CN105419381A - Purification method of natural dyestuff of mulberries - Google Patents
Purification method of natural dyestuff of mulberries Download PDFInfo
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- CN105419381A CN105419381A CN201510856455.8A CN201510856455A CN105419381A CN 105419381 A CN105419381 A CN 105419381A CN 201510856455 A CN201510856455 A CN 201510856455A CN 105419381 A CN105419381 A CN 105419381A
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Abstract
Provided is a purification method of natural dyestuff of mulberries. Natural dyestuff components in the mulberries can be effectively extracted, the extracted natural dyestuff components have a good dyeing property and a drug health-care function, and synthetic dyestuff does not have the drug health-care function; in the refining process, broussonetia papyrifera juice is added, the antimicrobial and antiviral effects of the natural dyestuff can be effectively improved, and the better drug health-care function is achieved.
Description
Technical field
The present invention relates to textile dyestuff technical field, particularly relate to a kind of method of purification of mulberries natural dyestuff.
Background technology
In human history, natural fuel has made indelible contribution for beautifying people's life.From 19 end of the centurys, due to developing rapidly of synthetic dyestuff, natural fuel is made substantially to have exited textile dyeing field.Along with the continuous enhancing of mankind's environmental consciousness and the growing interest to own health, the harm that partial synthesis dyestuff produces human health and ecotope is more and more noticeable.Along with the raising of state-of-the-art, the especially raising of modern manufacturing industry level, people require more fast higher to safe, the health care of rag trade etc., natural dyestuff starts again as people are paid attention to.In natural dyestuff, animals and plants dyestuff extracts by organism, good with Environmental compatibility, biodegradable.Natural dyestuff is mostly Chinese medicine, and in dyeing course, its medicine is absorbed by fabric together with pigment with flavour ingredient, and except dyeing function, natural dyestuff also has the several functions such as medicine, spices, makes the fabric after dyeing to the distinctive medicinal health-care function of human body.
Mulberries,
mulberry treematuration
fruit, mulberries are named again
sorosis, mulberry bubble youngster, he peasant likes its maturation
fresh fruitedible, taste sweet juice is many, is one of fruit of often eating of people.Ripe mulberries matter is glossy, sour and sweet palatability, with individual large, meat is thick, look purplish red, the sufficient person of sugar is good.During annual fruit maturation in 4 ~ June
gather, decon,
dryor dry edible after slightly steaming, also can come
steep in wine.Concrete maturation time various places are different, and earlier, the north slightly late a bit in south.
Have detailed elaboration to mulberry fruit in the multiple medical ancient books and records such as Compendium of Material Medica by value and usage, mulberry fruit is sweet in flavor and cold in property, there is liver-kidney tonifying, promote the production of body fluid moisturize, the effect such as black invention order.Sorosis is exactly a kind of diuresis that the common people often adopt since time immemorial, health care, the fresh fruit of relieving summer heat, its special efficacy on the books in Compendium of Materia Medica.
Summary of the invention
In order to develop the natural dyestuff being conducive to human body, the invention provides a kind of method of purification of mulberries natural dyestuff.
An extracting method for mulberries natural dyestuff, carries out according to following step:
Step one: the pre-treatment of raw material, rinses well mulberries raw material clear water, with weight milling process by clean for moisture content extruding, obtains natural dyestuff pressed liquor, after mechanical disintegration 3-5 time is carried out repeatedly to remaining solid matter, and mistake 25 mesh sieves, extracting screen underflow;
Step 2: by the mulberries powder ultrasonic extraction crushed, select concentration be the ethanol of 95% as solvent, ultrasonic power is 150-300W, and solid-liquid ratio is under the condition of 1: 15-60 after ultrasonic extraction 15-25 minute, filter, must natural dyestuff filtrate and filter residue be contained;
Step 3: second extraction is carried out to filter residue, with 95% alcohol reflux of 10 ~ 15 times amount, extract twice, first time extracts 2 hours, and second time is extracted 1 hour; Obtain natural dyestuff extracting solution;
Step 4: natural dyestuff pressed liquor, filtrate, extracting solution are concentrated by underpressure distillation, oven drying at low temperature, obtains thick mulberries natural dyestuff;
Step 5: thick mulberries natural dyestuff is refined, by above-mentioned thick mulberries natural dyestuff deionized water dissolving, after being mixed with weight ratio 2-8% mulberries natural dyestuff solution, cross positively charged ion macroporous adsorptive resins, coutroi velocity in 5-10 ml/min, after mulberries natural dyestuff solution stream is complete, use deionized water rinsing resin column, wash away raffinate, then be the ethanol elution of 3-5,50-95% by pH value; The elutriant obtained carries out underpressure distillation and concentrates, solidifies, pulverizes, and reclaims ethanol, obtains refining intense violet color Powdered mulberries natural dyestuff extract, and the rear cloth specimen of dyeing is intense violet color.
Preferably, the solid content of the solid matter in described step one after weight squeezing is 75%-85%.
The solid content of the solid matter after the weight squeezing in step one is 75%-85%, so both can ensure that main natural dyestuff composition is extracted by the form of pressed liquor, also can ensure that some pharmaceutical cpds in mulberries can not be destroyed.
Filter sieve in step one chooses 25 mesh sieves, and main purpose is the foreign material such as the cauline leaf screening out mulberries.
Preferably, it is better that temperature is adjusted to 40-60 DEG C of effect by described step 2.
At this temperature, both can promote the efficiency of ultrasonic extraction, also can ensure that some pharmaceutical cpds in mulberries can not be destroyed.
Preferably, described step 5 can also add paper mulberry juice before refining, and described additional proportion is thick mulberries natural dyestuff: paper mulberry juice=25-35:1.
Paper mulberry has that fast-growing, strong adaptability, distribution are wide, easily breeding, heat is high, felling cycle is short feature.Its root system is shallow, and root distribution in side is very wide, and growth is fast, rudiment power and ability for tillering strong, resistance to pruning.Resistance to crocking is strong.All distribution is had in the temperate zone of China, the torrid zone, no matter Plain,
hillsor mountain region can grow, its leaf is good pig feed, and its phloem fiber is the high-grade materials of papermaking, and material is pure white, and its root and seed all can be used as medicine, and resin can control tetter, and economic worth is very high.The juice of paper mulberry has inducing diuresis to remove edema removing toxic substances, swollen tinea disease of harnessing the river, and snake, worm, honeybee, scorpion, dog such as to sting at the effect, have good antibacterial, antiviral efficacy.
Mulberries natural dyestuff refining before add paper mulberry juice, effectively can promote antibacterial, the antiviral efficacy of natural dyestuff, reach better medicinal health-care effect.
The method of purification of mulberries natural dyestuff provided by the present invention, effectively can extract the natural dyestuff composition in mulberries, the natural dyestuff composition extracted not only has good dyeing behavior, and the medicinal health-care function in addition not available for synthetic dyestuff, paper mulberry juice is added in treating process, effectively can promote antibacterial, the antiviral efficacy of natural dyestuff, reach better medicinal health-care effect.
Embodiment
embodiment 1
An extracting method for mulberries natural dyestuff, carries out according to following step:
Step one: the pre-treatment of raw material, rinses well mulberries raw material clear water, with weight milling process by clean for moisture content extruding, obtains natural dyestuff pressed liquor, after mechanical disintegration 3-5 time is carried out repeatedly to remaining solid matter, and mistake 25 mesh sieves, extracting screen underflow;
The solid content of the solid matter in described step one after weight squeezing is 75%-85%.
Step 2: by the mulberries powder ultrasonic extraction crushed, select concentration be the ethanol of 95% as solvent, ultrasonic power is 300W, and solid-liquid ratio is 1: 40, and under the condition of 40-60 DEG C, ultrasonic extraction is after 20 minutes, filter, must natural dyestuff filtrate and filter residue be contained;
Step 3: second extraction is carried out to filter residue, with 95% alcohol reflux of 10 ~ 15 times amount, extract twice, first time extracts 2 hours, and second time is extracted 1 hour; Obtain natural dyestuff extracting solution;
Step 4: natural dyestuff pressed liquor, filtrate, extracting solution are concentrated by underpressure distillation, oven drying at low temperature, obtains thick mulberries natural dyestuff;
Step 5: refine thick mulberries natural dyestuff, add paper mulberry juice before refining, described additional proportion is thick mulberries natural dyestuff: paper mulberry juice=30:1.By above-mentioned thick mulberries natural dyestuff deionized water dissolving, after being mixed with weight ratio 5% mulberries natural dyestuff solution, cross positively charged ion macroporous adsorptive resins, coutroi velocity is in 5-10 ml/min, after mulberries natural dyestuff solution stream is complete, uses deionized water rinsing resin column, wash away raffinate, be 3-5 by pH value again, the ethanol elution of 85%; The elutriant obtained carries out underpressure distillation and concentrates, solidifies, pulverizes, and reclaims ethanol, obtains refining intense violet color Powdered mulberries natural dyestuff extract, and the rear cloth specimen of dyeing is intense violet color.
embodiment 2
An extracting method for mulberries natural dyestuff, carries out according to following step:
Step one: the pre-treatment of raw material, rinses well mulberries raw material clear water, with weight milling process by clean for moisture content extruding, obtains natural dyestuff pressed liquor, after mechanical disintegration 3-5 time is carried out repeatedly to remaining solid matter, and mistake 25 mesh sieves, extracting screen underflow;
The solid content of the solid matter in described step one after weight squeezing is 75%-85%.
Step 2: by the mulberries powder ultrasonic extraction crushed, select concentration be the ethanol of 95% as solvent, ultrasonic power is 250W, and solid-liquid ratio is 1: 35, and under the condition of 40-60 DEG C, ultrasonic extraction is after 15 minutes, filter, must natural dyestuff filtrate and filter residue be contained;
Step 3: second extraction is carried out to filter residue, with 95% alcohol reflux of 10 ~ 15 times amount, extract twice, first time extracts 2 hours, and second time is extracted 1 hour; Obtain natural dyestuff extracting solution;
Step 4: natural dyestuff pressed liquor, filtrate, extracting solution are concentrated by underpressure distillation, oven drying at low temperature, obtains thick mulberries natural dyestuff;
Step 5: refine thick mulberries natural dyestuff, add paper mulberry juice before refining, described additional proportion is thick mulberries natural dyestuff: paper mulberry juice=25:1.By above-mentioned thick mulberries natural dyestuff deionized water dissolving, after being mixed with weight ratio 7% mulberries natural dyestuff solution, cross positively charged ion macroporous adsorptive resins, coutroi velocity is in 5-10 ml/min, after mulberries natural dyestuff solution stream is complete, uses deionized water rinsing resin column, wash away raffinate, be 3-5 by pH value again, the ethanol elution of 85%; The elutriant obtained carries out underpressure distillation and concentrates, solidifies, pulverizes, and reclaims ethanol, obtains refining intense violet color Powdered mulberries natural dyestuff extract, and the rear cloth specimen of dyeing is intense violet color.
embodiment 3
An extracting method for mulberries natural dyestuff, carries out according to following step:
Step one: the pre-treatment of raw material, rinses well mulberries raw material clear water, with weight milling process by clean for moisture content extruding, obtains natural dyestuff pressed liquor, after mechanical disintegration 3-5 time is carried out repeatedly to remaining solid matter, and mistake 25 mesh sieves, extracting screen underflow;
The solid content of the solid matter in described step one after weight squeezing is 75%-85%.
Step 2: by the mulberries powder ultrasonic extraction crushed, select concentration be the ethanol of 95% as solvent, ultrasonic power is 150W, solid-liquid ratio is 1: 25, under the condition of 40-60 DEG C after ultrasonic extraction 15-25 minute, filter, must natural dyestuff filtrate and filter residue be contained;
Step 3: second extraction is carried out to filter residue, with 95% alcohol reflux of 10 ~ 15 times amount, extract twice, first time extracts 2 hours, and second time is extracted 1 hour; Obtain natural dyestuff extracting solution;
Step 4: natural dyestuff pressed liquor, filtrate, extracting solution are concentrated by underpressure distillation, oven drying at low temperature, obtains thick mulberries natural dyestuff;
Step 5: refine thick mulberries natural dyestuff, add paper mulberry juice before refining, described additional proportion is thick mulberries natural dyestuff: paper mulberry juice=35:1.By above-mentioned thick mulberries natural dyestuff deionized water dissolving, after being mixed with weight ratio 2% mulberries natural dyestuff solution, cross positively charged ion macroporous adsorptive resins, coutroi velocity is in 5-10 ml/min, after mulberries natural dyestuff solution stream is complete, uses deionized water rinsing resin column, wash away raffinate, be 3-5 by pH value again, the ethanol elution of 95%; The elutriant obtained carries out underpressure distillation and concentrates, solidifies, pulverizes, and reclaims ethanol, obtains refining intense violet color Powdered mulberries natural dyestuff extract, and the rear cloth specimen of dyeing is intense violet color.
embodiment 4
An extracting method for mulberries natural dyestuff, carries out according to following step:
Step one: the pre-treatment of raw material, rinses well mulberries raw material clear water, with weight milling process by clean for moisture content extruding, obtains natural dyestuff pressed liquor, after mechanical disintegration 3-5 time is carried out repeatedly to remaining solid matter, and mistake 25 mesh sieves, extracting screen underflow;
The solid content of the solid matter in described step one after weight squeezing is 75%-85%.
Step 2: by the mulberries powder ultrasonic extraction crushed, select concentration be the ethanol of 95% as solvent, ultrasonic power is 250W, solid-liquid ratio is 1: 40, under the condition of 40-60 DEG C after ultrasonic extraction 15-25 minute, filter, must natural dyestuff filtrate and filter residue be contained;
Step 3: second extraction is carried out to filter residue, with 95% alcohol reflux of 10 ~ 15 times amount, extract twice, first time extracts 2 hours, and second time is extracted 1 hour; Obtain natural dyestuff extracting solution;
Step 4: natural dyestuff pressed liquor, filtrate, extracting solution are concentrated by underpressure distillation, oven drying at low temperature, obtains thick mulberries natural dyestuff;
Step 5: thick mulberries natural dyestuff is refined, by above-mentioned thick mulberries natural dyestuff deionized water dissolving, after being mixed with weight ratio 2% mulberries natural dyestuff solution, cross positively charged ion macroporous adsorptive resins, coutroi velocity in 5-10 ml/min, after mulberries natural dyestuff solution stream is complete, use deionized water rinsing resin column, wash away raffinate, then be 3-5 by pH value, the ethanol elution of 60%; The elutriant obtained carries out underpressure distillation and concentrates, solidifies, pulverizes, and reclaims ethanol, obtains refining intense violet color Powdered mulberries natural dyestuff extract, and the rear cloth specimen of dyeing is intense violet color.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (4)
1. an extracting method for mulberries natural dyestuff, is characterized in that, carries out according to following step:
Step one: the pre-treatment of raw material, rinses well mulberries raw material clear water, with weight milling process by clean for moisture content extruding, obtains natural dyestuff pressed liquor, after mechanical disintegration 3-5 time is carried out repeatedly to remaining solid matter, and mistake 30 mesh sieves, extracting screen underflow;
Step 2: by the mulberries powder ultrasonic extraction crushed, select concentration be the ethanol of 95% as solvent, ultrasonic power is 150-300W, and solid-liquid ratio is after 1: 15-60, ultrasonic extraction 15-25 minute, filter, must natural dyestuff filtrate and filter residue be contained;
Step 3: second extraction is carried out to filter residue, with 95% alcohol reflux of 10 ~ 15 times amount, extract twice, first time extracts 2 hours, and second time is extracted 1 hour; Obtain natural dyestuff extracting solution;
Step 4: natural dyestuff pressed liquor, filtrate, extracting solution are concentrated by underpressure distillation, oven drying at low temperature, obtains thick mulberries natural dyestuff;
Step 5: thick mulberries natural dyestuff is refined, by above-mentioned thick mulberries natural dyestuff deionized water dissolving, after being mixed with weight ratio 2-8% mulberries natural dyestuff solution, cross positively charged ion macroporous adsorptive resins, coutroi velocity in 5-10 ml/min, after mulberries natural dyestuff solution stream is complete, use deionized water rinsing resin column, wash away raffinate, then be the ethanol elution of 3-5,50-95% by pH value; The elutriant obtained carries out underpressure distillation and concentrates, solidifies, pulverizes, and reclaims ethanol, obtains refining intense violet color Powdered mulberries natural dyestuff extract, and the rear cloth specimen of dyeing is intense violet color.
2. the extracting method of mulberries natural dyestuff as claimed in claim 1, is characterized in that, described step one, and the solid content of the solid matter after weight squeezing is 75%-85%.
3. the extracting method of mulberries natural dyestuff as claimed in claim 1, it is characterized in that, described step 2, is heated to 40-60 DEG C by ethanol.
4. the extracting method of mulberries natural dyestuff as claimed in claim 1, it is characterized in that described step 5 can also add paper mulberry juice before refining, additional proportion is thick mulberries natural dyestuff: paper mulberry juice=25-35:1.
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| CN201510856455.8A CN105419381A (en) | 2015-11-30 | 2015-11-30 | Purification method of natural dyestuff of mulberries |
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| CN201510856455.8A CN105419381A (en) | 2015-11-30 | 2015-11-30 | Purification method of natural dyestuff of mulberries |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106012144A (en) * | 2016-05-18 | 2016-10-12 | 湖南细心信息科技有限公司 | Pearl antibacterial lady underwear fabric and preparation method thereof |
| CN106046848A (en) * | 2016-06-06 | 2016-10-26 | 西昌学院 | Method for extracting and purifying anthocyanin from mulberry pomace |
| CN109825106A (en) * | 2019-03-29 | 2019-05-31 | 江苏省农业科学院宿迁农科所 | The one seed pod mulberry " Extraction of Pigment of no big ten " of seed |
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| CN102212053A (en) * | 2011-04-16 | 2011-10-12 | 湖州柳荫生物科技有限公司 | Method for extracting mulberry cyanidin |
| CN104403359A (en) * | 2014-11-14 | 2015-03-11 | 陕西科技大学 | Method for preparation of mulberry pigment by mulberry residue |
| CN104593150A (en) * | 2014-12-02 | 2015-05-06 | 云南中烟工业有限责任公司 | Preparation method of mulberry extract and application of mulberry extract in cigarettes |
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2015
- 2015-11-30 CN CN201510856455.8A patent/CN105419381A/en active Pending
Patent Citations (4)
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| CN102212053A (en) * | 2011-04-16 | 2011-10-12 | 湖州柳荫生物科技有限公司 | Method for extracting mulberry cyanidin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106012144A (en) * | 2016-05-18 | 2016-10-12 | 湖南细心信息科技有限公司 | Pearl antibacterial lady underwear fabric and preparation method thereof |
| CN106046848A (en) * | 2016-06-06 | 2016-10-26 | 西昌学院 | Method for extracting and purifying anthocyanin from mulberry pomace |
| CN109825106A (en) * | 2019-03-29 | 2019-05-31 | 江苏省农业科学院宿迁农科所 | The one seed pod mulberry " Extraction of Pigment of no big ten " of seed |
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Application publication date: 20160323 |