A kind of green peel of walnut multifunction finishing agent of high extraction and preparation method thereof
Technical field
The invention belongs to textile material technical fields, and in particular to a kind of green peel of walnut multifunction finishing agent of high extraction
And preparation method thereof.
Background technique
Green peel is the young fruit of rutaceae orange and plantation mutation or the drying pericarp of immature fruit.Juglans plants
In include fruit in green green peel also belong to one kind of green peel.Carbohydrate rich in, protein, amino in green peel of walnut
Acid, inorganic salts and vitamin etc. also have phenols, flavanone, naphthoquinones class bioactive substance, therefore green peel is normal since ancient times
It is used as Chinese medicine, has effects that dispersing stagnated hepatoqi, disperse accumulationization be stagnant, relieving distension and oppression.Therefore green peel of walnut is applied into woven face
It can also assign fabric new function in material, improve the added value of fabric.
Chinese patent CN 102516804B it is disclosed by green peel of walnut dye liquor of green peel of walnut preparation and preparation method thereof with
And the method dyed with its most fabric, green peel of walnut is dried into black, then after crushing cleaning, dechlorinated softening hot water is clear
The dust on surface is washed, then is soaked in filtering and concentrating in lye and obtains green peel filtrate, then uses green vitriol and chlorination
Sodium dyes fabric through mordant dyeing color method as medium, and the fabric suitable for baby is prepared.Chinese patent CN
A kind of antioxidant of the peel extract containing Queensland nut disclosed in 104323395A and the preparation method and application thereof, by Australia heavily fortified point
Fruit takes green peel after spontaneously drying, and green peel is crushed to be formed powdered, is then mentioned with ethyl alcohol, acetone, isobutanol or ethyl acetate
It takes, is concentrated, until organic solvent volatilizees completely obtains Queensland nut peel extract, finally dissolves Queensland nut peel extract
In above-mentioned organic solvent, standing obtains the antioxidant of the peel extract containing Queensland nut.By the above-mentioned prior art it is found that mesh
Application of the preceding green peel of walnut in terms of weaving is mostly that pigment or functional component are extracted by organic solvent, and green peel of walnut is mentioned
Take object that fabric is dyed or arranged as dyestuff or functional finishing agent, but the extraction gimmick of walnut peel extract
Simply, recovery rate is limited, is still wasted there are many resource.The dye of Cortex walnut plant disclosed in Chinese patent CN 102172937B
Walnut husk is banked up fermentation and is dried to obtain auburn blocky dye for fabrics raw material, fabric is contaminated by the method for material dye bamboo chip
Material raw material is ground into dye powder, adds bleeding agent, bath foam water and bamboo chip and is disseminated, and taking-up bamboo chip washing, which is dried, to be contaminated
The bamboo chip of color.Dye powder is prepared using fermentation technique to dye bamboo chip, takes full advantage of the ingredient inside green peel, still
Hot fermentation can cause certain injury, therefore, research and develop a kind of green peel of walnut of high extraction to the active constituent inside green peel
Extracting method seems very necessary.
Applicant of the present invention combines low temperature enzyme fermentation with solvent extraction techniques, and the walnut for preparing high extraction is green
Skin finishing agent remains pigment, antimicrobial component, antioxidant content and pro-skin ingredient etc. in green peel of walnut to greatest extent, makes
The finishing agent of preparation has several functions.
Summary of the invention
The technical problem to be solved in the present invention is to provide the green peel of walnut multifunction finishing agents and its system of a kind of high extraction
Preparation Method, using the green peel of walnut of freeze-drying as raw material, after low temperature enzyme fermentation, successively through ethanol water and methanol solution
Extraction obtains first-time filtrate and secondary filtrate, and secondary filtrate is added microcapsules and forms sustained release agent, and auxiliary agent is added after the two is combined
Form green peel of walnut multifunction finishing agent.Preparation method of the present invention is simple, using the extracting method of multiple low-cost high-efficiency, system
It is standby to obtain the multi-functional green peel of walnut finishing agent of high extraction, the effective component of green peel of walnut is made full use of, waste is reduced.
In order to solve the above technical problems, the technical scheme is that
A kind of green peel of walnut multifunction finishing agent of high extraction, the green peel of walnut multifunction finishing agent of the high extraction
In include green peel pigment, phenolic compound, flavanone compound, naphthoquinone compound and auxiliary agent, the core of the high extraction
It further include Microencapsulated Slow ingredient in peach green peel multifunction finishing agent, the auxiliary agent is surfactant.
As a preferred embodiment of the above technical solution, the green peel of walnut multifunction finishing agent of the high extraction is by enzyme solutions low temperature
Fermentation is prepared in conjunction with multiple solvent extraction techniques.
The present invention also provides a kind of preparation methods of the green peel of walnut multifunction finishing agent of high extraction, including following step
It is rapid:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying forms pretreated walnut
Green peel, will be added enzyme solutions in pretreated green peel, cold fermentation obtains the tunning of green peel of walnut;
(2) tunning of the green peel of walnut of step (1) preparation is broken into mud, be added in an Extraction solvent, ultrasound
After processing, heating stirring filters to obtain first-time filtrate and a filter residue;
(3) filter residue by step (2) preparation is added in second extraction solvent, after ultrasonic treatment, heating stirring, and filtering
Secondary filtrate and secondary filter residue are obtained, microcapsule wall material will be added in secondary filtrate, stirs, obtains sustained release agent;
(4) sustained release agent of first-time filtrate and step (3) preparation in step (2) is merged, surfactant, stirring is added
Uniformly, purification is concentrated to get the green peel of walnut multifunction finishing agent of high extraction.
As a preferred embodiment of the above technical solution, in the step (1), the length of pretreated green peel of walnut is lower than 1cm.
As a preferred embodiment of the above technical solution, in the step (1), the mass fraction of enzyme solutions is 3-5%, and the enzyme is
Fermenting enzyme.
As a preferred embodiment of the above technical solution, in the step (1), the solid-liquid ratio of pretreated green peel and enzyme solutions is
1g:8-10ml。
As a preferred embodiment of the above technical solution, in the step (2), Extraction solvent is ethanol water, ethyl alcohol with
The volume ratio of water is 2-4:1.
As a preferred embodiment of the above technical solution, in the step (3), second extraction solvent is methanol.
As a preferred embodiment of the above technical solution, in the step (3), the microcapsule wall material is gelatin.
As a preferred embodiment of the above technical solution, in the step (4), the surfactant is paregal O.
Compared with prior art, the invention has the following advantages:
(1) the green peel of walnut multifunction finishing agent of high extraction prepared by the present invention uses the core of first freeze-dried processing
Peach green peel can eliminate the moisture in fresh green peel of walnut as raw material, the freeze-dried processing of fresh green peel of walnut
Meanwhile the effective component in green peel of walnut, the fermentation and extraction technique after being conducive to are remained to greatest extent.
(2) the green peel of walnut multifunction finishing agent of high extraction prepared by the present invention first uses enzymatic treatment cold fermentation skill
Art, enzymatic treatment can most fast cellulose macromolecule and protein macromolecule by green peel of walnut be decomposed into lesser molecule,
Accelerate the speed decomposed in conjunction with cold fermentation technology, and does not influence pigment, phenolic compound, flavanone in peach skin green peel
Object, naphthoquinone compound are closed, solvent extraction is fast and effective after being more conducive to.
(3) the green peel of walnut multifunction finishing agent of high extraction prepared by the present invention is using solution extractive technique twice, first
It is extracted with ethanol water, again with methanol is extracted, in conjunction with ultrasonic wave added and heating stirring technology, the effective component in green peel of walnut is fast
Speed efficiently extracts.
(4) in addition, also carrying out Microencapsulated Slow processing to secondary filtrate, be conducive to finishing agent and fabric is effectively made for a long time
With qucik-acting agent is combined with sustained release agent, the finishing agent of multifunction long-acting is prepared.
(5) preparation method of the green peel of walnut multifunction finishing agent of high extraction prepared by the present invention is simple and efficient, by core
Effective component in peach green peel is sufficiently extracted, and antibacterial, anti-oxidant and pro-skin finishing agent is prepared, but also can be to weaving
Product carry out plant dyeing, and color fastness is high.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying formation length is lower than 1cm's
The fermentation enzyme solutions that the mass fraction of 8ml is 3% will be added, 40 in pretreated green peel of walnut in the pretreated green peel of 1g
Cold fermentation 1d obtains the tunning of green peel of walnut at DEG C.
(2) tunning of green peel of walnut is broken into mud, is 1g:30ml with solid-liquid ratio, addition volume ratio is 2:1 ethyl alcohol
In aqueous solvent, after being ultrasonically treated 30min, the heating stirring 30min at 60 DEG C filters to obtain first-time filtrate and a filter residue;
(3) it is 1g:10ml with solid-liquid ratio, a filter residue is added in methanol, 60min is ultrasonically treated, is heated at 60 DEG C
Stir 30min, filter mass fraction be 10% secondary filtrate, be 10ml:1g with solid-liquid ratio, it is bright by being added in secondary filtrate
Glue stirs 20min at 50 DEG C, obtains sustained release agent
(4) first-time filtrate and sustained release agent are merged, paregal O surfactant is added, stirs evenly, purification is concentrated to get
Mass fraction is the green peel of walnut multifunction finishing agent of the high extraction of 10-25%.
Embodiment 2:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying formation length is lower than 1cm's
The fermentation enzyme solutions that the mass fraction of 10ml is 5% will be added, 50 in pretreated green peel of walnut in the pretreated green peel of 1g
Cold fermentation 2d obtains the tunning of green peel of walnut at DEG C.
(2) tunning of green peel of walnut is broken into mud, is 1g:50ml with solid-liquid ratio, addition volume ratio is 4:1 ethyl alcohol
In aqueous solvent, after being ultrasonically treated 30min, the heating stirring 60min at 70 DEG C filters to obtain first-time filtrate and a filter residue;
(3) it is 1g:20ml with solid-liquid ratio, a filter residue is added in methanol, 60min is ultrasonically treated, is heated at 70 DEG C
Stir 60min, filter mass fraction be 15% secondary filtrate, be 20ml:1g with solid-liquid ratio, it is bright by being added in secondary filtrate
Glue stirs 30min at 50 DEG C, obtains sustained release agent
(4) first-time filtrate and sustained release agent are merged, paregal O surfactant is added, stirs evenly, purification is concentrated to get
Mass fraction is the green peel of walnut multifunction finishing agent of the high extraction of 10-25%.
Embodiment 3:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying formation length is lower than 1cm's
The fermentation enzyme solutions that the mass fraction of 9ml is 4% will be added, 45 in pretreated green peel of walnut in the pretreated green peel of 1g
Cold fermentation 1-2d obtains the tunning of green peel of walnut at DEG C.
(2) tunning of green peel of walnut is broken into mud, is 1g40ml with solid-liquid ratio, addition volume ratio is 2-4:1 second
In alcohol aqueous solvent, after being ultrasonically treated 30min, the heating stirring 40min at 65 DEG C filters to obtain first-time filtrate and a filter residue;
(3) it is 1g:15ml with solid-liquid ratio, a filter residue is added in methanol, 60min is ultrasonically treated, is heated at 70 DEG C
Stir 40min, filter mass fraction be 12% secondary filtrate, be 15ml:1g with solid-liquid ratio, it is bright by being added in secondary filtrate
Glue stirs 25min at 50 DEG C, obtains sustained release agent
(4) first-time filtrate and sustained release agent are merged, paregal O surfactant is added, stirs evenly, purification is concentrated to get
Mass fraction is the green peel of walnut multifunction finishing agent of the high extraction of 10-25%.
Embodiment 4:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying formation length is lower than 1cm's
The fermentation enzyme solutions that the mass fraction of 10ml is 3% will be added, 40 in pretreated green peel of walnut in the pretreated green peel of 1g
Cold fermentation 1.5d obtains the tunning of green peel of walnut at DEG C.
(2) tunning of green peel of walnut is broken into mud, is 1g:35ml with solid-liquid ratio, addition volume ratio is 2:1 ethyl alcohol
In aqueous solvent, after being ultrasonically treated 30min, the heating stirring 60min at 60 DEG C filters to obtain first-time filtrate and a filter residue;
(3) it is 1g:10ml with solid-liquid ratio, a filter residue is added in methanol, 60min is ultrasonically treated, is heated at 70 DEG C
Stir 40min, filter mass fraction be 10% secondary filtrate, be 10ml:1g with solid-liquid ratio, it is bright by being added in secondary filtrate
Glue stirs 20min at 50 DEG C, obtains sustained release agent
(4) first-time filtrate and sustained release agent are merged, paregal O surfactant is added, stirs evenly, purification is concentrated to get
The green peel of walnut multifunction finishing agent for the high extraction that mass fraction is 15%.
Embodiment 5:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying formation length is lower than 1cm's
The fermentation enzyme solutions that the mass fraction of 8.5ml is 3.5% will be added in pretreated green peel of walnut in the pretreated green peel of 1g,
Cold fermentation 1d obtains the tunning of green peel of walnut at 50 DEG C.
(2) tunning of green peel of walnut is broken into mud, is 1g:45ml with solid-liquid ratio, addition volume ratio is 3:1 ethyl alcohol
In aqueous solvent, after being ultrasonically treated 30min, the heating stirring 35min at 70 DEG C filters to obtain first-time filtrate and a filter residue;
(3) it is 1g:20ml with solid-liquid ratio, a filter residue is added in methanol, 60min is ultrasonically treated, is heated at 70 DEG C
Stir 50min, filter mass fraction be 15% secondary filtrate, be 20ml:1g with solid-liquid ratio, it is bright by being added in secondary filtrate
Glue stirs 30min at 50 DEG C, obtains sustained release agent
(4) first-time filtrate and sustained release agent are merged, paregal O surfactant is added, stirs evenly, purification is concentrated to get
The green peel of walnut multifunction finishing agent for the high extraction that mass fraction is 15%.
Embodiment 6:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying formation length is lower than 1cm's
The fermentation enzyme solutions that the mass fraction of 10ml is 4% will be added, 40 in pretreated green peel of walnut in the pretreated green peel of 1g
Cold fermentation 2d obtains the tunning of green peel of walnut at DEG C.
(2) tunning of green peel of walnut is broken into mud, is 1g:45ml with solid-liquid ratio, addition volume ratio is 4:1 ethyl alcohol
In aqueous solvent, after being ultrasonically treated 30min, the heating stirring 50min at 70 DEG C filters to obtain first-time filtrate and a filter residue;
(3) it is 1g:20ml with solid-liquid ratio, a filter residue is added in methanol, 60min is ultrasonically treated, is heated at 60 DEG C
Stir 45min, filter mass fraction be 15% secondary filtrate, be 20ml:1g with solid-liquid ratio, it is bright by being added in secondary filtrate
Glue stirs 25min at 50 DEG C, obtains sustained release agent
(4) first-time filtrate and sustained release agent are merged, paregal O surfactant is added, stirs evenly, purification is concentrated to get
The green peel of walnut multifunction finishing agent for the high extraction that mass fraction is 20%.
Embodiment 7:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying formation length is lower than 1cm's
The fermentation enzyme solutions that the mass fraction of 10ml is 4.5% will be added in pretreated green peel of walnut in the pretreated green peel of 1g,
Cold fermentation 2d obtains the tunning of green peel of walnut at 45 DEG C.
(2) tunning of green peel of walnut is broken into mud, is 1g:45ml with solid-liquid ratio, addition volume ratio is 4:1 ethyl alcohol
In aqueous solvent, after being ultrasonically treated 30min, the heating stirring 60min at 70 DEG C filters to obtain first-time filtrate and a filter residue;
(3) it is 1g:20ml with solid-liquid ratio, a filter residue is added in methanol, 60min is ultrasonically treated, is heated at 65 DEG C
Stir 50min, filter mass fraction be 15% secondary filtrate, be 10ml:1g with solid-liquid ratio, it is bright by being added in secondary filtrate
Glue stirs 25min at 50 DEG C, obtains sustained release agent
(4) first-time filtrate and sustained release agent are merged, paregal O surfactant is added, stirs evenly, purification is concentrated to get
The green peel of walnut multifunction finishing agent for the high extraction that mass fraction is 20%.
Embodiment 8:
(1) prematuration period fresh green peel of walnut is gone down, after cleaning, chopping, freeze-drying formation length is lower than 1cm's
The fermentation enzyme solutions that the mass fraction of 9.5ml is 4.5% will be added in pretreated green peel of walnut in the pretreated green peel of 1g,
Cold fermentation 2d obtains the tunning of green peel of walnut at 45 DEG C.
(2) tunning of green peel of walnut is broken into mud, is 1g:45ml with solid-liquid ratio, addition volume ratio is 4:1 ethyl alcohol
In aqueous solvent, after being ultrasonically treated 30min, the heating stirring 55min at 65 DEG C filters to obtain first-time filtrate and a filter residue;
(3) it is 1g:10ml with solid-liquid ratio, a filter residue is added in methanol, 60min is ultrasonically treated, is heated at 70 DEG C
Stir 55min, filter mass fraction be 15% secondary filtrate, be 10ml:1g with solid-liquid ratio, it is bright by being added in secondary filtrate
Glue stirs 20min at 50 DEG C, obtains sustained release agent
(4) first-time filtrate and sustained release agent are merged, paregal O surfactant is added, stirs evenly, purification is concentrated to get
The green peel of walnut multifunction finishing agent for the high extraction that mass fraction is 22%.
Through detecting, the recovery rate of green peel of walnut multifunction finishing agent of the high extraction of embodiment 1-8 preparation, antibiotic property,
The result of dyeability, inoxidizability and pro-skin is as follows:
As seen from the above table, the recovery rate of the green peel of walnut multifunction finishing agent of high extraction prepared by the present invention is high, has
The performance of the anti-oxidant pro-skin of antibacterial, dye-uptake might as well.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.