CN109021611A - A kind of extracting method and its application of natural plant dye - Google Patents
A kind of extracting method and its application of natural plant dye Download PDFInfo
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- CN109021611A CN109021611A CN201811032235.3A CN201811032235A CN109021611A CN 109021611 A CN109021611 A CN 109021611A CN 201811032235 A CN201811032235 A CN 201811032235A CN 109021611 A CN109021611 A CN 109021611A
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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
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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
- 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
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- 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
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- 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
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to textile dyeing and finishing fields, a kind of extracting method more particularly to rhizome of cyrtomium natural plant dye and its application in dyeing and printing process, the step of extracting method is, 1) by rhizome of cyrtomium impurity removing, clean, dry, it is ground into about 80-150 mesh, is then added in extractant and impregnates, after rhizome of cyrtomium sufficiently soaks, pH adjusting agent is continuously added, the pH value for adjusting solution is about 9-14；Then it is added and extracts auxiliary agent, solution is warming up to about 60-100 DEG C, keep the temperature about 60-180min, filtering；It repeats to extract about 3-5 times, the leaching liquor repeatedly obtained is merged, natural dye stoste is obtained；2) the natural dye stoste that step 1) obtains first is concentrated under reduced pressure, is then freeze-dried, obtains powdered natural dye.Extraction process of the present invention is simple, by the extraction auxiliary agent for selecting to have specific composition, extraction efficiency can be made to have unexpected raising.
Description
Technical field
The invention belongs to textile dyeing and finishing fields, and in particular to a kind of extracting method of rhizome of cyrtomium natural plant dye and its print
Application in dyeing technique.
Background technique
As the improvement of people's living standards, more and more people start to advocate nature and healthy lifestyles, people
It is more more and more intense to the concern consciousness of own health and health care etc., and partially synthetic dyestuff is to human health and ecological environment
Generated harm is more and more noticeable.Existing result of study is it has been shown that have 23 kinds of carcinogenic aromatic amines, more than 100
Kind of synthetic dyestuffs are possible to generate carcinogen, and more than 20 synthetic dyestuffs generate allergy to skin, therefore European Union land in recent years
Regulation of the supervention cloth including prohibitive dye and other chemicals, as European Union 67/648/EC instruction, European Union 2001/C96E/18 refer to
It enables, European Union 2002/61/EC instruction, European Union 2003/3/EC instruction, ECO--Label new standard, chemicals REACH regulation etc., this
Seriously constrain China's textile exports.Moreover, synthetic dyestuffs can also generate a large amount of pollution in the process of production to environment.
Compared with traditional synthetic dyestuffs, natural dye is many with its is unique nontoxic, harmless, pollution-free and is concerned
Can also have healthcare function to human body using Chinese herbal medicine as the natural dye of raw material.For the needs to environmental protection, exploitation is natural
Resource is more urgent.With the raising that people's ecological, environmental protective is realized, in the development trend for increasingly focusing on environmental protection, eco-dyeing and finishing processing
Under, the exploitation and application of natural dye necessarily obtain continuous development.
Natural pigment is from a wealth of sources, it is made to have become the emphasis of new dye exploitation and source.The research of natural dye
It mainly include extraction process, dyeability and upper dye mechanism etc..Asia is concentrated mainly on to the research of natural dye in the world
Continent, especially South Korea, Japan etc..Research about natural dye has become one as technical coopreation among developing countries plan
Part, i.e. United Nations Development Programme (UNDP).Although China is of long standing and well established using the history of natural plants dyeing, synthesizing
After dyestuff replaces natural dye, in addition to some ethnic groups still use vegetable colour to produce artifacts, to natural dye
The research for carrying out system development and utilizing is seldom.At the beginning of 21 century, with the rise of natural dye in the world, the country is to day
The research report of right dyeing is just increasing.
Rhizome of cyrtomium, also known as pass through canal, pass through section, it is fern herbaceos perennial, rhizomes is short, overgrown, pinnate compound leaf, leaflet
It is sickle-shaped.Its is cold in nature, slight bitter, slightly poisonous.Its main component is complicated phloroglucin derivative etc., there is antivirus action, right
Influenza virus has strong inhibition effect, has the effects that clearing heat and detoxicating, expelling parasite, cool blood, hemostasis.Clinically for treating wind-heat sense
It emits, damp and hot ecchymosis, haematemesis, the diseases such as hematochezia and metrorrhagia and metrostaxis.
The pigment composition content of rhizome of cyrtomium is very high, can be used as a kind of natural brown dyestuff and is dyed, printed to textile
Flower, also have the function of it is antibacterial, antiviral, mosquito larvae can be killed etc..Therefore, a kind of brown natural dye is extracted from rhizome of cyrtomium and is answered
For textile dyeing, the shelves of textile are improved for expanding natural dye chromatography and application range, development functionality textile
Secondary and added value, has a very important significance.
A kind of extracting method of rhizome of cyrtomium natural dye as disclosed in Chinese patent CN01177542A passes through elder generation in this method
Plant rhizome of cyrtomium is cleaned, is dried, is mechanically pulverized, is then added in 5~20 times of aqueous solutions and impregnates, after rhizome of cyrtomium sufficiently soaks,
Sodium hydroxide, sodium carbonate, sodium metasilicate or sodium phosphate is added, the pH for adjusting solution is 10~13, is warming up to 95~100 DEG C, heat preservation
60~90min, filtering；Filter residue continues to be extracted with the aqueous slkali that pH is 10~13, and filtering merges leaching liquor twice, obtains and naturally contaminate
Expect stoste；Then, by the concentration of rhizome of cyrtomium natural dye stoste, solidification, the crushing of extraction, powdered natural dye is obtained.Though this method
A kind of extraction process of rhizome of cyrtomium is so given, still, the technique is relatively low to the recovery rate of natural pigment contained by rhizome of cyrtomium on the whole.
As Institutes Of Technology Of Zhejiang's master thesis " extraction and its application on cotton fabric of natural dye " discloses
For the traditional extraction technique of rhizome of cyrtomium natural dye, wherein optimal extraction conditions are as follows: 10g/L promotor ZS-l, temperature 100
DEG C, time 180min, material ratio 1:30, extraction time 2 times.But the document does not refer to promotor ZS-l used in the whole text
Specifically what substance.
Summary of the invention
For this purpose, technical problems to be solved in this application are how to improve existing rhizome of cyrtomium natural dye extraction process to passing through
The recovery rate of many natural dyes (that is, the effective component that can be used as pigment), and how to utilize the rhizome of cyrtomium natural dye pair
The method that real silk fabric is dyed.
In order to solve the above technical problems, present inventor is by the research conscientiously with effort, it was found that one kind has
Synergistic extraction process, by optimizing adjustment to process conditions when extracting, especially into specific group
At extraction auxiliary agent, can significantly improve the recovery rate of rhizome of cyrtomium natural dye, thus solve the above technical problem.Of the invention
Technical solution is as follows: the invention discloses a kind of extracting methods of rhizome of cyrtomium natural dye, include the following steps:
1) by rhizome of cyrtomium impurity removing, clean, dry, be ground into about 80-150 mesh, be then added in extractant and impregnate, to
After rhizome of cyrtomium sufficiently soaks, pH adjusting agent is continuously added, the pH value for adjusting solution is about 9-14；Then it is added and extracts auxiliary agent, it will
Solution is warming up to about 60-100 DEG C, keeps the temperature about 60-180min, filtering；It repeats to extract about 3-5 times, the leaching liquor that will repeatedly obtain
Merge, obtains natural dye stoste；
2) the natural dye stoste that step 1) obtains first is concentrated under reduced pressure, is then freeze-dried, obtains powdered natural dye
Material.
The extractant is the mixed solvent of ethyl alcohol and water, and the volume content of ethyl alcohol is about 50- about 80v.%, with mixing
On the basis of the total volume of solvent.
The pH adjusting agent is preferably hydroxide, carbonate, silicate and/or the phosphate of alkali metal, more excellent
It is selected as sodium hydroxide, sodium carbonate, sodium metasilicate and/or sodium phosphate.
The extraction auxiliary agent is clay, can be selected from kaolin, bentonite and attapulgite；Preferably bentonite and bumps
The mixture of stick stone, wherein bentonitic content is about 30- about 50wt.%, even more preferably about 35- about 45wt.%, more preferably
About 40wt.%.The bentonite is preferably sodium bentonite and organobentonite, more preferably organobentonite.
The organobentonite can choose commercial product, and following methods preparation can also be used:
First using water as decentralized medium, impurity in bentonite is removed, the suspension that bentonite content is about 15-18wt.% is made
Liquid, then high speed shear dispersion is carried out, so that granularity is reached clay grade；It is with containing at least one group carbon atom number by the slurries
The quaternary ammonium reactant salt of 15-24, the quaternary ammonium salt are about the 20-40wt.% of bentonite consumption, when suitably heating, and controlling reaction
PH value meta-alkalescence；Then it is filtered, washed, in room temperature to drying at 50 DEG C.
The additive amount for extracting auxiliary agent is preferably 5-30g/L, on the basis of the volume of solution；More preferably 10-25g/
L；More preferably 15g/L.
Material ratio in the step 1), that is, rhizome of cyrtomium raw material weight ratio/(extractant and the rhizome of cyrtomium original being added in extractant
The weight of acquired solution after material mixing), preferably 0~1:50 of 1:1, more preferably 1:20~1:40, most preferably 1:25.
The smashed partial size of rhizome of cyrtomium raw material is preferably from about 100-130 mesh, more preferably 120 mesh in the step 1)；Solution
PH value be preferably from about 10-13, more preferably 11；Temperature when extraction is preferably from about 70-90 DEG C, even more preferably about 80 DEG C；Leaching
Mentioning the time is preferably from about 80-160min, more preferably about 120min；Extraction time is preferably 4 times.
The rhizome of cyrtomium natural dye obtained disclosed herein as well is the extracting method is knitted in real silk fabric, wool product, cotton
Application in object dyeing.
1, rhizome of cyrtomium natural dye is configured under conditions of not having to mordant by dye liquor using conventional direct staining method,
Real silk fabric or wool product are dyed, then washes, is dry, then being soaped, washed and dried, can be obtained brown
Real silk fabric or wool product.
2, using mordant dyeing after conventional first dyeing, rhizome of cyrtomium natural dye is first configured to dye liquor, to real silk fabric or sheep
Woolen is dyed, and then washes, is dry, then being soaped, washed and dried, mixed chlorinated rare earth, such as chlorine is then added
Change the mixture of lanthanum and cerium chloride, carry out mordant dyeing, then washes, is dry, then being soaped, washed and dried, can be obtained Huang
The real silk fabric or wool product of brown.
3, using mordant dyeing after conventional first dyeing, rhizome of cyrtomium natural dye is first configured to dye liquor, to real silk fabric or sheep
Woolen is dyed, and then washes, is dry, then being soaped, washed and dried, Metal aluminum salt, such as sulfuric acid is then added
Aluminium carries out mordant dyeing, then washes, is dry, then being soaped, washed and dried, can be obtained real silk fabric or the sheep of rufous
Woolen.
4, using mordant dyeing after conventional first dyeing, rhizome of cyrtomium natural dye is first configured to dye liquor, to real silk fabric or sheep
Woolen is dyed, and then washes, is dry, then being soaped, washed and dried, metal ferrous salt, such as sulphur is then added
It is sour ferrous, carry out mordant dyeing, then wash, is dry, then being soaped, washed and dried, can be obtained brown real silk fabric or
Wool product.
5, using conventional direct staining method, cotton fabric is used to commercially available cation modifier and polyethylene glycol respectively first
Successively it is modified；Rhizome of cyrtomium natural dye is then configured to dye liquor, cotton fabric is dyed；Then it washes, is dry, then into
Row is soaped, washes and is dried, and can be obtained the cotton fabric of brown.
The application has the beneficial effect that
1, compared with existing natural dye extracts, extraction process of the present invention is simple, by introducing particular kind of extraction
Auxiliary agent can be such that extraction efficiency obviously increases；And preparation process is very friendly to environment, not will cause environmental pollution.
2, the extracted rhizome of cyrtomium natural dye of the application not only has nontoxic, harmless, pollution-free, biodegradable, environment
The strong advantage of compatibility, and be used for real silk fabric, wool product, cotton fabric dyeing process when with excellent color fastness.
3, using dyed fabric made from the extracted rhizome of cyrtomium natural dye of the application or product using safe, with human body flesh
Skin, which directly contacts, there will not be carcinogenic, teratogenesis or causes allergic reaction；But also there is certain medicinal health-care effect, it can
Play the role of antibacterial anti-inflammatory, and can mosquito-proof sting.
4, obtain that color is uniform, color is soft using dyed fabric made from the extracted rhizome of cyrtomium natural dye of the application or product
With typical case naturally, the aesthetic needs of modern can be met；And different face can be obtained by selecting different mordants
Color, such as brown, rufous, yellowish-brown, brown.
Other advantage will be partly show in the following description, and can be partly able to by specific embodiment
Understand.Especially by point out in the dependent claims Chemical composition that, method and combinations thereof, will realize and obtain down
State advantage.It should be appreciated that general description and detailed description below above is merely exemplary and illustrative, rather than
It is restrictive.
Complementary definition
Material, compound, composition and component described herein, can be used for method and composition described herein,
Or it can be in connection or the production that can be used for implementing the method and prepare the composition or obtained as the method
Product.It should be appreciated that when disclosing combination, subset, interaction, the group etc. of these materials, although may not clearly have
Body refers to each and collective combinations and arrangement of these compounds, but specifically considers and describe wherein in this application
Each.For example, extracting adjuvant component if disclosing and discussing, and a variety of alternative solid-state forms of the component are discussed,
Then unless there is specific opposite instruction, each possible for referring to adjuvant component and solid-state form is otherwise specifically considered
Combination and permutation.The concept is suitable for all aspects of the application, is including but not limited to making and using disclosed combination
Step in the method for object.Therefore, if there is the multiple other steps that can be executed, then it should be appreciated that these are other
Each of step can be executed by the combination of any specific embodiment or multiple embodiments of disclosed method,
And each such combination is specifically considered, they should be considered as disclosing.
In claims in this specification and its later, refer to many terms, they should be defined as with
Lower meaning:
It must be noted that unless context is in addition clearly stipulate that otherwise such as institute in this specification and appended claims
Not only may include a referring to thing with, singular " one ", "/kind " and " should/described ", but may include multiple referring to thing (i.e.
Two or more, including two).Thus, for example, referring to that " pH adjusting agent " may include single pH adjusting agent or two
Kind or more mixture of pH adjusting agent, etc..
Unless otherwise specified, therefore it and may include in the model about that the numberical range in the application, which is,
Enclose outer value.The numberical range can be expressed as in the application from " about " particular value and/or to " about " another particular value.
It on the other hand include from one particular value and/or to another particular value when stating such range.Similarly,
When value is expressed as approximation by using antecedent " about ", it should be understood that the particular value is formed on the other hand.Also answer
Work as understanding, the endpoint of each in numberical range is important and independently of another end in the relationship with another endpoint
Point.
The parts by weight of element-specific or component in composition or product are referred in specification and last claims
Refer to the weight relationships stated in composition or product between the element or component and any other element or component with parts by weight.
Therefore, in the composition comprising 2 parts by weight of component X and 5 parts by weight of component Y, X and Y exist with the weight ratio of 2:5, and nothing
It whether include that other component exists with the ratio by composition.
Unless specifically stated to the contrary meanings, ways customary is dark or in context or technical field based on context
Show, all scores and percentage otherwise referred in the application are by weight, and the weight percent of component be based on comprising
The composition of the component or the total weight of product.
"comprising", " comprising ", " having " and the similar terms referred in the application are not intended to exclude any optional group
Divide, the presence of step or program, regardless of whether specifically disclosing any optional component, step or program.It is doubted in order to avoid any
It asks, unless may include otherwise that one or more are additional by using all methods that term "comprising" requires there are state otherwise
Step, equipment part or component part and/or substance.In contrast, term " by ... form " exclude be not specifically delineated or
Any component, step or the program enumerated.Unless otherwise stated, otherwise term "or" refers to individually and in any combination
The member enumerated.
In addition, the side that the content of any referenced patent document or non-patent literature is all quoted in its entirety in the application
Formula is incorporated herein, especially with respect to disclosed in fields definition (any definition not provided specifically with the application not
Under unanimous circumstances) and common sense.
Specific embodiment
Iing is proposed the following example is to provide how to be made and evaluate the application institute to those skilled in the art
Entire disclosure and the description of compound state and claimed, composition, product, device and/or method,
And it is intended only to be illustrative, is not intended to be limiting the range that inventor is considered as its invention.Effort has been made to ensure
About the accuracy of digital (such as amount, temperature etc.), but it is contemplated that some errors and deviation.Unless otherwise specified, no
Then number is parts by weight, and temperature is DEG C to indicate or under environment temperature, and pressure is atmospheric pressure or close to atmospheric pressure.
There are reaction condition (such as concentration of component, required solvent, solvent mixture, temperature, pressure and other reaction ranges) and
It can be used for optimizing a variety of variations and combination of the condition of the product purity and yield that obtain by the method.It will only need
Reasonable routine experiment optimizes such method condition.
Embodiment 1:
It by rhizome of cyrtomium impurity removing, cleans, dry, be ground into 80 mesh, the in the mixed solvent for being then added to ethyl alcohol and water is soaked
Bubble, material ratio 1:10, and the volume content of in the mixed solvent ethyl alcohol is 50v.%, on the basis of the total volume of mixed solvent.
After rhizome of cyrtomium sufficiently soaks, sodium carbonate is continuously added, the pH value for adjusting solution is 9；Then it is added and extracts the organic swelling of auxiliary agent-
The mixture of soil and attapulgite, wherein the additive amount for extracting auxiliary agent is 5g/L, and the content of organobentonite in the mixture
For 30wt.%；Solution is warming up to about 60 DEG C, keeps the temperature about 180min, filtering；It repeats to extract about 3 times, the extraction that will repeatedly obtain
Liquid merges, and obtains natural dye stoste；
Then, the natural dye stoste of acquisition is first concentrated under reduced pressure, is then freeze-dried, obtains powdered rhizome of cyrtomium and naturally contaminate
Material.
Organobentonite used in it is prepared using following methods:
First using water as decentralized medium, impurity in bentonite is removed, the suspension that bentonite content is about 16wt.% is made,
High speed shear dispersion is carried out again, and granularity is made to reach clay grade；It is 20 by the slurries and containing at least one group carbon atom number
Quaternary ammonium reactant salt, the quaternary ammonium salt are about the 30wt.% of bentonite consumption, and pH value when being heated to 60 DEG C, and controlling reaction is
8；Then it is filtered, washed, is dry at 45 DEG C.
Using conventional direct staining method, under conditions of not having to mordant, obtained rhizome of cyrtomium natural dye is prepared
At dye liquor, real silk fabric or wool product are dyed, then washes, is dry, then being soaped, washed and dried
Obtain the real silk fabric or wool product of brown.
Embodiment 2
It by rhizome of cyrtomium impurity removing, cleans, dry, be ground into 150 mesh, the in the mixed solvent for being then added to ethyl alcohol and water is soaked
Bubble, material ratio 1:50, and the volume content of in the mixed solvent ethyl alcohol is 80v.%, on the basis of the total volume of mixed solvent.
After rhizome of cyrtomium sufficiently soaks, sodium hydroxide is continuously added, the pH value for adjusting solution is 14；Then it is added and extracts auxiliary agent-organic bentonite
The mixture of profit soil and attapulgite, wherein the additive amount for extracting auxiliary agent is 30g/L, and organobentonite containing in the mixture
Amount is 50wt.%, and solution is warming up to about 100 DEG C, keeps the temperature about 60min, filtering；It repeats to extract about 5 times, the leaching that will repeatedly obtain
Extract merges, and obtains natural dye stoste；
Then, the natural dye stoste of acquisition is first concentrated under reduced pressure, is then freeze-dried, obtains powdered rhizome of cyrtomium and naturally contaminate
Material.
Organobentonite used is made according to the extracting method of embodiment 1.
Embodiment 3
It by rhizome of cyrtomium impurity removing, cleans, dry, be ground into 100 mesh, the in the mixed solvent for being then added to ethyl alcohol and water is soaked
Bubble, material ratio 1:20, and the volume content of in the mixed solvent ethyl alcohol is 60v.%, on the basis of the total volume of mixed solvent.
After rhizome of cyrtomium sufficiently soaks, sodium hydroxide is continuously added, the pH value for adjusting solution is 10；Then it is added and extracts auxiliary agent-organic bentonite
The mixture of profit soil and attapulgite, wherein the additive amount for extracting auxiliary agent is 10g/L, and organobentonite containing in the mixture
Amount is 35wt.%, and solution is warming up to about 70 DEG C, keeps the temperature about 160min, filtering；It repeats to extract about 4 times, the leaching that will repeatedly obtain
Extract merges, and obtains natural dye stoste；
Then, the natural dye stoste of acquisition is first concentrated under reduced pressure, is then freeze-dried, obtains powdered rhizome of cyrtomium and naturally contaminate
Material.
Organobentonite used is made according to the extracting method of embodiment 1.
Embodiment 4
It by rhizome of cyrtomium impurity removing, cleans, dry, be ground into 130 mesh, the in the mixed solvent for being then added to ethyl alcohol and water is soaked
Bubble, material ratio 1:40, and the volume content of in the mixed solvent ethyl alcohol is 70v.%, on the basis of the total volume of mixed solvent.
After rhizome of cyrtomium sufficiently soaks, sodium phosphate is continuously added, the pH value for adjusting solution is 13；Then it is added and extracts the organic swelling of auxiliary agent-
The mixture of soil and attapulgite, wherein the additive amount for extracting auxiliary agent is 25g/L, and the content of organobentonite in the mixture
For 45wt.%, solution is warming up to about 90 DEG C, keeps the temperature about 80min, filtering；It repeats to extract about 4 times, the extraction that will repeatedly obtain
Liquid merges, and obtains natural dye stoste；
Then, the natural dye stoste of acquisition is first concentrated under reduced pressure, is then freeze-dried, obtains powdered rhizome of cyrtomium and naturally contaminate
Material.
Organobentonite used is made according to the extracting method of embodiment 1.
Embodiment 5
It by rhizome of cyrtomium impurity removing, cleans, dry, be ground into 120 mesh, the in the mixed solvent for being then added to ethyl alcohol and water is soaked
Bubble, material ratio 1:25, and the volume content of in the mixed solvent ethyl alcohol is 65v.%, on the basis of the total volume of mixed solvent.
After rhizome of cyrtomium sufficiently soaks, sodium phosphate is continuously added, the pH value for adjusting solution is 11；Then it is added and extracts the organic swelling of auxiliary agent-
The mixture of soil and attapulgite, wherein the additive amount for extracting auxiliary agent is 15g/L, and the content of organobentonite in the mixture
For 40wt.%, solution is warming up to about 80 DEG C, keeps the temperature about 120min, filtering；It repeats to extract about 4 times, the extraction that will repeatedly obtain
Liquid merges, and obtains natural dye stoste；
Then, the natural dye stoste of acquisition is first concentrated under reduced pressure, is then freeze-dried, obtains powdered rhizome of cyrtomium and naturally contaminate
Material.
Organobentonite used is made according to the extracting method of embodiment 1.
Embodiment 6
Preparation process is substantially the same manner as Example 5, and difference is only that: bentonite used is sodium bentonite.
Embodiment 7
Preparation process is substantially the same manner as Example 5, and difference is only that: bentonite used is commercially available organobentonite.
Embodiment 8
Preparation process is substantially the same manner as Example 5, and difference is only that: extraction auxiliary agent used is only single organic swelling
Soil.
Embodiment 9
Preparation process is substantially the same manner as Example 5, and difference is only that: extraction auxiliary agent used is only single concave convex rod
Soil.
Embodiment 10
Preparation process is substantially the same manner as Example 5, and difference is only that: extraction auxiliary agent used is only single kaolin.
Embodiment 11
Preparation process is substantially the same manner as Example 5, and difference is only that: extraction auxiliary agent used be kaolin, bentonite and
The mixture of attapulgite, the weight ratio of three are 1:1:1.
Embodiment 12
Preparation process is substantially the same manner as Example 5, and difference is only that: swollen in the mixture of organobentonite and attapulgite
The content of profit soil is 25wt.%.
Embodiment 13
Preparation process is substantially the same manner as Example 5, and difference is only that: swollen in the mixture of organobentonite and attapulgite
The content of profit soil is 55wt.%.
Comparative example 1
Preparation process is substantially the same manner as Example 5, and difference is only that: the smashed partial size of rhizome of cyrtomium raw material is 70 mesh, solution
PH value be 8, the in the mixed solvent alcohol volume content as extractant be 40v.%, repeat extract 2 times.
Comparative example 2
Preparation process is substantially the same manner as Example 5, and difference is only that: the smashed partial size of rhizome of cyrtomium raw material is 160 mesh, solution
PH value be 15, the in the mixed solvent alcohol volume content as extractant be 90v.%, repeat extract 5 times.
Comparative example 3
Preparation process is substantially the same manner as Example 5, and difference is only that: the additive amount for extracting auxiliary agent is 4g/L, material
Than for 1:5.
Comparative example 4
Preparation process is substantially the same manner as Example 5, and difference is only that: the additive amount for extracting auxiliary agent is 35g/L, material
Than for 1:55.
Comparative example 5
Preparation process is substantially the same manner as Example 5, and difference is only that: the additive amount for extracting auxiliary agent is 4g/L, material
Than for 1:25.
Comparative example 6
Preparation process is substantially the same manner as Example 5, and difference is only that: extractant is only water, rather than the mixing of ethyl alcohol and water
Solvent.
Comparative example 7
Preparation process is substantially the same manner as Example 5, and difference is only that: extractant is only ethyl alcohol, rather than ethyl alcohol and water is mixed
Bonding solvent.
Comparative example 8
Preparation process is substantially the same manner as Example 5, and difference is only that: being not added with extraction auxiliary agent.
Comparative example 9
According to the preparation process of CN01177542A embodiment 1, wherein filter residue is extracted with 10 times of aqueous solutions.
Recovery rate test and test result
The recovery rate of the rhizome of cyrtomium natural dye of embodiment 1-7, comparative example 1-8 preparation process is tested respectively, is tested
The results are shown in Table 1.
The weight of the powdered rhizome of cyrtomium natural dye for the recovery rate (%) of rhizome of cyrtomium natural dye=finally obtain/smashed
Rhizome of cyrtomium raw material weight.
Table 1- recovery rate data
It can be seen that the application by the way that extracting factor is groped and improved, one is logical from the test result of table 1
It crosses and uses the mixed solvent with specific composition as extractant, the second is being helped by introducing particular kind of clay as extraction
Agent, so that occurring raising beyond expectation to the recovery rate of rhizome of cyrtomium natural dye；Also, by embodiment 5 and embodiment
The recovery rate of 8-13 is compared, and has also been well demonstrated that while having used organobentonite and attapulgite as extraction auxiliary agent, the two
Really synergistic function is produced.
In text of the statement, various publications are referred to.Disclosures of these publications full text is accordingly with reference side
During formula is incorporated herein, so that compound, composition and method described herein is described more fully with.
Various modifications and change can be made to compound described herein, composition and method.In view of specification and
The practice of compound, composition and method disclosed in the present application, compound described herein, composition and method it is other
Aspect will be evident.Specification and example are intended to be considered as illustrative.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (8)
1. a kind of extracting method of rhizome of cyrtomium natural dye, it is characterised in that the step of this method is as follows:
1) by rhizome of cyrtomium impurity removing, clean, dry, be ground into about 80-150 mesh, be then added in extractant and impregnate, to rhizome of cyrtomium
Sufficiently after wetting, pH adjusting agent is continuously added, the pH value for adjusting solution is about 9-14；Then it is added and extracts auxiliary agent, by solution
It is warming up to about 60-100 DEG C, keeps the temperature about 60-180min, filtering；It repeats to extract about 3-5 times, the leaching liquor repeatedly obtained is merged,
Obtain natural dye stoste；
2) the natural dye stoste that step 1) obtains first is concentrated under reduced pressure, is then freeze-dried, obtains powdered natural dye.
2. extracting method according to claim 1, the extractant is the mixed solvent of ethyl alcohol and water, the volume of ethyl alcohol
Content is 50-80v.%, on the basis of the total volume of mixed solvent.
3. extracting method according to claim 1, the pH adjusting agent is preferably the hydroxide of alkali metal, carbonic acid
Salt, silicate and/or phosphate.
4. extracting method according to claim 1, described extracts the mixture that auxiliary agent is bentonite and attapulgite,
In bentonitic content be preferably 30-50wt.%.
5. extracting method according to claim 4, the bentonitic content is preferably 35-45wt.%.
6. extracting method according to claim 4, the bentonite is preferably sodium bentonite and/or organobentonite.
7. extracting method according to claim 1, the smashed partial size of rhizome of cyrtomium raw material is preferably 100- in the step 1)
130 mesh；The pH value of solution is preferably 10-13；Temperature when extraction is preferably from about 70-90 DEG C；Extraction time is preferably from about 80-
160min；Extraction time is preferably 4 times.
8. rhizome of cyrtomium natural dye made from extracting method described in any one of -7 is in real silk fabric, wool system according to claim 1
Application in product, cotton fabric dyeing process.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110424169A (en) * | 2019-08-06 | 2019-11-08 | 安徽恒益纺织科技有限公司 | A kind of textile fabric environmentally friendly coloring agent and preparation method thereof |
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| CN104353333A (en) * | 2014-10-21 | 2015-02-18 | 青岛智谷创新技术有限公司 | Methanal purifying agent based on traditional Chinese medicine components |
| CN106381244A (en) * | 2016-08-26 | 2017-02-08 | 华侨大学 | Tea saponin handmade soap |
| CN107488363A (en) * | 2017-06-05 | 2017-12-19 | 中国科学院兰州化学物理研究所 | Utilize the method for attapulgite absorption stabilization of carotenoids class antioxidation activity natural pigment |
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| US5593458A (en) * | 1995-03-16 | 1997-01-14 | Ocean Wash, Inc. | Process and composition for decorating a dyed cloth fabric |
| CN101177542A (en) * | 2007-11-16 | 2008-05-14 | 浙江理工大学 | Method for preparing aspidium rhizoma natural dye and product thereof |
| CN104353333A (en) * | 2014-10-21 | 2015-02-18 | 青岛智谷创新技术有限公司 | Methanal purifying agent based on traditional Chinese medicine components |
| CN106381244A (en) * | 2016-08-26 | 2017-02-08 | 华侨大学 | Tea saponin handmade soap |
| CN107488363A (en) * | 2017-06-05 | 2017-12-19 | 中国科学院兰州化学物理研究所 | Utilize the method for attapulgite absorption stabilization of carotenoids class antioxidation activity natural pigment |
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| CN110424169A (en) * | 2019-08-06 | 2019-11-08 | 安徽恒益纺织科技有限公司 | A kind of textile fabric environmentally friendly coloring agent and preparation method thereof |
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