CN103881414A - Method for extracting indigo by adopting indigofera suffruticosa Mill. - Google Patents
Method for extracting indigo by adopting indigofera suffruticosa Mill. Download PDFInfo
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- CN103881414A CN103881414A CN201410066631.3A CN201410066631A CN103881414A CN 103881414 A CN103881414 A CN 103881414A CN 201410066631 A CN201410066631 A CN 201410066631A CN 103881414 A CN103881414 A CN 103881414A
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Abstract
The invention belongs to a natural vegetable dye extraction processing method and provides a method for extracting indigo by adopting indigofera suffruticosa Mill. The method is characterized by firstly obtaining indigo mud by using a traditional method for extracting indigo mud with indigofera suffruticosa Mill. branches and leaves and then purifying the indigo mud, wherein in the purification process, hydrochloric acid is added to catalyze hydrolysis of indigofera suffruticosa Mill. glycosides and accelerate dissociation of indoxyl; in an alkaline solution of which the pH value is 9, ketonic tautomerism can happen and two molecular indolones are subjected to condensation reaction to be oxidized into indigo and slowly sink in a state of suspended matters insoluble in water; therefore, the indigo yield is increased while removing impurities in the purification process, and harmful matters are not generated or discharged, so that the method is safe and environment-friendly. The method is simple to operate, is convenient and practicable, is low in cost and is environment-friendly, non-toxic and harmless.
Description
Technical field
The invention belongs to natural plant dye and extract working method, particularly, relate to a kind of by the wild blue or green indigo method of extracting of setting.
Background technology
Indigo is the natural plant dye that people of all nationalities of China tradition is used, and is widely used in cotton, fiber crops, wool textile dyeing and batik, tie dyeing etc.In five kinds of different plants tradition makes indigo raw material sources: woaded blue (Isatis tinctoria L.), Root of Indigowoad (Baphicacanthus cusia (Nees) Bremek.), indigo plant (Polygonum tinctorium Ait.), wood blue (Indigofera tinctoria Linn.) and wild blue or green set (Indigofera suffruticosa Mill.).Due to the impact of synthetic dyestuff, various nationalities area extract indigo natural, environmental protection, traditional method and technology reproducible and to HUMAN HEALTH safety be mostly lost, only be stored at present the indivedual peasant households in Some Minority Races area and use, and have the possibility of whole disappearances.China ethnobotany worker, for rescuing this Chinese nation's rarity, in this national tradition technique of deep excavation, improves its technique, to provide technical basis for forming the quality products of local characteristic.At present, in prior art, extract the indigo report of improving one's methods there are no adopting wild green grass or young crops to set.
Summary of the invention
Object of the present invention aims to provide a kind of by the indigo method of wild blue or green tree extraction.The advantages such as the method possesses simple to operate, convenient and practical, with low cost, and environment-protecting asepsis is harmless.
In order to realize above-mentioned purpose of the present invention, the invention provides following technical scheme:
Extract indigo method with wild blue or green tree, first extract indigo mud with wild blue or green tree branches and leaves, more indigo mud is carried out to purifying obtain indigo.
Described method, gets indigo mud, adds distilled water, stirs, and slowly stirs and adds hydrochloric acid, stops stirring heating in water bath to 100 ℃ 1 hour while not emitting bubble; Then carry out extracting, extract water above out, then add distilled water, stir, be washed to neutral PH-7, drain water, leave precipitation, then after regulating distilled water to be added to be PH-9 with 5% sodium hydroxide, pour the container of dress precipitation into, stir, heating in water bath boils 1 hour again, suction filtration, be washed to neutral PH-7, drain water and obtain purification of samples, this sample is dried 4 hours in 60 ℃, baking oven, pulverize 100 mesh sieves, obtained purification of samples.
Accompanying drawing explanation
Fig. 1 for slightly carrying, purification and standard substance high performance liquid chromatograph test result, 1A is the wild blue or green indigo test result of local method system, 1B is the open country green grass or young crops indigo test result of purifying, 1C is standard substance test result.
Embodiment
Further illustrate essentiality content of the present invention with following embodiment of the present invention below, but do not limit the present invention with this.
Embodiment 1
One, materials and methods
1. material: Ye Qingshu (Indigofera suffrutiosa Mill.) is Papilionaceae plant, and adopting its branches and leaves that are about 30 centimetres is the raw material of the indigo mud of processing.The place of production is Man Falong village, Meng Han town, In Xishuangbanna of Yunnan Jinghong City.This kind of plant is different from wood blue (Indigofera tinctoria Linn.), and the blue temperate zone of producing of wood, is machaka; And wild blue or green tree is for to belong to tropical evergreen shrubs not of the same race together, be now detected in a small amount of artificial culture of Xishuangbannadaizu, if rescue not in time protection, be about to extinction.
2. method:
1) local method is produced indigo mud
2) purifying of indigo mud
3) mensuration of indigo purity: indigo high performance liquid chromatograph (HPLC) HP-1200 (DAD) detector for purity detecting, U.S.'s Agilent is produced.Indigo standard substance are provided by Yi Da group, are artificial synthetic goods.
Two, test results and analysis
1. the Dai nationality by the traditional method that wild blue or green tree branches and leaves extracts indigo mud is:
10 kilograms, the fresh feed branches and leaves of plucking, equivalent is put into respectively 5 buckets (raw material: water=1:7.5) that 15 kg of water are housed, and the smooth stone that upper pressure is one heavily approximately 1 kilogram, allows water cover raw material, retting 32 hours under 23 ℃ of-32 ℃ of alternating temperatures.Take out stone, pull impurity such as not macerating the pectin, wax, ash content and the careless slag that carry on rotten vegetable material out for making farm manure.Then in every barrel, put into 0.2 kilogram of white lime [Ca (OH) is housed
2] cloth pocket, stir and within 2-3 minute, there will be a lot of blue-greenish colour foams, the cloth bag of lime is equipped with in taking-up, be stirred to again lather collapse, leave standstill approximately 5 minutes, if there is blue foam to occur, be stained with edible oil with forefinger, removing again to stir 1 minute foam disappears, raw material has carbon dioxide generating when retting is fermented in water, the white lime adding during with stirring reacts and generates water-fast calcium carbonate (CaCO3) precipitation, and white lime can make indigo glycoside be hydrolyzed simultaneously, generates water-fast indigo and water-soluble monose etc.Calcium carbonate can adsorb and is suspended in indigo in water, accelerates sedimentation speed.Allow it staticly settle 3-4 days, indigo mud forms, and isolates.
2. the purification process of indigo mud of the present invention is:
Get 1 kilogram, the indigo mud that obtains in above-mentioned 1 step (the Dai nationality traditional fabrication wild blue clay indigo), put into container, then add 2 liters of distilled water, and stir slowly add again approximately 538 milliliters of hydrochloric acid (HCL) do not stop stir, constantly there is bubble to emerge, while making it not emit bubble, stop stirring.Then heating in water bath to 100 ℃, and maintain 100 ℃ 1 hour.Then carry out extracting, extract water above out, add again distilled water, then stir, be washed till and add water PH-7(neutrality), drain water, leave precipitation, then after using 5% sodium hydroxide (NaOH) to regulate 2 liters of distilled water to be added to be PH-9, pour the container of dress precipitation into.And stir, heating in water bath boils again, and maintains 1 hour.Then suction filtration again, is washed to neutrality (PH-7).Drain water and obtain purification of samples.This sample (60 ℃) in baking oven is dried 4 hours, pulverizes 100 mesh sieves, obtains purification of samples.
In purge process, add hydrochloric acid, can be hydrolyzed by the wild blue or green glucoside thing of catalysis, accelerate the free of indoxyl, and keto-acid tautomerism also can occur in the basic solution of PH-9,2 molecule indolone generation condensation reactions, be oxidized to indigoly, be water-fast suspended substance state and slowly sink.Therefore purge process, goes the deimpurity while, has increased indigo output, and also unharmful substance produces and discharge, so be environmental protection.
3. wild blue or green indigo purity testing (seeing Figure 1A-Fig. 1 C)
1) the dry indigo mud (traditional method) of test sample, 3 kinds of indigo purified (purification process of the present invention) and standard substance (synthetic is indigo).
2) sample preparation: above-mentioned three kinds of samples respectively take 7 milligrams, dissolves and is settled to 100 milliliters with chloroform.
3) chromatographic condition: detect wavelength 280 nanometer chromatographic columns, Agilent 20RABXSB-C18 (4.6X250 millimeter, 5 millimeters), 25 ℃ of column temperatures, flow velocity 1 ml/min.Moving phase: methyl alcohol: water (volume ratio is 75:25), sample size is 5 milliliters.
4) purity: the peak area size and peak retention time that record respectively 3 samples.By peak area size, the indigo purity that calculates three samples is: indigo mud is 22.7%, and purification sample is 96.5%, and standard substance are 92%.
Xishuangbannadaizu is made indigo raw material with wild blue or green tree conduct, though at the centuries that used among the people, but so far there are no introduces specially it with word and makes indigo technique, and products obtained therefrom purity is not high, raw material has carbon dioxide generating when retting is fermented in water, the white lime adding during with stirring reacts and generates water-fast calcium carbonate (CaC03) precipitation, and white lime can make indigo glycoside be hydrolyzed simultaneously, generates water-fast indigo and water-soluble monose etc.Of the present invention improving one's methods, easy to operate, method is reliable, and technique is simple, and product purity is high, and yield is higher.In making, do not need specific installation and sample, all can implement in the ethnic mimority area, borderland that traffic is less-developed.This provides a kind of new technology and support for rural prosperity, the poor areas of the western region.
Claims (2)
1. extract indigo method with wild blue or green tree, first extract indigo mud with wild blue or green tree branches and leaves, more indigo mud is carried out to purifying obtain indigo.
2. the method for claim 1, is characterized in that, gets indigo mud, adds distilled water, stirs, and slowly stirs and adds hydrochloric acid, stops stirring heating in water bath to 100 ℃ 1 hour while not emitting bubble; Then carry out extracting, extract water above out, then add distilled water, stir, be washed to neutral PH-7, drain water, leave precipitation, then after regulating distilled water to be added to be PH-9 with 5% sodium hydroxide, pour the container of dress precipitation into, stir, heating in water bath boils 1 hour again, suction filtration, be washed to neutral PH-7, drain water and obtain purification of samples, this sample is dried 4 hours in 60 ℃, baking oven, pulverize 100 mesh sieves, obtained purification of samples.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106336685A (en) * | 2016-08-24 | 2017-01-18 | 张永成 | Method for extracting natural dye by using biological fermentation method, and applications thereof |
| CN107365512A (en) * | 2016-05-12 | 2017-11-21 | 雷炳忠 | From a kind of method of the indigo natural dye of Radix Isatidis plant extract |
| CN112898798A (en) * | 2019-11-19 | 2021-06-04 | 哈工大机器人南昌智能制造研究院 | Method for preparing indigo from fresh leaves of kale |
| CN112898800B (en) * | 2021-01-18 | 2022-09-16 | 山东云卿生物科技有限公司 | Method for extracting indigo |
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| CN101397408A (en) * | 2008-10-30 | 2009-04-01 | 五邑大学 | Production process of high-purity vegetable indigo dye |
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| CN101397408A (en) * | 2008-10-30 | 2009-04-01 | 五邑大学 | Production process of high-purity vegetable indigo dye |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107365512A (en) * | 2016-05-12 | 2017-11-21 | 雷炳忠 | From a kind of method of the indigo natural dye of Radix Isatidis plant extract |
| CN106336685A (en) * | 2016-08-24 | 2017-01-18 | 张永成 | Method for extracting natural dye by using biological fermentation method, and applications thereof |
| CN112898798A (en) * | 2019-11-19 | 2021-06-04 | 哈工大机器人南昌智能制造研究院 | Method for preparing indigo from fresh leaves of kale |
| CN112898800B (en) * | 2021-01-18 | 2022-09-16 | 山东云卿生物科技有限公司 | Method for extracting indigo |
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