CN106400474A - High-extraction rate green walnut peel multifunctional finishing agent and preparation method thereof - Google Patents

High-extraction rate green walnut peel multifunctional finishing agent and preparation method thereof Download PDF

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CN106400474A
CN106400474A CN201610838909.3A CN201610838909A CN106400474A CN 106400474 A CN106400474 A CN 106400474A CN 201610838909 A CN201610838909 A CN 201610838909A CN 106400474 A CN106400474 A CN 106400474A
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finishing agent
exocarpium juglandis
juglandis immaturus
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extraction
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CN106400474B (en
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王文庆
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Gansu Jiuyuan Agriculture And Forestry Technology Co ltd
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Dongguan Lianzhou Intellectual Property Operation and Management Co Ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/11Compounds containing epoxy groups or precursors thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/12Aldehydes; Ketones
    • D06M13/123Polyaldehydes; Polyketones
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/152Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/12Processes in which the treating agent is incorporated in microcapsules
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    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/34General 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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 insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64General 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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
    • D06P1/65112Compounds containing aldehyde or ketone groups
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    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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 insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64General 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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
    • D06P1/65118Compounds containing hydroxyl groups

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  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicines Containing Plant Substances (AREA)
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Abstract

The invention provides a preparation method for a high-extraction rate green walnut peel multifunctional finishing agent. The preparation method comprises the following steps: separating fresh green walnut peel in an early stage of maturity, washing, cutting, performing freeze drying so as to obtain pretreated green walnut peel, adding an enzyme solution, and performing low-temperature fermentation so as to obtain a fermented product of the green walnut peel; crushing the fermented product of the green walnut peel into paste, performing ultrasonic treatment with an extraction solvent twice, performing heating stirring extraction, filtering so as to obtain primary filtrate and secondary filtrate, adding a micro capsule wall material into the secondary filtrate, and stirring so as to obtain a slow-release agent; and combining the primary filtrate with the slow-release agent, adding a surfactant, stirring uniformly, and performing purification concentration to obtain the high-extraction rate green walnut peel multifunctional finishing agent. The preparation method provided by the invention is simple, convenient and efficient, and the finishing agent can be used as a dyeing finishing agent, an antibacterial finishing agent, an anti-ultraviolet finishing agent and a skin-friendly finishing agent.

Description

A kind of Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction and preparation method thereof
Technical field
The invention belongs to textile material technical field is and in particular to a kind of Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction And preparation method thereof.
Background technology
Pericarpium Citri Reticulatae Viride be rutaceae orange and the plantation young fruit of mutation or immature fruit peel is dried.Juglans plants In green Pericarpium Citri Reticulatae Viride in the fruit that comprises fall within one kind of Pericarpium Citri Reticulatae Viride.Abundant saccharide, protein, amino is contained in Exocarpium Juglandis Immaturus Acid, inorganic salt and vitamin etc., also have phenols, flavanone, naphthoquinone class bioactive substance, therefore Pericarpium Citri Reticulatae Viride is normal since ancient times It is used as Chinese crude drug, have functions that depressed liver-energy dispersing and QI regulating, removing food stagnancyization be stagnant, relieving distension and oppression.Therefore Exocarpium Juglandis Immaturus is applied to woven face Also can give fabric new function in material, improve the added value of fabric.
Disclosed Exocarpium Juglandis Immaturus dye liquor prepared by Exocarpium Juglandis Immaturus of Chinese patent CN 102516804B and preparation method thereof with And the method being dyeed with its fabric, Exocarpium Juglandis Immaturus is dried into black, then after pulverizing cleaning, dechlorinated softening hot water is clear Wash the dust on surface, then be soaked in filtering and concentrating in alkali liquor and obtain Pericarpium Citri Reticulatae Viride filtrate, then adopt green vitriol and chlorination Sodium, as medium, dyes to fabric through mordant dyeing color method, prepares the fabric being applied to baby.Chinese patent CN A kind of antioxidant containing macadimia nut Pericarpium Citri Reticulatae Viride extract and preparation method and application disclosed in 104323395A, Australia is hard Fruit takes Pericarpium Citri Reticulatae Viride after spontaneously drying, and Pericarpium Citri Reticulatae Viride is pulverized and forms powder, then carried with ethanol, acetone, isobutanol or ethyl acetate Take, concentrate, volatilize completely to organic solvent and obtain macadimia nut Pericarpium Citri Reticulatae Viride extract, finally macadimia nut Pericarpium Citri Reticulatae Viride extract is dissolved In above-mentioned organic solvent, standing obtains the antioxidant containing macadimia nut Pericarpium Citri Reticulatae Viride extract.From above-mentioned prior art, mesh Mostly application in terms of weaving for the front Exocarpium Juglandis Immaturus is to go out pigment or functional component by organic solvent extraction, and Exocarpium Juglandis Immaturus is carried Thing is taken as dyestuff or functional finishing agent, fabric to be dyeed or arrange, but the extraction maneuver of walnut peel extract Simply, extraction ratio is limited, still has many resources to be wasted.Cortex walnut plant dye disclosed in Chinese patent CN 102172937B Material dye bamboo chip method, by walnut husk bank up fermentation dried obtain auburn bulk dye for fabrics raw material, fabric is contaminated Material raw material pulverizing becomes dye powder, adds penetrating agent, body lotion water and bamboo chip and is contaminated, and taking-up bamboo chip washing is dried and contaminated The bamboo chip of color.Prepare dye powder using fermentation technique bamboo chip is dyeed, take full advantage of the composition inside Pericarpium Citri Reticulatae Viride, but Hot fermentation can cause certain injury to the active component inside Pericarpium Citri Reticulatae Viride, therefore, researches and develops a kind of Exocarpium Juglandis Immaturus of high extraction Extracting method seems very necessary.
Low temperature enzyme fermentation is combined by applicant of the present invention with solvent extraction techniques, and the Semen Juglandiss preparing high extraction are blue or green Skin finishing agent, remains pigment in Exocarpium Juglandis Immaturus, antimicrobial component, antioxidant content and pro-skin composition etc. to greatest extent, makes The finishing agent of preparation has several functions.
Content of the invention
The technical problem to be solved in the present invention is Exocarpium Juglandis Immaturus multifunction finishing agent and its system providing a kind of high extraction Preparation Method, using cryodesiccated Exocarpium Juglandis Immaturus as raw material, after low temperature enzyme fermentation, through ethanol water and methanol solution after elder generation Extraction obtains first-time filtrate and secondary filtrate, and secondary filtrate adds microcapsule to form slow releasing agent, and both are combined rear addition auxiliary agent Form Exocarpium Juglandis Immaturus multifunction finishing agent.Preparation method of the present invention is simple, using the extracting method of multiple low-cost high-efficiency, makes For obtaining high extraction multi-functional Exocarpium Juglandis Immaturus finishing agent, make full use of the effective ingredient of Exocarpium Juglandis Immaturus, reduce and waste.
For solving above-mentioned technical problem, the technical scheme is that:
A kind of Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction, the Exocarpium Juglandis Immaturus multifunction finishing agent of described high extraction Include Pericarpium Citri Reticulatae Viride pigment, phenolic compound, flavanone compound, naphthoquinone compound and auxiliary agent, the core of described high extraction Microencapsulated Slow composition is also included, described auxiliary agent is surfactant in Fructus Persicae Pericarpium Citri Reticulatae Viride multifunction finishing agent.
Preferred as technique scheme, the Exocarpium Juglandis Immaturus multifunction finishing agent of described high extraction is by enzymatic solution low temperature Fermentation is prepared from reference to multiple solvent extraction techniques.
The present invention also provides a kind of preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction, walks including following Suddenly:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms the Semen Juglandiss of pretreatment Pericarpium Citri Reticulatae Viride, will add enzymatic solution, low temperature fermentation obtains the tunning of Exocarpium Juglandis Immaturus in the Pericarpium Citri Reticulatae Viride of pretreatment;
(2) tunning of the Exocarpium Juglandis Immaturus preparing step (1) is broken into mud, adds in an Extraction solvent, ultrasonic After process, heated and stirred, filters to obtain first-time filtrate and a filtering residue;
(3) filtering residue prepared by step (2) is added in second extraction solvent, after supersound process, heated and stirred, filters Obtain secondary filtrate and secondary filtering residue, microcapsule wall material, stirring will be added in secondary filtrate, and obtain slow releasing agent;
(4) slow releasing agent prepared by the first-time filtrate in step (2) and step (3) is merged, add surfactant, stirring Uniformly, purification is concentrated to give the Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction.
Preferred as technique scheme, in described step (1), the length of the Exocarpium Juglandis Immaturus of pretreatment is less than 1cm.
Preferred as technique scheme, in described step (1), the mass fraction of enzymatic solution is 3-5%, and described enzyme is Fermentation enzyme.
Preferred as technique scheme, in described step (1), the Pericarpium Citri Reticulatae Viride of pretreatment with the solid-liquid ratio of enzymatic solution is 1g:8-10ml.
Preferred as technique scheme, in described step (2), Extraction solvent is ethanol water, ethanol with The volume ratio of water is 2-4:1.
Preferred as technique scheme, in described step (3), second extraction solvent is methanol.
Preferred as technique scheme, in described step (3), described microcapsule wall material is gelatin.
Preferred as technique scheme, in described step (4), described surfactant is paregal O.
Compared with prior art, the invention has the advantages that:
(1) the Exocarpium Juglandis Immaturus multifunction finishing agent of the high extraction of present invention preparation is using the core of first freeze-dried process , as raw material, the freeze-dried process of fresh Exocarpium Juglandis Immaturus can be in the moisture in eliminating fresh Exocarpium Juglandis Immaturus for Fructus Persicae Pericarpium Citri Reticulatae Viride Meanwhile, the effective ingredient in Exocarpium Juglandis Immaturus, the fermentation after being conducive to and extraction process are remained to greatest extent.
(2) the Exocarpium Juglandis Immaturus multifunction finishing agent of the high extraction of present invention preparation first adopts ferment treatment low temperature fermentation skill Art, what ferment treatment can be the fastest is decomposed into less molecule by the cellulose macromolecule in Exocarpium Juglandis Immaturus and protein macromolecule, Accelerate the speed decomposed in conjunction with low temperature fermentation technology, and do not affect pigment in Fructus Persicae skin Pericarpium Citri Reticulatae Viride, phenolic compound, flavanone Compound, naphthoquinone compound, advantageously quickly effective in solvent extraction afterwards.
(3) the Exocarpium Juglandis Immaturus multifunction finishing agent of the high extraction of present invention preparation is using solution extractive technique twice, first With ethanol-water extraction, again with methanol is extracted, in conjunction with ultrasonic wave added and heated and stirred technology, will be fast for the effective ingredient in Exocarpium Juglandis Immaturus Speed efficiently extracts.
(4) additionally, also carrying out Microencapsulated Slow process to secondary filtrate, be conducive to finishing agent that fabric is effectively made for a long time With, qucik-acting agent is combined with slow releasing agent, prepare multifunction long-acting finishing agent.
(5) preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction of present invention preparation is simply efficient, by core Effective ingredient in Fructus Persicae Pericarpium Citri Reticulatae Viride fully extracts, and prepares the finishing agent of antibacterial, antioxidation and pro-skin, but also can be to weaving Product carry out plant dyeing, and color fastness is high.
Specific embodiment
To describe the present invention, the illustrative examples of the here present invention and explanation below in conjunction with specific embodiment in detail It is used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms length and is less than 1cm's The Exocarpium Juglandis Immaturus of pretreatment, the fermentation enzymatic solution that the mass fraction adding 8ml in the Pericarpium Citri Reticulatae Viride of the pretreatment of 1g is 3%, 40 At DEG C, low temperature fermentation 1d obtains the tunning of Exocarpium Juglandis Immaturus.
(2) tunning of Exocarpium Juglandis Immaturus is broken into mud, with solid-liquid ratio as 1g:30ml, adds volume ratio to be 2:1 ethanol In aqueous solvent, after supersound process 30min, heated and stirred 30min at 60 DEG C, filters to obtain first-time filtrate and a filtering residue;
(3) with solid-liquid ratio as 1g:10ml, a filtering residue is added in methanol, and supersound process 60min heats at 60 DEG C Stirring 30min, filter mass fraction be 10% secondary filtrate, with solid-liquid ratio as 10ml:1g, bright by adding in secondary filtrate Glue, stirs 20min at 50 DEG C, obtains slow releasing agent.
(4) first-time filtrate and slow releasing agent are merged, add paregal O surfactant, stir, purification is concentrated to give Mass fraction is the Exocarpium Juglandis Immaturus multifunction finishing agent of the high extraction of 10-25%.
Embodiment 2:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms length and is less than 1cm's The Exocarpium Juglandis Immaturus of pretreatment, the fermentation enzymatic solution that the mass fraction adding 10ml in the Pericarpium Citri Reticulatae Viride of the pretreatment of 1g is 5%, 50 At DEG C, low temperature fermentation 2d obtains the tunning of Exocarpium Juglandis Immaturus.
(2) tunning of Exocarpium Juglandis Immaturus is broken into mud, with solid-liquid ratio as 1g:50ml, adds volume ratio to be 4:1 ethanol In aqueous solvent, after supersound process 30min, heated and stirred 60min at 70 DEG C, filters to obtain first-time filtrate and a filtering residue;
(3) with solid-liquid ratio as 1g:20ml, a filtering residue is added in methanol, and supersound process 60min heats at 70 DEG C Stirring 60min, filter mass fraction be 15% secondary filtrate, with solid-liquid ratio as 20ml:1g, bright by adding in secondary filtrate Glue, stirs 30min at 50 DEG C, obtains slow releasing agent.
(4) first-time filtrate and slow releasing agent are merged, add paregal O surfactant, stir, purification is concentrated to give Mass fraction is the Exocarpium Juglandis Immaturus multifunction finishing agent of the high extraction of 10-25%.
Embodiment 3:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms length and is less than 1cm's The Exocarpium Juglandis Immaturus of pretreatment, the fermentation enzymatic solution that the mass fraction adding 9ml in the Pericarpium Citri Reticulatae Viride of the pretreatment of 1g is 4%, 45 At DEG C, low temperature fermentation 1-2d obtains the tunning of Exocarpium Juglandis Immaturus.
(2) tunning of Exocarpium Juglandis Immaturus is broken into mud, with solid-liquid ratio as 1g40ml, addition volume ratio is 2-4:1 second In alcohol aqueous solvent, after supersound process 30min, heated and stirred 40min at 65 DEG C, filters to obtain first-time filtrate and a filtering residue;
(3) with solid-liquid ratio as 1g:15ml, a filtering residue is added in methanol, and supersound process 60min heats at 70 DEG C Stirring 40min, filter mass fraction be 12% secondary filtrate, with solid-liquid ratio as 15ml:1g, bright by adding in secondary filtrate Glue, stirs 25min at 50 DEG C, obtains slow releasing agent.
(4) first-time filtrate and slow releasing agent are merged, add paregal O surfactant, stir, purification is concentrated to give Mass fraction is the Exocarpium Juglandis Immaturus multifunction finishing agent of the high extraction of 10-25%.
Embodiment 4:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms length and is less than 1cm's The Exocarpium Juglandis Immaturus of pretreatment, the fermentation enzymatic solution that the mass fraction adding 10ml in the Pericarpium Citri Reticulatae Viride of the pretreatment of 1g is 3%, 40 At DEG C, low temperature fermentation 1.5d obtains the tunning of Exocarpium Juglandis Immaturus.
(2) tunning of Exocarpium Juglandis Immaturus is broken into mud, with solid-liquid ratio as 1g:35ml, adds volume ratio to be 2:1 ethanol In aqueous solvent, after supersound process 30min, heated and stirred 60min at 60 DEG C, filters to obtain first-time filtrate and a filtering residue;
(3) with solid-liquid ratio as 1g:10ml, a filtering residue is added in methanol, and supersound process 60min heats at 70 DEG C Stirring 40min, filter mass fraction be 10% secondary filtrate, with solid-liquid ratio as 10ml:1g, bright by adding in secondary filtrate Glue, stirs 20min at 50 DEG C, obtains slow releasing agent.
(4) first-time filtrate and slow releasing agent are merged, add paregal O surfactant, stir, purification is concentrated to give Mass fraction is the Exocarpium Juglandis Immaturus multifunction finishing agent of 15% high extraction.
Embodiment 5:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms length and is less than 1cm's The Exocarpium Juglandis Immaturus of pretreatment, the fermentation enzymatic solution that the mass fraction adding 8.5ml in the Pericarpium Citri Reticulatae Viride of the pretreatment of 1g is 3.5%, At 50 DEG C, low temperature fermentation 1d obtains the tunning of Exocarpium Juglandis Immaturus.
(2) tunning of Exocarpium Juglandis Immaturus is broken into mud, with solid-liquid ratio as 1g:45ml, adds volume ratio to be 3:1 ethanol In aqueous solvent, after supersound process 30min, heated and stirred 35min at 70 DEG C, filters to obtain first-time filtrate and a filtering residue;
(3) with solid-liquid ratio as 1g:20ml, a filtering residue is added in methanol, and supersound process 60min heats at 70 DEG C Stirring 50min, filter mass fraction be 15% secondary filtrate, with solid-liquid ratio as 20ml:1g, bright by adding in secondary filtrate Glue, stirs 30min at 50 DEG C, obtains slow releasing agent.
(4) first-time filtrate and slow releasing agent are merged, add paregal O surfactant, stir, purification is concentrated to give Mass fraction is the Exocarpium Juglandis Immaturus multifunction finishing agent of 15% high extraction.
Embodiment 6:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms length and is less than 1cm's The Exocarpium Juglandis Immaturus of pretreatment, the fermentation enzymatic solution that the mass fraction adding 10ml in the Pericarpium Citri Reticulatae Viride of the pretreatment of 1g is 4%, 40 At DEG C, low temperature fermentation 2d obtains the tunning of Exocarpium Juglandis Immaturus.
(2) tunning of Exocarpium Juglandis Immaturus is broken into mud, with solid-liquid ratio as 1g:45ml, adds volume ratio to be 4:1 ethanol In aqueous solvent, after supersound process 30min, heated and stirred 50min at 70 DEG C, filters to obtain first-time filtrate and a filtering residue;
(3) with solid-liquid ratio as 1g:20ml, a filtering residue is added in methanol, and supersound process 60min heats at 60 DEG C Stirring 45min, filter mass fraction be 15% secondary filtrate, with solid-liquid ratio as 20ml:1g, bright by adding in secondary filtrate Glue, stirs 25min at 50 DEG C, obtains slow releasing agent.
(4) first-time filtrate and slow releasing agent are merged, add paregal O surfactant, stir, purification is concentrated to give Mass fraction is the Exocarpium Juglandis Immaturus multifunction finishing agent of 20% high extraction.
Embodiment 7:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms length and is less than 1cm's The Exocarpium Juglandis Immaturus of pretreatment, the fermentation enzymatic solution that the mass fraction adding 10ml in the Pericarpium Citri Reticulatae Viride of the pretreatment of 1g is 4.5%, At 45 DEG C, low temperature fermentation 2d obtains the tunning of Exocarpium Juglandis Immaturus.
(2) tunning of Exocarpium Juglandis Immaturus is broken into mud, with solid-liquid ratio as 1g:45ml, adds volume ratio to be 4:1 ethanol In aqueous solvent, after supersound process 30min, heated and stirred 60min at 70 DEG C, filters to obtain first-time filtrate and a filtering residue;
(3) with solid-liquid ratio as 1g:20ml, a filtering residue is added in methanol, and supersound process 60min heats at 65 DEG C Stirring 50min, filter mass fraction be 15% secondary filtrate, with solid-liquid ratio as 10ml:1g, bright by adding in secondary filtrate Glue, stirs 25min at 50 DEG C, obtains slow releasing agent.
(4) first-time filtrate and slow releasing agent are merged, add paregal O surfactant, stir, purification is concentrated to give Mass fraction is the Exocarpium Juglandis Immaturus multifunction finishing agent of 20% high extraction.
Embodiment 8:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms length and is less than 1cm's The Exocarpium Juglandis Immaturus of pretreatment, the fermentation enzymatic solution that the mass fraction adding 9.5ml in the Pericarpium Citri Reticulatae Viride of the pretreatment of 1g is 4.5%, At 45 DEG C, low temperature fermentation 2d obtains the tunning of Exocarpium Juglandis Immaturus.
(2) tunning of Exocarpium Juglandis Immaturus is broken into mud, with solid-liquid ratio as 1g:45ml, adds volume ratio to be 4:1 ethanol In aqueous solvent, after supersound process 30min, heated and stirred 55min at 65 DEG C, filters to obtain first-time filtrate and a filtering residue;
(3) with solid-liquid ratio as 1g:10ml, a filtering residue is added in methanol, and supersound process 60min heats at 70 DEG C Stirring 55min, filter mass fraction be 15% secondary filtrate, with solid-liquid ratio as 10ml:1g, bright by adding in secondary filtrate Glue, stirs 20min at 50 DEG C, obtains slow releasing agent.
(4) first-time filtrate and slow releasing agent are merged, add paregal O surfactant, stir, purification is concentrated to give Mass fraction is the Exocarpium Juglandis Immaturus multifunction finishing agent of 22% high extraction.
After testing, embodiment 1-8 preparation the extraction ratio of Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction, antibiotic property, The result of dyeability, non-oxidizability and pro-skin is as follows:
As seen from the above table, the extraction ratio of the Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction of present invention preparation is high, has The performance of antibacterial antioxidation pro-skin, dye-uptake might as well.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as All equivalent modifications becoming or change, must be covered by the claim of the present invention.

Claims (10)

1. a kind of high extraction Exocarpium Juglandis Immaturus multifunction finishing agent it is characterised in that:The Exocarpium Juglandis Immaturus of described high extraction is many Functional finishing agent includes Pericarpium Citri Reticulatae Viride pigment, phenolic compound, flavanone compound, naphthoquinone compound and auxiliary agent, described height Microencapsulated Slow composition is also included, described auxiliary agent is surfactant in the Exocarpium Juglandis Immaturus multifunction finishing agent of extraction ratio.
2. a kind of high extraction according to claim 1 Exocarpium Juglandis Immaturus multifunction finishing agent it is characterised in that:Described height The Exocarpium Juglandis Immaturus multifunction finishing agent of extraction ratio is prepared from reference to multiple solvent extraction techniques by enzymatic solution low temperature fermentation.
3. a kind of preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction is it is characterised in that comprise the following steps:
(1) Exocarpium Juglandis Immaturus fresh prematuration period is gone down, after cleaning, chopping, lyophilization forms the Exocarpium Juglandis Immaturus of pretreatment, Enzymatic solution will be added, low temperature fermentation obtains the tunning of Exocarpium Juglandis Immaturus in the Pericarpium Citri Reticulatae Viride of pretreatment;
(2) tunning of the Exocarpium Juglandis Immaturus preparing step (1) is broken into mud, adds in an Extraction solvent, supersound process Afterwards, heated and stirred, filters to obtain first-time filtrate and a filtering residue;
(3) filtering residue preparing step (2) adds in second extraction solvent, after supersound process, heated and stirred, filter two Secondary filtrate and secondary filtering residue, will add microcapsule wall material, stirring, obtain slow releasing agent in secondary filtrate;
(4) slow releasing agent prepared by the first-time filtrate in step (2) and step (3) is merged, add surfactant, stirring is all Even, purification is concentrated to give the Exocarpium Juglandis Immaturus multifunction finishing agent of high extraction.
4. the preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of a kind of high extraction according to claim 3, its feature It is:In described step (1), the length of the Exocarpium Juglandis Immaturus of pretreatment is less than 1cm.
5. the preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of a kind of high extraction according to claim 3, its feature It is:In described step (1), the mass fraction of enzymatic solution is 3-5%, and described enzyme is fermentation enzyme.
6. the preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of a kind of high extraction according to claim 3, its feature It is:In described step (1), the Pericarpium Citri Reticulatae Viride of pretreatment and the solid-liquid ratio of enzymatic solution are 1g:8-10ml.
7. the preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of a kind of high extraction according to claim 3, its feature It is:In described step (2), an Extraction solvent is ethanol water, and ethanol is 2-4 with the volume ratio of water:1.
8. the preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of a kind of high extraction according to claim 3, its feature It is:In described step (3), second extraction solvent is methanol.
9. the preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of a kind of high extraction according to claim 3, its feature It is:In described step (3), described microcapsule wall material is gelatin.
10. the preparation method of the Exocarpium Juglandis Immaturus multifunction finishing agent of a kind of high extraction according to claim 3, its feature It is:In described step (4), described surfactant is paregal O.
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