CN102838882A - Extraction method of chestnut shell coloring matters - Google Patents
Extraction method of chestnut shell coloring matters Download PDFInfo
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- CN102838882A CN102838882A CN 201210333698 CN201210333698A CN102838882A CN 102838882 A CN102838882 A CN 102838882A CN 201210333698 CN201210333698 CN 201210333698 CN 201210333698 A CN201210333698 A CN 201210333698A CN 102838882 A CN102838882 A CN 102838882A
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Abstract
The invention discloses an extraction method of chestnut shell coloring matters. Chestnut shell particles are extracted by using a mixing solution of an alcohol solution and an inorganic acid solution, the coloring matters deposit after an extracting solution is diluted by water, precipitates are obtained after filtering and separation, and the chestnut shell coloring matters can be obtained by drying the precipitates. The extraction method utilizes the mixing solution of the alcohol solution and the inorganic acid solution to extract, hydrogen ions produced by mineral acid ionization express strong permeation and acid catalysis functions of protonic acid, coloring matter molecules in bonding states are catalyzed and dissociated, and foundations for high-efficiency dissolution are provided. Heating is favorable for improvement of a spread speed and promotion of a catalyzing and dissociating speed, a mixed solvent has an excellent dissolving and extracting ability, and chemical constituents are promoted to enter the solution. Appropriate acid concentration, solvent composition and temperature conditions wholly enable the coloring matters to be high in recovery rate, low in comprehensive cost, simple in operation process and free of discharge and pollution.
Description
Technical field
The present invention relates to a kind of process for extracting of pigment, especially a kind of process for extracting of chestnut shell pigment.
Background technology
Chinese chestnut is one of Chinese cultivated fruit tree the earliest, and the cultivation history in 2000～3000 years is arranged approximately.Leaf lanceolar or Long Circle, leaf margin has sawtooth.Flower unisexuality, monoecism; Male flower is an amentum, and ripe back involucre splits, and the chestnut fruit comes off.Branch, bark and involucre contain tannin, can extract tannin extract.The nut puce, by tawny pubescence, or dipped beam is sliding, and pulp is yellowish.Fruit contains sugar, starch, protein, fat and multivitamin, mineral substance.But usually chestnut shell is passed into disuse, become waste.
In fact, chestnut shell is as the outer peel of Chinese chestnut fruit, and the property of medicine is sweet, puckery, flat, has to fall contrary, hematostatic effect, disease such as cure mainly gastric disorder causing nausea, nosebleed epistaxis, have blood in stool.The chestnut shell pigment that from chestnut shell, extracts belongs to flavonoid; Tone belongs to the brown pigments series that is difficult to obtain in the general plant material; Not only can be used as the tinting material of products such as food, household chemicals and medicine widely, also have certain pharmaceutical use.But present research and development focus mostly in chestnut shell act as a fuel, aspect such as gac raw material, make progress to some extent though extract the research of pigment, total extraction yield have only about 15% or below, utilization ratio is not high, efficient is on the low side.
Summary of the invention
The technical problem that the present invention will solve provides the process for extracting of the high chestnut shell pigment of a kind of extraction yield.
For solving the problems of the technologies described above; The technical scheme that the present invention taked is: it extracts the mixing solutions of chestnut shell particle with alcohol solution and inorganic acid solution; Pigment precipitates behind the extracting solution dilute with water, obtains throw out after the filtering separation, and drying precipitate can obtain the chestnut shell pigment.
Alcohol solution of the present invention is one or more in methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, 2-butanols and the primary isoamyl alcohol solution; Described mineral acid is phosphoric acid, sulfuric acid, hydrochloric acid and/or sulfurous acid.The volume(tric)fraction of said alcohol solution is 30%～99.9%; The concentration of said inorganic acid solution is 0.1～3 mol/L; The volume ratio of alcohol solution and inorganic acid solution is 100:1～1:1.
During extraction according to the invention, the solid-liquid weight ratio is according to the difference of used concentration, and its ratio is both economical between 1:5～15, and rationally extracting temperature is 0～100 ℃, and extraction time is 1～10 hour.
Chestnut shell particle according to the invention is that chestnut shell is pulverized 50～100 microns the crushed material that forms.Particle is meticulous to be unfavorable for extracting to product generation absorption easily, and the excessive then solvent of particle seepage velocity is slow, influences extraction efficiency, and consumes excessive power.
Extracting solution according to the invention is with the water dilution of 1 to 10 times of volume.
Throw out according to the invention dries perhaps 25～50 ℃ of dryings.
After extracting solution behind the filtering precipitate according to the invention is measured acid concentration, add acid, alcohol solution or water as required again after, be used for extracting next time as mixing solutions.
Chemical composition in the chestnut shell is said compositions such as containing phenols, organic acid, sugar, polysaccharide (or glucoside), lactone, tonka bean camphor, tannin, steroidal (or triterpene) and flavones from classification.These chemical compositions are not that independent or relative free state is present among the chestnut shell, but exist with xylogen, Mierocrystalline cellulose and mutual link coupled complex combination attitude.Mineral acid helps bringing into play the acid catalysis effect owing to can go out proton hydrogen ion freely by electric power, strengthens dissociating of these chemical compositions, helps the extraction stripping of solvent.The mixture of alcohols and water is β-Gu Zaichun in the chestnut shell, β-daucosterol, beans steroid-5-alkene-3 β; 7 α-alcohol, ergot steroid-6; 22-diene-3 β; 5 α, the high-quality solvent of 8 α-triol, beans steroid-4-alkene-6 α-alcohol-3-ketone, beans steroid-4-alkene-6 β-alcohol-3-ketone, beans steroid-5-alkene-3 beta-hydroxies-7-ketone, Hydroxycinnamic acid methyl esters, Vanillin, lactose and rutin can extract stripping easily.Therefore, use the mixed solvent of mineral acid and alcohols, can bring into play synergistic extraction and render a service, improve percentage extraction.
Adopt the beneficial effect that technique scheme produced to be: the present invention utilizes the mixing solutions of alcohol solution and inorganic acid solution to extract; The strong osmosis and the acid catalysis function of the hydrogen ion performance protonic acid that mineral acid ionization produces; The pigment molecular catalysis of combined is dissociated, for efficient stripping lays the foundation.Heating helps the raising of velocity of diffusion and the lifting of catalysis dissociation rate, and mixed solvent has good dissolving and extracting power, promotes chemical composition to get into solution.Suitable acid concentration, solvent composition and temperature condition make the pigment recovery high on the whole, and comprehensive cost is low, and operating process is simple, zero release, pollution-free.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed explanation.
Embodiment 1: the process for extracting of this chestnut shell pigment adopts following process step.
1) chestnut shell is dried naturally; Grind; Be sized to 50 to 100 microns, get chestnut shell particle 5g and be placed in the Erlenmeyer flask, sulphuric acid soln and the volume(tric)fraction that adds 0.1mol/L is the mixing solutions of 50% ethanolic soln; The volume ratio of alcohol solution and inorganic acid solution is 50:1, and the solid-liquid weight ratio is 1:10; Vibration is 4 hours on the room-temperature water bath vibrator;
2) filter 20 milliliters of the filtratings obtain, add the dilution of 20 ml distilled waters, precipitate, filter, dry throw out, obtain brown solid powder 1.02 grams, the pigment extraction yield is 20.4%; Product purity is checked through liquid chromatography, and purity is 99%; 35 milliliters of recovery of raffinate are subsequent use.
Embodiment 2: the process for extracting of this chestnut shell pigment adopts following process step.
1) chestnut shell is dried naturally; Grind; Be sized to 50 to 100 microns, get chestnut shell particle 5g and be placed in the Erlenmeyer flask, the sulphuric acid soln that adds 0.3mol/L and the hydrochloric acid (volume ratio 1:1) of 0.3mol/L and and volume(tric)fraction be the mixing solutions of 75% methanol solution; The volume ratio of alcohol solution and inorganic acid solution is 20:1, and the solid-liquid weight ratio is 1:7.5; Vibration is 2.5 hours on 50 ℃ water bath chader;
2) filter 60 milliliters of the filtratings obtain, add 180 milliliters in water, deposition, filter, 25 ℃ of dryings, brown solid powder 1.56 grams, extraction yield is 31.2%; Product is checked through liquid chromatography, and purity is 99.1%.The 108 milliliters of recovery of filtrating are subsequent use.
Embodiment 3: the process for extracting of this chestnut shell pigment adopts following process step.
1) chestnut shell is dried naturally; Grind; Be sized to 50 to 100 microns, get chestnut shell particle 5g and be placed in the Erlenmeyer flask, phosphoric acid solution and the volume(tric)fraction that adds 1mol/L is the mixing solutions of 30% aqueous isopropanol; The volume ratio of alcohol solution and inorganic acid solution is 80:1, and the solid-liquid weight ratio is 1:12; Vibration is 1 hour on 80 ℃ water bath chader;
2) filter 40 milliliters of the filtratings obtain, add the dilution of 200 ml waters, after filtering-depositing and the drying brown solid powder 1.56 grams, extraction yield is 31.2%; Product is checked with liquid chromatography, and purity is 99%, and the 65 milliliters of recovery of filtrating are subsequent use.
Embodiment 4: the process for extracting of this chestnut shell pigment adopts following process step.
1) chestnut shell is dried naturally; Grind; Be sized to 50 to 100 microns, get chestnut shell particle 20g, sulfurous acid solution and the volume(tric)fraction that adds 3mol/L is that 99.9% propanol solution and volume(tric)fraction are the mixing solutions of 60% butanol solution (volume ratio 1:1); The volume ratio of alcohol solution and inorganic acid solution is 10:1, and the solid-liquid weight ratio is 1:5; 100 ℃ of water-bath vibrations 2 hours;
2) filter the water dilution of the filtrating obtain with 8 times of volumes, after filtering-depositing and the drying brown solid powder 5.36 restrains, extraction yield is 26.8%; Product is checked with liquid chromatography, and purity is 99%.
Embodiment 5: the process for extracting of this chestnut shell pigment adopts following process step.
1) chestnut shell is dried naturally; Grind; Be sized to 50 to 100 microns, get chestnut shell particle 20g, hydrochloric acid soln and the volume(tric)fraction that adds 2mol/L is that 85% 2-butanol solution and volume(tric)fraction are the mixing solutions of 85% primary isoamyl alcohol solution (volume ratio 1:1); The volume ratio of alcohol solution and inorganic acid solution is 100:1, and the solid-liquid weight ratio is 1:15; 0 ℃ of water-bath vibration 10 hours;
2) filter the water dilution of the filtrating obtain with 6 times of volumes, after filtering-depositing and the drying brown solid powder 5.14 restrains, extraction yield is 25.7%; Product is checked with liquid chromatography, and purity is 99%.
Embodiment 6: the process for extracting of this chestnut shell pigment adopts following process step.
1) chestnut shell is dried naturally, grind, be sized to 50 to 100 microns; Get chestnut shell particle 20g; Phosphoric acid solution and the volume(tric)fraction that adds 1.5mol/L is the mixing solutions of 45% ethanolic soln, and the volume ratio of alcohol solution and inorganic acid solution is 1:1, and the solid-liquid weight ratio is 1:13; 40 ℃ of water-bath vibrations 6 hours;
2) filter the water dilution of the filtrating obtain with 10 times of volumes, after filtering-depositing and the drying brown solid powder 5.66 restrains, extraction yield is 28.3%; Product is checked with liquid chromatography, and purity is 99%.
Claims (8)
1. the process for extracting of a chestnut shell pigment; It is characterized in that: it extracts the mixing solutions of chestnut shell particle with alcohol solution and inorganic acid solution; Pigment precipitates behind the extracting solution dilute with water, obtains throw out after the filtering separation, and drying precipitate can obtain the chestnut shell pigment.
2. the process for extracting of a kind of chestnut shell pigment according to claim 1 is characterized in that: described alcohol solution is one or more in methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, 2-butanols and the primary isoamyl alcohol solution; Described mineral acid is phosphoric acid, sulfuric acid, hydrochloric acid and/or sulfurous acid.
3. the process for extracting of a kind of chestnut shell pigment according to claim 3 is characterized in that: the volume(tric)fraction of said alcohol solution is 30%～99.9%; The concentration of said inorganic acid solution is 0.1～3 mol/L; The volume ratio of alcohol solution and inorganic acid solution is 100:1～1:1.
4. according to the process for extracting of claim 1,2 or 3 described a kind of chestnut shell pigments, it is characterized in that: during said extraction, the solid-liquid weight ratio is 1:5～15, and extracting temperature is at 0～100 ℃, and extraction time is 1～10 hour.
5. according to the process for extracting of claim 1,2 or 3 described a kind of chestnut shell pigments, it is characterized in that: said chestnut shell particle is chestnut shell to be pulverized 50～100 powder and micron that form mince.
6. according to the process for extracting of claim 1,2 or 3 described a kind of chestnut shell pigments, it is characterized in that: said extracting solution is with the water dilution of 1 to 10 times of volume.
7. according to the process for extracting of claim 1,2 or 3 described a kind of chestnut shell pigments, it is characterized in that: said throw out dries perhaps 25～50 ℃ of dryings.
8. according to the process for extracting of claim 1,2 or 3 described a kind of chestnut shell pigments; It is characterized in that: after the extracting solution behind the said filtering precipitate is measured acid concentration; After adding acid, alcohol solution or water as required again, be used for extracting next time as mixing solutions.
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| CN 201210333698 CN102838882A (en) | 2012-09-11 | 2012-09-11 | Extraction method of chestnut shell coloring matters |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232725A (en) * | 2013-04-24 | 2013-08-07 | 湖北紫鑫生物科技有限公司 | High-stability chestnut shell brown pigment as well as refining method and application thereof |
| CN104497623A (en) * | 2014-12-04 | 2015-04-08 | 常州大学 | Method for extracting natural pigment from fruit shell |
| CN106189354A (en) * | 2016-07-26 | 2016-12-07 | 武汉黄鹤楼香精香料有限公司 | A kind of micronizing works in coordination with the method that impulse electric field prepares chestnut shell brown pigment |
-
2012
- 2012-09-11 CN CN 201210333698 patent/CN102838882A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232725A (en) * | 2013-04-24 | 2013-08-07 | 湖北紫鑫生物科技有限公司 | High-stability chestnut shell brown pigment as well as refining method and application thereof |
| CN104497623A (en) * | 2014-12-04 | 2015-04-08 | 常州大学 | Method for extracting natural pigment from fruit shell |
| CN106189354A (en) * | 2016-07-26 | 2016-12-07 | 武汉黄鹤楼香精香料有限公司 | A kind of micronizing works in coordination with the method that impulse electric field prepares chestnut shell brown pigment |
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Application publication date: 20121226 |