, collecting eluent, eluent concentrates, and after drying with organic solvent dissolution, removes insoluble matter, clear liquor concentrates, and adds precipitation organic solvent, is sufficiently stirred for, cold preservation, goes precipitation, after taking clear liquor concentration, add chromatographic silica gel and carry out mixing sample, be evaporated, upper silica gel column chromatography, adopting organic solvent or mixed organic solvents to carry out remove impurity and eluting or gradient elution, adopt thin layer detection, collecting principal spot is the eluent of butyl alcohol, reclaims eluent, obtains solid matter and carry out recrystallization with recrystallization organic solvent, to obtain final product. the method complicated operation is loaded down with trivial details, separates purification time long, and silicagel column extremely adsorbs seriously, and butyl alcohol loss is more, eluent thin layer monitors butyl alcohol, collects the eluent that principal spot is butyl alcohol and merges, and concentration, in the inapplicable and large-scale production of this mode, owing to silicagel column cannot reuse, relatively costly, and it is unfavorable for environmental protection and energy-saving and emission-reduction.
Summary of the invention
The present invention is to solve the preparation method that above-mentioned technical problem is to provide a kind of butyl alcohol, operating procedure is simple, is suitable for industrialized production, and cost is low, and dead absorption is few, and the butyl alcohol rate of transform is high, and without the use of toxic solvent, safety is high.
The preparation method that the technical scheme is that a kind of butyl alcohol, comprises the following steps:
Step (1): take Radix Rhodiolae medical material, adopt decoct, ultrasonic, microwave, backflow, seepage, dipping or warm macerating technique are extracted;
Step (2): after limit adds the stirring of flocculate and clarify limit, standing in the extracting solution prepare step (1), filter;
Filtrate after step (2) filtration is crossed NF membrane by step (3), and the aperture of NF membrane is 1～2nm, and molecular cut off is 100～1000 dalton;
The membrane filtration liquid that step (4) processes through step (3) crosses polymer microsphere, below microspherulite diameter 300um;
Step (5), through the filtrate water of step (4) polymer microsphere or 0.5-5wt% ethanol elution remove impurity, 10%-25wt% ethanol elution, collects eluent when being eluted beginning from butyl alcohol, merges eluent and obtains and collect liquid; The filtrate 0.5-5wt% ethanol elution remove impurity of preferred polymer microsphere, good impurity removing effect, then use 25wt% ethanol elution, the butyl alcohol rate of transform is high.
The collection liquid concentrating under reduced pressure that step (5) is obtained by step (6), the dry purity that obtains is the butyl alcohol of more than 80%.
On the basis of technique scheme, the present invention can also do following improvement.
The preparation method of the present invention a kind of butyl alcohol described above, further, step (1) extracting solution is water or 1～100% ethanol, extracts 1～3 time, and solvent load is 3～20 times.
The preparation method of the present invention a kind of butyl alcohol described above, further, a kind of or arbitrarily several in described selection of polymeric flocculants acetic acid chitosan solution, ZTC1+1 solution, fruit juice clarifier or Chinese medicine clarifier.
The preparation method of the present invention a kind of butyl alcohol described above, further, described fruit juice clarifier selects KBT-GZC fruit juice clarifier or 101 fruit juice clarifiers. It is a kind of or arbitrarily several that described Chinese medicine clarifier selects in KBT-ZTC series traditional Chinese clarifier. In described acetic acid chitosan solution, the mass/volume mark of chitosan and 1% acetic acid is 1～3%.
The preparation method of the present invention a kind of butyl alcohol described above, further, polymeric microball material in polystyrene type or divinyl benzene polymers type or polymethyl methacrylate type or polyacrylic acid epoxy-type any one.
The preparation method of the present invention a kind of butyl alcohol described above, further, described microspherulite diameter scope 5～200um.
The preparation method of the present invention a kind of butyl alcohol described above, further, described microspherulite diameter scope 100～150um. The polymer microsphere adopting this particle size range can obtain higher degree butyl alcohol, and its purity reaches more than 90%.
The preparation method of the present invention a kind of butyl alcohol described above, further, described flocculant addition 0.5～5wt%, mixing time is 5 minutes～2 hours, and time of repose is 6～24 hours.
Compared with prior art there is following advantage in the present invention:
1, skill operating process is simple, is suitable for industrialized production;
2, in extraction separation and purification process, all material all can reuse, and cost is low;
3, the inventive method have employed NF membrane and polymer microsphere separation purification, and dead absorption is less, and the butyl alcohol rate of transform is high;
4, the inventive method is prepared in the process of butyl alcohol only with water, ethanol, belongs to innocuous agents, and operator's body harm is little.
Detailed description of the invention
With the following Examples principles of the invention and feature being described, example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Fruit juice clarifier used by the embodiment of the present invention and Chinese medicine clarifier are all purchased from Ke Lier biotechnology company.
Embodiment 1
Take Radix Rhodiolae medical material 1kg, add 8 times amount water, microwave extraction 2 times, each 5 minutes, extracting solution is merged together, add 2.5% amount (V/V, volume ratio) 1% acetic acid chitosan solution, limit edged stirs, stirring is stopped after 30 minutes, room temperature is placed 6 hours, filter, filtrate crosses NE40 film, and (model is NF membrane, 4.0 inches), collection membrane filtrate, on membrane filtration liquid, (microsphere is polystyrene type to polymer microsphere, model is NM100, particle diameter is 150um), first wash with water to effluent and be practically free of other composition, after change 15% ethanol elution into, Liquid Detection, start when butyl alcohol is eluted to collect, to butyl alcohol not subsequently, merge and collect liquid, it is evaporated to small size, vacuum drying, obtain butyl alcohol. purity detecting is 90%, and the butyl alcohol rate of transform is 73%.
The 1% acetic acid chitosan solution that embodiment 1 uses is that laboratory now joins product, concrete compound method is: the preparation of 1% chitosan solution: first with the acetum of glacial acetic acid and water preparation 1%, then 1g chitosan powder is dissolved with a small amount of 1% acetum, stir, add 1% acetum of remaining amount, fully it is dissolved into colloid solution, to obtain final product.
Embodiment 2
Take Radix Rhodiolae medical material 1kg, add 10 times amount water, decoct and extract 3 times, each 2 hours, extracting solution is merged together, add 4% amount (V/V, volume ratio) ZTC1+1 solution, limit edged stirs, stirring is stopped after 3 minutes, room temperature is placed 12 hours, filter, filtrate crosses NE80 film, and (model is NF membrane, 8.0 inches), collection membrane filtrate, on membrane filtration liquid, (microsphere is polystyrene type to polymer microsphere, model is UniPs5-100, particle diameter is 5um), first wash with water to effluent and be practically free of other composition, after change 10% ethanol elution into, Liquid Detection, start when butyl alcohol is eluted to collect, to butyl alcohol not subsequently, merge and collect liquid, it is evaporated to small size, microwave drying, obtain butyl alcohol.Purity detecting is 81%, and the butyl alcohol rate of transform is 67%.
In embodiment 2, ZTC1+1 solution is that laboratory now joins product, and concrete compound method is:
ZTC1+1 clarifier
The preparation of 1%A solution: weigh 1g, add water 100ml compound method: first uses a small amount of water dissolution, stirring, adds the solvent of remaining amount, stirs, and after swelling 24 hours, filters, to obtain final product.
The preparation of 1%B solution: weigh 1g, adds 1% acetate solvate 100ml
Compound method: first with the acetum of glacial acetic acid and water preparation 1%, then dissolves 1gB component with a small amount of 1% acetum, and stirs into pasty state, add 1% acetum of remaining amount, swelling 24 hours, filter, to obtain final product.
It is initially charged A during use, stirs 3 minutes, add B afterwards, stir, 15min under 60 DEG C of water bath condition.
Embodiment 3
Take Radix Rhodiolae medical material 1kg, add 6 times amount water, supersound extraction 2 times, each 30 minutes, extracting solution is merged together, add 5% amount (V/V, volume ratio) Chinese medicine clarifier (now joining), limit edged stirs, stirring is stopped after 3 minutes, place 24 hours, filter, filtrate crosses NE25 film, and (model is NF membrane, 2.5 inches), collection membrane filtrate, on membrane filtration liquid, (microsphere is polystyrene type to polymer microsphere, model is UniCoreS10, particle diameter is 10um), first wash with water to effluent and be practically free of other composition, after change 20% ethanol elution into, Liquid Detection, start when butyl alcohol is eluted to collect, to butyl alcohol not subsequently, merge and collect liquid, it is evaporated to small size, spray drying, obtain butyl alcohol. purity detecting is 83%, and the butyl alcohol rate of transform is 70%.
Embodiment 3 Chinese medicine clarifier is that laboratory now joins product, and concrete compound method is:
The preparation of 5%A: measure 5mlA component, add water to 100ml, stir, to obtain final product.
The preparation of 5%B: weigh 5gB component, add water to 100ml, stir, to obtain final product.
During use, to treating clear liquor is initially charged 5% diluent of A agent, stirring, (when adding clarifier, mixing speed is preferably 60-100r/min, mixing time 2-3min, uniformly), 50 DEG C-60 DEG C insulations stand 30-60 minute, under agitation adding 5% diluent of B agent, addition is identical with A agent, after stirring 2-3min mixing, stop stirring, wait for 5-10min quietly.
Embodiment 4
Take Radix Rhodiolae medical material 1kg, add 20 times amount 40% ethanol, continuous seepage is extracted, impregnate 24 hours, start to collect impregnation liquid, collection limit, limit adds new 40% ethanol to 20 times amount, extracting solution is merged together, add 6% amount (V/V, volume ratio) fruit juice clarifier, limit edged stirs, stirring is stopped after 2 minutes, place 12 hours, filter, filtrate crosses NE18 film, and (model is NF membrane, 1.8 inches), molecular cut off is 100～1000 dalton, collection membrane filtrate, on membrane filtration liquid, (microsphere is polystyrene type to polymer microsphere, model is UniPMM50-300, particle diameter is 50um), first wash with water to effluent and be practically free of other composition, after change 25% ethanol elution into, Liquid Detection, start when butyl alcohol is eluted to collect, to butyl alcohol not subsequently, merge and collect liquid, it is evaporated to small size, vacuum drying, obtain butyl alcohol. purity detecting is 87%. the butyl alcohol rate of transform is 76%.
Embodiment 4 fruit juice clarifier is that laboratory now joins product, and concrete compound method is: weigh appropriate A agent, and dilute is the solution of 5%;Weighing appropriate B agent, dilute is the solution of 5%. To treating settled solution is initially charged 5% diluent of A agent during use, stirring, (when adding clarifier, mixing speed is preferably 60-100r/min, mixing time 1-2min mix homogeneously), stand 10-30 minute, being stirred for lower 5% diluent adding B agent, addition is identical with A agent, after adding B agent mixing, stop stirring, wait for 2-10min quietly and visible flocculent deposit generates and settles gradually.
Embodiment 5
Take Radix Rhodiolae medical material 1kg, add 8 times amount water, microwave extraction 2 times, each 5 minutes, extracting solution is merged together, add 2.5% amount (V/V, volume ratio) 1% acetic acid chitosan solution, limit edged stirs, stirring is stopped after 30 minutes, room temperature is placed 6 hours, filter, filtrate crosses NE40 film, and (model is NF membrane, 4.0 inches), collection membrane filtrate, on membrane filtration liquid, (microsphere is polystyrene type to polymer microsphere, model is NM100, particle diameter is 100um), first wash with water to effluent and be practically free of other composition, after change 15% ethanol elution into, Liquid Detection, start when butyl alcohol is eluted to collect, to butyl alcohol not subsequently, merge and collect liquid, it is evaporated to small size, vacuum drying, obtain butyl alcohol. purity detecting is 91%, and the butyl alcohol rate of transform is 73%.
Embodiment 6
Take Radix Rhodiolae medical material 1kg, grind to form coarse powder, add 8 times amount water, microwave extraction 2 times, each 5 minutes, extracting solution is merged together, add 2.5% amount (V/V, volume ratio) 1% acetic acid chitosan solution, limit edged stirs, stirring is stopped after 30 minutes, room temperature is placed 12 hours, filter, filtrate crosses NE40 film, and (model is NF membrane, 4.0 inches), collection membrane filtrate, on membrane filtration liquid, (microsphere is polystyrene type to polymer microsphere, model is NM100, particle diameter is 150um), first wash with water to effluent and be practically free of other composition, after change 15% ethanol elution into, Liquid Detection, start when butyl alcohol is eluted to collect, to butyl alcohol not subsequently, merge and collect liquid, it is evaporated to small size, vacuum drying, obtain butyl alcohol. purity detecting is 92.5%, and the butyl alcohol rate of transform is 74%.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a butyl alcohol, it is characterised in that comprise the following steps:
Step (1): take Radix Rhodiolae medical material, adopt decoct, ultrasonic, microwave, backflow, seepage, impregnation technology are extracted;
Step (2): after limit adds the stirring of Old Region limit, standing in the extracting solution prepare step (1), filter;
Step (3) is by the filtrate after step (2) filtration by NF membrane, and the aperture of NF membrane is 1～2nm, and molecular cut off is 100～1000 dalton;
The membrane filtration liquid that step (4) processes through step (3) crosses polymer microsphere, below microspherulite diameter 300um;
Step (5), through the filtrate water of step (4) polymer microsphere or 0.5～5% ethanol elution remove impurity, 10%-25% ethanol elution, collects eluent when being eluted beginning from butyl alcohol, merges eluent and obtains and collect liquid;
The collection liquid concentrating under reduced pressure that step (5) is obtained by step (6), the dry purity that obtains is the butyl alcohol of more than 80%.
2. the preparation method of a kind of butyl alcohol according to claim 1, it is characterised in that step (1) extracting solution is water or 1～100% ethanol, extracts 1～3 time, and solvent load is 3～20 times.
3. the preparation method of a kind of butyl alcohol according to claim 1, it is characterised in that a kind of or arbitrarily several in described selection of polymeric flocculants acetic acid chitosan solution, ZTC1+1 solution, fruit juice clarifier or Chinese medicine clarifier.
4. the preparation method of a kind of butyl alcohol according to claim 3, it is characterised in that described fruit juice clarifier selects KBT-GZC fruit juice clarifier or 101 fruit juice clarifiers; Described Chinese medicine clarifier selects KBT-ZTC series traditional Chinese clarifier; In described acetic acid chitosan solution, the mass body fraction of chitosan and 1% acetic acid is 1～3%.
5. the preparation method of a kind of butyl alcohol according to claim 3, it is characterised in that described NF membrane is any one in NE18, NE25, NE40 or NE80.
6. the preparation method of a kind of butyl alcohol according to any one of claim 1 to 5, it is characterised in that polymeric microball material in polystyrene type or divinyl benzene polymers type or polymethyl methacrylate type or polyacrylic acid epoxy-type any one.
7. the preparation method of a kind of butyl alcohol according to any one of claim 1 to 5, it is characterised in that described microspherulite diameter ranges for 5～200 μm.
8. the preparation method of a kind of butyl alcohol according to claim 5, it is characterised in that described microspherulite diameter ranges for 100～150um.
9. the preparation method of a kind of butyl alcohol according to any one of claim 1 to 5, it is characterised in that described flocculant addition is 0.5～6wt%, mixing time is 5 minutes～2 hours, and time of repose is 6～24 hours.
10. the preparation method of a kind of butyl alcohol according to any one of claim 1 to 5, it is characterised in that described flocculant addition is 2.5～5wt%, mixing time is 30 minutes～60 minutes, and time of repose is 6～24 hours.
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