CN108912729A - The natural dye and colouring method for extracting the method for natural dye from madder and being prepared by this method - Google Patents
The natural dye and colouring method for extracting the method for natural dye from madder and being prepared by this method Download PDFInfo
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- CN108912729A CN108912729A CN201810724943.7A CN201810724943A CN108912729A CN 108912729 A CN108912729 A CN 108912729A CN 201810724943 A CN201810724943 A CN 201810724943A CN 108912729 A CN108912729 A CN 108912729A
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- madder
- natural dye
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- extracting
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/14—Wool
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/24—Polyamides; Polyurethanes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/82—Textiles which contain different kinds of fibres
Abstract
The present invention relates to natural dye extraction and colouring arts, disclose a kind of method that natural dye is extracted from madder and the natural dye and colouring method that are prepared by this method.It is described from madder extract natural dye method include：Madder is cleaned, is dry, is crushed, obtained crushed material is extracted in alkaline aqueous solution, then obtained extracting solution is successively filtered, distilled and is freeze-dried.Madder natural dye using the method preparation of the present invention for extracting natural dye from madder has obvious preferable dyeing effect, and specifically, the surface color of stained specimens is deeper, and color fastness is more preferable.
Description
Technical field
The present invention relates to natural dye extraction and colouring arts, and in particular to a kind of side that natural dye is extracted from madder
Method and the natural dye and colouring method prepared by this method.
Background technique
Natural dye is that one kind is good with the compatibility of ecological environment, biodegradable, and the dyestuff of nonhazardous, is a kind of
Very environmentally protective and affine to human body dyestuff, and the raw material for being used to produce these dyestuffs is substantially from plant, moves
It is extracted in the raw materials such as object, mineral and microorganism.Natural dye is in addition to dyeing, and there are also antibacterial anti-inflammatory, anti-oxidant, anti-ultraviolet radiation
The effect of, therefore, natural dye has a wide range of applications in fields in home textile product, ornament etc..
Madder also known as blood activating grass, belong to Rubiaceae, are herbaceos perennials, its root is many in China in orange
Area is all distributed, and adaptability is preferable.Madder can be not only used for extracting natural dye, but also be traditional Chinese medicine, I
Already by its medication, madder, madder, india madder stem and leaf have antitumor, antibacterial and increase quantity of leucocyte in human body state's ancient Chinese medicine
Effect.Either for oral administration or external application, suffers from good performance, is a kind of important Chinese patent drug.Madder in madder
Element has inhibiting effect etc. to staphylococcus aureus, Diplococcus pneumopniae, Bacillus influenzae and dermatophyte.Studies have shown that madder
Dyeing the main component to work is alizarin and its derivative, such as rubican, rubia element.
In the prior art it has been reported that the method for extracting natural dye from madder with organic solvents such as alcohol, ketone, such as
A kind of preparation method of madder haematochrome is disclosed in CN107501992A, this method is using 25% ethanol solution to madder
Root powder extracts.However, the madder natural dye extracted using these organic solvents is in the mistake for being applied to textile dyeing
Dyeing effect obtained in journey is bad, as the textile surface color after dyeing is shallower.
Summary of the invention
The purpose of the invention is to overcome dyeing effect present in the extracted madder natural dye of existing method not
Good defect provides a kind of method that natural dye is extracted from madder and natural dye and dyeing side by this method preparation
Method.
To achieve the goals above, one aspect of the present invention provides a kind of method that natural dye is extracted from madder, the party
Method includes：Madder is cleaned, is dry, is crushed, obtained crushed material is extracted in alkaline aqueous solution, then will be obtained
Extracting solution successively filtered, distilled and be freeze-dried.
Second aspect of the present invention provides the natural dye prepared by the above method.
Third aspect present invention provides a kind of colouring method, and this method includes with containing natural dye, mordant and water
Dye liquor dyes textile, wherein the natural dye is that the madder prepared according to the method described in the present invention naturally contaminates
Material.
It is natural using madder is carried out under alkaline condition of the present invention from the method for extracting natural dye in madder
The extraction of dyestuff can be such that madder color is substantially dissolved in alkaline aqueous solution, not only can obtain higher madder day
Right dyestuff recovery rate, but also preferable natural dye dying effect can be obtained.
Moreover, extraction process of the present invention is simple, the time is short, and extraction process not will cause environmental pollution.Dyeing
Color fastness is good, and dress safety does not have carcinogenesis or causes allergic reaction；It is good with ecological environment compatibility, it can biology
Degradation.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
According to the first aspect of the invention, the method that the present invention provides a kind of extracts natural dye from madder, the party
Method includes：Madder is cleaned, is dry, is crushed, obtained crushed material is extracted in alkaline aqueous solution, then will be obtained
Extracting solution successively filtered, distilled and be freeze-dried.
According to the method described in the present invention, the pigment in madder (such as alizarin, rubican, rubia element) can be sufficiently molten
Solution is in alkaline aqueous solution, so that the madder natural dye thus prepared can obtain preferable dye during textile dyeing
Color effect, in particular, with using organic solvent (such as methanol, ethyl alcohol, ketone) extract madder natural dye compared with, using according to
Textile surface after the natural dye dying that method of the present invention is extracted has relatively deep color.
In method of the present invention, the concentration of the alkaline aqueous solution can be 0.1~5g/L, specifically, such as
Can for 0.1g/L, 0.5g/L, 1g/L, 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L, 4.5g/L, 5g/L and
The arbitrary value in range that any two in these point values are constituted.In the preferred case, the concentration of the alkaline aqueous solution
For 0.3-1g/L.
In method of the present invention, the alkali in the alkaline aqueous solution can be the conventional selection of this field, such as
It can be at least one of sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium carbonate and saleratus.Most preferably
Ground, the alkali are sodium hydroxide.
In method of the present invention, the condition of the extraction may include：Temperature, which is 50-100 DEG C, (such as can be
50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C or 100 DEG C), the time be 1-3 hours (such as
Can be 1h, 1.5h, 2h, 2.5h or 3h), solid-liquid mass ratio 1:10-50 (such as can be 1:10,1:15,1:20,1:25,
1:30,1:35,1:40,1:45,1:50).Herein, solid-liquid mass ratio refers to the mass ratio of crushed material and alkaline aqueous solution.
In method of the present invention, the process of the extraction preferably carries out under stiring.
It, can be real according to the method for this field routine by the madder drying after cleaning in method of the present invention
It applies, such as directly dries the madder after cleaning.
In method of the present invention, dry madder is carried out crushing can be real according to the method for this field routine
It applies, such as dry madder can be mechanically pulverized.In the preferred case, the operation of mechanical crushing with obtain having a size of
0.5-3 millimeters of madder powder.
In method of the present invention, the side preferably using vacuum distillation is distilled to the extracting solution obtained after suction filtration
Formula is implemented.It is highly preferred that by vacuum distillation by the reduction in bulk of extracting solution to the 1/8 to 1/3 of former extracting liquid volume, further
Preferably 1/6 to 1/4.
In method of the present invention, by being freeze-dried available red blocky madder natural fuel.
A preferred embodiment of the invention, the method that natural dye is extracted from madder include：By madder
It cleans, dry, be mechanically pulverized, obtained crushed material is placed in the NaOH solution of 0.1-5g/L, at 50-100 DEG C, stir 1-
3h, wherein solid-liquid mass ratio 1:10-50；Then obtained extracting solution is filtered by vacuum, then through vacuum distillation obtain it is dense
Contracting liquid, by concentrate it is freeze-dried after obtain red blocky dyestuff.
According to the second aspect of the invention, the present invention provides the natural dyes prepared by the above method.According to the present invention
The method can be such that pigment most in madder is substantially dissolved in alkaline aqueous solution, so that is so prepared is natural
Dyestuff can obtain obvious preferable dyeing effect in dyeing course.
According to the third aspect of the invention we, the present invention provides a kind of colouring method, this method includes with containing natural dye
The dye liquor of material, mordant and water dyes textile, wherein the natural dye is according to extraction side of the present invention
The madder natural dye of method preparation.
In the present invention, there is no particular limitation for the mode of the dyeing, can be the conventional selection of this field.The dye
The condition of color may include：Temperature is 50-100 DEG C (such as can be 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C or 100 DEG C), when
Between be 0.5-3 hours (such as can be 0.5h, 1h, 1.5h, 2h, 2.5h or 3h), pH value be 4-11 (such as can for 4,4.5,
5,5.5 or 6), bath raio 1:10-50 (such as can be 1:10,1:20,1:30,1:40 or 1:50).
In the present invention, the mordant can be the conventional selection of this field, such as can be aluminum aluminum sulfate, sulfuric acid
Zinc, ferrous sulfate etc..Most preferably, the mordant is aluminum aluminum sulfate.When the mordant is aluminum aluminum sulfate, institute of the present invention
The madder natural dye stated can obtain preferable dyeing effect.
In the present invention, for the textile of dyeing, there is no particular limitation, can be the weaving to be dyed of any conventional
Product, such as staple in bulk, yarn, fabric or ready-made clothes.
It in the present invention, can be cotton, silk, hair, polyamide fibre or their blending product for the material of the textile of dyeing.
The present invention will be described in detail by way of examples below, but protection scope of the present invention is not limited to that.
In following embodiment and comparative example, madder is purchased from Bozhou City Fang Hai pharmaceutcal corporation, Ltd；Aluminum aluminum sulfate is purchased from upper
Hai Lingfeng chemical reagent Co., Ltd.
Embodiment 1
Madder is cleaned, dry, is mechanically pulverized, the crushed material having a size of 0.5-3 millimeters is obtained.Weigh madder crushing
Object 10g is added in the NaOH solution that 200mL concentration is 0.1g/L, and stirs 60min at 70 DEG C.Then extracting solution is carried out
Vacuum filtration, vacuum distillation is to 50mL, then freeze-dried obtains red blocky madder natural dye.
Silk to be dyed is put into the dye liquor being made of madder natural dye, mordant aluminum aluminum sulfate and water and is contaminated
Color, wherein weighing 2g silk, the quality of madder natural dye accounts for the 4% of silk quality, and the quality of mordant aluminum aluminum sulfate accounts for silk
The 2% of silk fabric quality, bath raio when dyeing are 1:40, it is 5 that dyeing temperature, which is 70 DEG C, dyeing time 60min, dye liquor pH,.Dyeing
Silk afterwards carries out washing drying, obtains stained specimens A1.
Embodiment 2
Madder is cleaned, dry, is mechanically pulverized, the crushed material having a size of 0.5-3 millimeters is obtained.Weigh madder crushed material
10g is added in the NaOH solution that 300mL concentration is 0.5g/L, and stirs 80min at 80 DEG C.Then extracting solution is carried out true
Empty pump filter, vacuum distillation is to 50mL, then freeze-dried obtains red blocky madder natural dye.
Silk to be dyed is put into the dye liquor being made of madder natural dye, mordant aluminum aluminum sulfate and water and is contaminated
Color, wherein weighing 2g silk, the quality of madder natural dye accounts for the 3% of silk quality, and the quality of mordant aluminum aluminum sulfate accounts for cotton
The 3% of yarn qualities, bath raio when dyeing are 1:30, it is 4.5 that dyeing temperature, which is 70 DEG C, dyeing time 60min, dye liquor pH,.
Silk after dyeing carries out washing drying, obtains stained specimens A2.
Embodiment 3
Madder is cleaned, dry, is mechanically pulverized, the crushed material having a size of 0.5-3 millimeters is obtained.Weigh madder crushed material
10g is added in the NaOH solution that 300mL concentration is 1g/L, and stirs 90min at 90 DEG C.Then vacuum is carried out to extracting solution
It filters, vacuum distillation is to 50mL, then freeze-dried obtains red blocky madder natural dye.
Silk to be dyed is put into the dye liquor being made of madder natural dye, mordant aluminum aluminum sulfate and water and is contaminated
Color, wherein weighing 2g silk, the quality of madder accounts for the 3% of silk quality, and the quality of mordant aluminum aluminum sulfate accounts for silk matter
The 4% of amount, bath raio when dyeing are 1:20, it is 4 that dyeing temperature, which is 70 DEG C, dyeing time 60min, dye liquor pH,.After dyeing
Silk carries out washing drying, obtains stained specimens A3.
Embodiment 4
Madder natural dye is extracted according to the method for embodiment 3 and is dyed, the difference is that natural in preparation madder
Alkali in alkaline aqueous solution used in during dyestuff is Na2CO3, to obtain stained specimens A4.
Embodiment 5
Madder natural dye is extracted according to the method for embodiment 3 and is dyed, the difference is that the institute in dyeing course
The mordant used is zinc sulfate, to obtain stained specimens A4.
Comparative example 1
Madder natural dye is extracted according to the method for embodiment 3 and is dyed, the difference is that natural in preparation madder
The ethanol solution that Extraction solvent used in during dyestuff is 25%, to obtain stained specimens D1.
Test case
(1) measurement of stained specimens K/S value
Using color measurement and color match instrument (being purchased from U.S. Datacolor company, model Datacolor110) respectively to implementation
Stained specimens prepared by example 1-5 and comparative example 1 measure, and measure the K/S value of each sample, test result is as follows shown in table 1.
K/S value is bigger, and the surface color for illustrating sample is deeper, and the dye strength of sample surfaces is bigger；The smaller table for illustrating sample of K/S value
Face color is more shallow, and the dye strength of sample surfaces is lower.
(2) test of color fastness
According to the dry friction color of stained specimens prepared by GB/T 3920-2008 method testing example 1-5 and comparative example 1
Fastness, as a result as shown in table 1 below.
According to the resistance to wet friction of stained specimens prepared by GB/T 3920-2008 method testing example 1-5 and comparative example 1
Color fastness, as a result as shown in table 1 below.
According to the solarization color jail of stained specimens prepared by GB/T 8427-2008 method testing example 1-5 and comparative example 1
Degree, as a result as shown in table 1 below.
Table 1
It can be seen that the method preparation for extracting natural dye from madder using of the present invention by the result of table 1
Madder natural dye there is obvious preferable dyeing effect, specifically, the surface color of stained specimens is deeper, and color fastness is more
It is good.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (10)
1. a kind of method for extracting natural dye from madder, this method include：Madder is cleaned, is dry, is crushed, will be obtained
Crushed material extracted in alkaline aqueous solution, then obtained extracting solution is successively filtered, distilled and is freeze-dried.
2. the method according to claim 1, wherein the concentration of the alkaline aqueous solution is 0.1~5g/L.
3. method according to claim 1 or 2, which is characterized in that the alkali in the alkaline aqueous solution is sodium hydroxide, carbon
At least one of sour sodium, sodium bicarbonate, potassium hydroxide, potassium carbonate and saleratus.
4. method according to claim 1 or 2, which is characterized in that the condition of the extraction includes：Temperature is 50-100
DEG C, the time is 1-3 hours, solid-liquid mass ratio 1:10-50.
5. the natural dye of the preparation of the method as described in any one of claim 1-4.
6. a kind of colouring method, this method includes being dyed with the dye liquor containing natural dye, mordant and water to textile,
It is characterized in that, the natural dye is natural dye described in claim 5.
7. according to the method described in claim 6, it is characterized in that, the condition of the dyeing includes：Temperature is 50-100 DEG C, when
Between be 0.5-3 hours, pH value 4-11, bath raio 1:10-50.
8. method according to claim 6 or 7, which is characterized in that the mordant is aluminum aluminum sulfate.
9. method according to claim 6 or 7, which is characterized in that the textile be staple in bulk, yarn, fabric or at
Clothing.
10. method according to claim 6 or 7, which is characterized in that the material of the textile is cotton, silk, hair, polyamide fibre
Or their blending product.
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| CN111500085A (en) * | 2020-04-22 | 2020-08-07 | 南通大学 | Green pigment extracted from radix Rubiae, and extraction method and application thereof |
| CN113174763A (en) * | 2021-05-06 | 2021-07-27 | 苏州大学 | Method for dyeing nylon fabric by using natural dye |
| CN113388263A (en) * | 2021-06-22 | 2021-09-14 | 浙江超凡制衣有限公司 | Green harmless plant dye for thermosensitive clothing material and dyeing method thereof |
| CN114808484A (en) * | 2022-04-15 | 2022-07-29 | 常州大学 | Preparation method of madder and gardenia compound antibacterial cotton fabric |
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| CN114808484A (en) * | 2022-04-15 | 2022-07-29 | 常州大学 | Preparation method of madder and gardenia compound antibacterial cotton fabric |
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Application publication date: 20181130 |
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