CN111454587A - Comprehensive processing and utilizing method for dyeing of pericarpium juglandis - Google Patents
Comprehensive processing and utilizing method for dyeing of pericarpium juglandis Download PDFInfo
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- 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
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- 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
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- 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
- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/46—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
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- 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
- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/64—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
- D06P1/651—Compounds without nitrogen
- D06P1/65106—Oxygen-containing compounds
- D06P1/65118—Compounds containing hydroxyl groups
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Abstract
The invention discloses a comprehensive processing and utilizing method of undaria pinnatifida for dyeing, which comprises the following steps: the first step is as follows: selecting the pericarpium juglandis; the second step is that: adding the pericarpium juglandis into a mixed solution of ethyl acetate solution and chitosan subjected to ultrasonic degradation for primary extraction to obtain a chitosan and juglone mixed solution and the pericarpium juglandis subjected to primary extraction, and recovering ethyl acetate, wherein the third step is as follows: the juglone is prepared by performing secondary extraction on the exocarpium juglandis extracted for the first time by adopting a double water phase high temperature method to obtain a solution containing flavone and polyphenol, and then performing reduced pressure distillation to prepare a concentrated solution; the invention greatly improves the additional performance and simultaneously reduces the harm of the waste Qinglongyi to the soil after processing by agriculture and forestry, food enterprises and beverage enterprises.
Description
Technical Field
The invention relates to the field of research, development and production of natural plant dyes, in particular to a comprehensive processing and utilizing method for dyeing of pericarpium juglandis.
Background
The walnut green husk is immature walnut green husk, and the green dragon skin is peeled off, namely the hickory peel. In 2017, the yield of Chinese walnuts reaches 189 million tons, which accounts for 47% of the global yield, and processed walnut products are divided into primary products and deep-processed products, wherein the primary products comprise walnut kernels, cakes, beverages and other products; the deep-processed product comprises: the walnut processing method comprises the steps of processing a large number of walnuts every year due to series products such as walnut oil, walnut protein, walnut powder and walnut milk, removing green husks on the surface layer of the walnuts before processing, removing the green husks of the walnuts to obtain a large amount of green husks, and generating about 1000 kg of green husks for every 200kg of dried walnuts. Because the green husks are colored, the environmental pollution is easily caused, and after the green husks of the walnuts piled in the field are soaked in rainwater, leachate flows into rivers and lakes, so that the water body is seriously polluted, the water quality is blackened, and the fishes are poisoned; in addition, the lignin content in the green tangerine peel is high, the alkalinity is strong, the degradation speed of the green tangerine peel is slow in nature, the green tangerine peel is not easy to rot, and the crops are difficult to grow when being buried or piled in the ground. The walnut green husks which are randomly stacked not only seriously pollute water and soil, but also generate unpleasant gas to pollute the environment. The green tangerine peel has high lignin content, is not easy to rot and has poor fertilizer efficiency. The pericarpium juglandis contains secondary metabolites such as flavone, polyphenol and naphthoquinone, and can be used as a dye for plant dyeing, although the components contained in the pericarpium juglandis are many, the content of each component is not high, the separation and purification of various components are very complicated, the separation cost is very high, and the purposes of various different components are different and the difference is large, so that the pericarpium juglandis can not be applied to large-scale plant dyeing.
The existing preparation method of the pigment component of the pericarpium juglandis and the preparation method of the multicolor hair dye thereof are used for hair dyeing, a conventional extraction and separation method is adopted, the preparation rate of the traditional extraction method is very low, and particularly when juglone is taken as a target product, the juglone begins to sublimate at the temperature higher than 60 ℃, and volatilizes along with the evaporation of a solvent or water, and the subsequent macroporous resin adsorption and ethanol elution are high in cost and are accompanied with the loss of the juglone, so that the preparation rate is lower.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a comprehensive processing and utilizing method for dyeing of the pericarpium juglandis.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the comprehensive processing and utilizing method of the Qinglongyi for dyeing comprises the following steps:
the first step is as follows: selecting the pericarpium juglandis;
the second step is that: adding the pericarpium juglandis into a mixed solution of an ethyl acetate solution and chitosan subjected to ultrasonic degradation for primary extraction to obtain a mixed solution of chitosan and juglone and the pericarpium juglandis subjected to primary extraction, and recovering the ethyl acetate, wherein the mixed solution of chitosan and juglone is used as an additive of a plant dye or used for plant dyeing;
the third step: and (3) carrying out secondary extraction on the exocarpium Juglandis Immaturum subjected to the primary extraction by adopting a two-aqueous-phase high-temperature method to obtain a solution containing flavone and polyphenol, and carrying out reduced pressure distillation on the solution containing flavone and polyphenol to prepare a concentrated solution, wherein the concentrated solution is used for plant dyeing.
The ultrasonic degradation of chitosan comprises the following steps:
step a 1: weighing 2 parts of chitosan with the molecular weight of more than 80 ten thousand and the deacetylation degree of more than 80 percent and 98 parts of formic acid solution according to the parts by weight;
step a 2: starting 40KHZ ultrasonic wave, running for 1 minute, then stopping running for 1 minute, and reacting for 60-90 minutes at 45 ℃ to obtain the chitosan degraded by ultrasonic wave.
Preferably, in the second step, 8 to 16 parts of pericarpium juglandis, 90 parts of ethyl acetate solution and 10 parts of chitosan subjected to ultrasonic degradation.
Preferably, the temperature of the first extraction is 25-30 ℃ and the time of the first extraction is 40-70 minutes.
Preferably, the concentration of the formic acid solution is between 0.1 and 0.5 percent by mass.
Preferably, the ethyl acetate solution has a concentration of 90% by mass.
Preferably, the steps of carrying out secondary extraction on the first extracted pericarpium juglandis by adopting a two-aqueous-phase high-temperature method are as follows:
step s 1: weighing 0.2-1 part of tween, 0.5-1 part of monoglyceride and 1-2 parts of turkey red oil in parts by weight, and mixing to obtain a double aqueous phase solution;
step s 2: weighing 8-16 parts of first-extracted pericarpium juglandis and 80-91 parts of purified water in parts by weight, and adding the materials into the aqueous two-phase solution;
step s 3: performing second extraction at 70-80 deg.C for 60-120 min.
Preferably, the concentration of Turkey red oil is 60% by mass.
Preferably, in the first step, the Qinglongyi produced in the current year is selected.
The invention has the following beneficial effects: the pigment components of the black dragon clothes are extracted step by step, the concentrated solution extracted for the second time by a double aqueous phase high-temperature method can be used for plant dyeing of cellulose such as cotton, hemp, tencel, modal, wool, silk and the like, protein fibers, yarns, fabrics and clothes, the juglone solution extracted for the first time is used for plant dyeing of chemical fibers such as modified polyester, chinlon, regenerated terylene and the like, yarns, fabrics and clothes, and the juglone solution extracted for the first time can also be used as an additive of plant dye; the green dragon's clothes are extracted into different products in different extraction modes, the additional performance is greatly improved after comprehensive utilization, and meanwhile, the harm of the waste green dragon's clothes after processing in agriculture and forestry, food enterprises and beverage enterprises to soil is reduced; the juglone has small molecular weight, has sublimation property, is not suitable for high-temperature extraction, and is easy to sublimate during high-temperature dyeing due to the sublimation property of the juglone, so that the coloring rate is low.
Detailed Description
The technical solution of the present invention is further explained below:
example 1:
the comprehensive processing and utilizing method of the Qinglongyi for dyeing comprises the following steps:
the first step is as follows: selecting the Qinglongyi produced in the current year;
the second step is that: 8-16 parts of pericarpium juglandis, 90 parts of ethyl acetate solution, 10 parts of chitosan subjected to ultrasonic degradation and 90% of ethyl acetate solution in percentage by mass, adding the pericarpium juglandis into a mixed solution of the ethyl acetate solution and the chitosan subjected to ultrasonic degradation, performing first extraction at 25-30 ℃ for 40-70 minutes to obtain a mixed solution of chitosan and juglone and the pericarpium juglandis subjected to first extraction, and recovering ethyl acetate, wherein the mixed solution of chitosan and juglone is used as an additive of a plant dye or used for dyeing plants; the mixed solution of chitosan and juglone is used for plant dyeing of chinlon and polyester textiles, 0.5-3 parts of the mixed solution of chitosan and juglone extracted during dyeing are added into 97-99.5 parts of water according to parts by weight, the dyeing temperature is 95-125 ℃, the temperature is kept for 40-60 minutes, 0.1-0.2 part of iron acetate is added when the temperature is reduced to 80 ℃, the temperature is kept for 25-50 minutes at 80 ℃, and then the liquor is drained and washed with water to dye the mixture into bright gray.
The third step: the method comprises the following steps of carrying out secondary extraction on the exocarpium Juglandis Immaturum extracted for the first time by adopting a two-aqueous-phase high-temperature method to obtain a solution containing flavone and polyphenol, carrying out reduced pressure distillation on the solution containing flavone and polyphenol to prepare a concentrated solution, wherein the concentrated solution is used for plant dyeing, the concentrated solution is used for plant dyeing of cellulose, protein fibers, yarns, fabrics and clothes such as cotton, hemp, tencel, modal, wool and silk, and different mordant can be used for dyeing gray according to a conventional dyeing method.
The ultrasonic degradation of chitosan comprises the following steps:
step a 1: weighing 2 parts of chitosan with the molecular weight of more than 80 ten thousand and the deacetylation degree of more than 80 percent and 98 parts of formic acid solution according to the parts by weight, wherein the mass percentage concentration of the formic acid solution is between 0.1 and 0.5 percent;
step a 2: starting 40KHZ ultrasonic wave, running for 1 minute, then stopping running for 1 minute, and reacting for 60-90 minutes at 45 ℃ to obtain the chitosan degraded by ultrasonic wave.
The method for extracting the exocarpium Juglandis Immaturum for the first time comprises the following steps:
step s 1: weighing 0.2-1 part of tween, 0.5-1 part of monoglyceride and 1-2 parts of turkey red oil in parts by weight, and mixing to obtain a double aqueous phase solution, wherein the mass percent concentration of the turkey red oil is 60%;
step s 2: weighing 8-16 parts of first-extracted pericarpium juglandis and 80-91 parts of purified water in parts by weight, and adding the materials into the aqueous two-phase solution;
step s 3: performing second extraction at 70-80 deg.C for 60-120 min.
The pigment components of the black dragon clothes are extracted step by step, the concentrated solution extracted for the second time by a double aqueous phase high-temperature method can be used for plant dyeing of cellulose such as cotton, hemp, tencel, modal, wool, silk and the like, protein fibers, yarns, fabrics and clothes, the juglone solution extracted for the first time is used for plant dyeing of chemical fibers such as modified polyester, chinlon, regenerated terylene and the like, yarns, fabrics and clothes, and the juglone solution extracted for the first time can also be used as an additive of plant dye; the green dragon's clothes are extracted into different products in different extraction modes, the additional performance is greatly improved after comprehensive utilization, and meanwhile, the harm of the waste green dragon's clothes after processing in agriculture and forestry, food enterprises and beverage enterprises to soil is reduced; the juglone has small molecular weight, has sublimation property, is not suitable for high-temperature extraction, and is easy to sublimate during high-temperature dyeing due to the sublimation property of the juglone, so that the coloring rate is low.
Example 2:
the comprehensive processing and utilizing method of the Qinglongyi for dyeing comprises the following steps:
the first step is as follows: selecting the Qinglongyi produced in the current year;
the second step is that: 8 parts of pericarpium juglandis, 90 parts of ethyl acetate solution, 10 parts of chitosan subjected to ultrasonic degradation and 90% of ethyl acetate solution by mass percent, adding the pericarpium juglandis into a mixed solution of the ethyl acetate solution and the chitosan subjected to ultrasonic degradation, performing primary extraction at 25 ℃ for 40 minutes to obtain a chitosan and juglone mixed solution and the exocarpium juglandis subjected to primary extraction, and recovering the ethyl acetate, wherein the chitosan and juglone mixed solution is used as an additive of a plant dye or used for plant dyeing; the mixed solution of chitosan and juglone is used for plant dyeing of chinlon and polyester textiles, 0.5 part of the mixed solution of chitosan and juglone extracted during dyeing is added into 97 parts of water according to the parts by weight, the dyeing temperature is 95 ℃, the temperature is kept for 40 minutes, 0.1 part of ferric acetate is added when the temperature is reduced to 80 ℃, the temperature is kept for 25 minutes at 80 ℃, and then the liquor is discharged and washed with water to dye the mixture into bright gray.
The third step: carrying out secondary extraction on the dracaena cochinchinensis subjected to primary extraction by adopting a two-aqueous-phase high-temperature method to obtain a solution containing flavone and polyphenol, carrying out reduced pressure distillation on the solution containing flavone and polyphenol to prepare a concentrated solution, wherein the concentrated solution is used for plant dyeing, the concentrated solution is used for plant dyeing of cellulose, protein fibers, yarns, fabrics and clothes such as cotton, hemp, tencel, modal, wool, silk and the like, different mordant can be used for dyeing gray according to a conventional dyeing method, the dyed textiles are soaped for 30 minutes at 40 ℃ by standard soap chips, and the soaping fastness is measured to be higher than 3.5 grade.
The ultrasonic degradation of chitosan comprises the following steps:
step a 1: weighing 2 parts of chitosan with the molecular weight of more than 80 ten thousand and the deacetylation degree of more than 80 percent and 98 parts of formic acid solution according to the weight parts, wherein the mass percent concentration of the formic acid solution is 0.1 percent;
step a 2: starting 40KHZ ultrasonic wave, running for 1 minute, then stopping running for 1 minute, and reacting for 60 minutes at 45 ℃ to obtain the chitosan degraded by ultrasonic wave.
The method for extracting the exocarpium Juglandis Immaturum for the first time comprises the following steps:
step s 1: weighing 0.2 part of tween, 0.5 part of monoglyceride and 1 part of Turkey red oil in parts by weight, and mixing the components to obtain a double aqueous phase solution, wherein the mass percent concentration of the Turkey red oil is 60%;
step s 2: weighing 8 parts of first-extracted pericarpium juglandis and 80 parts of purified water in parts by weight, and adding the materials into the aqueous two-phase solution;
step s 3: the second extraction was carried out at 70 ℃ for 60 minutes.
The pigment components of the black dragon clothes are extracted step by step, the concentrated solution extracted for the second time by a double aqueous phase high-temperature method can be used for plant dyeing of cellulose such as cotton, hemp, tencel, modal, wool, silk and the like, protein fibers, yarns, fabrics and clothes, the juglone solution extracted for the first time is used for plant dyeing of chemical fibers such as modified polyester, chinlon, regenerated terylene and the like, yarns, fabrics and clothes, and the juglone solution extracted for the first time can also be used as an additive of plant dye; the green dragon's clothes are extracted into different products in different extraction modes, the additional performance is greatly improved after comprehensive utilization, and meanwhile, the harm of the waste green dragon's clothes after processing in agriculture and forestry, food enterprises and beverage enterprises to soil is reduced; the juglone has small molecular weight, has sublimation property, is not suitable for high-temperature extraction, and is easy to sublimate during high-temperature dyeing due to the sublimation property of the juglone, so that the coloring rate is low.
Example 3:
the comprehensive processing and utilizing method of the Qinglongyi for dyeing comprises the following steps:
the first step is as follows: selecting the Qinglongyi produced in the current year;
the second step is that: the preparation method comprises the following steps of (1) adding the pericarpium juglandis to a mixed solution of an ethyl acetate solution and chitosan subjected to ultrasonic degradation at a temperature of 30 ℃ for carrying out first extraction for 70 minutes to obtain a chitosan and juglone mixed solution and the exocarpium juglandis subjected to first extraction, and recovering ethyl acetate, wherein the exocarpium juglandis is 16 parts by weight, the ethyl acetate solution is 90 parts by weight, the chitosan subjected to ultrasonic degradation is 10 parts by weight, and the mass percent concentration of the ethyl acetate solution is 90%, the chitosan and juglone mixed solution is used as an additive of a plant dye or used for plant dyeing; the mixed solution of chitosan and juglone is used for plant dyeing of chinlon and polyester textiles, 3 parts of the mixed solution of chitosan and juglone extracted during dyeing are added into 99.5 parts of water according to parts by weight, the dyeing temperature is 125 ℃, the temperature is kept for 60 minutes, 0.2 part of ferric acetate is added when the temperature is reduced to 80 ℃, the temperature is kept for 50 minutes at 80 ℃, and then the liquor is discharged and washed with water to dye the mixture into bright gray.
The third step: the method comprises the following steps of carrying out secondary extraction on the exocarpium Juglandis Immaturum extracted for the first time by adopting a two-aqueous-phase high-temperature method to obtain a solution containing flavone and polyphenol, carrying out reduced pressure distillation on the solution containing flavone and polyphenol to prepare a concentrated solution, wherein the concentrated solution is used for plant dyeing, the concentrated solution is used for plant dyeing of cellulose, protein fibers, yarns, fabrics and clothes such as cotton, hemp, tencel, modal, wool and silk, and different mordant can be used for dyeing gray according to a conventional dyeing method. The dyed textile is soaped for 30 minutes at 40 ℃ by standard soap chips, and the soaping fastness is measured to be more than 3.5 grade.
The ultrasonic degradation of chitosan comprises the following steps:
step a 1: weighing 2 parts of chitosan with the molecular weight of more than 80 ten thousand and the deacetylation degree of more than 80 percent and 98 parts of formic acid solution according to the weight parts, wherein the mass percent concentration of the formic acid solution is 0.5 percent;
step a 2: starting 40KHZ ultrasonic wave, running for 1 minute, then stopping running for 1 minute, and reacting for 90 minutes at 45 ℃ to obtain the chitosan degraded by ultrasonic wave.
The method for extracting the exocarpium Juglandis Immaturum for the first time comprises the following steps:
step s 1: weighing 1 part of tween, 1 part of monoglyceride and 2 parts of Turkey red oil according to the parts by weight, and mixing the components to obtain a double aqueous phase solution, wherein the mass percent concentration of the Turkey red oil is 60%;
step s 2: weighing 16 parts by weight of first-extracted pericarpium juglandis and 91 parts by weight of purified water, and adding the materials into the aqueous two-phase solution;
step s 3: the second extraction was carried out at 80 ℃ for 120 minutes.
The pigment components of the black dragon clothes are extracted step by step, the concentrated solution extracted for the second time by a double aqueous phase high-temperature method can be used for plant dyeing of cellulose such as cotton, hemp, tencel, modal, wool, silk and the like, protein fibers, yarns, fabrics and clothes, the juglone solution extracted for the first time is used for plant dyeing of chemical fibers such as modified polyester, chinlon, regenerated terylene and the like, yarns, fabrics and clothes, and the juglone solution extracted for the first time can also be used as an additive of plant dye; the green dragon's clothes are extracted into different products in different extraction modes, the additional performance is greatly improved after comprehensive utilization, and meanwhile, the harm of the waste green dragon's clothes after processing in agriculture and forestry, food enterprises and beverage enterprises to soil is reduced; the juglone has small molecular weight, has sublimation property, is not suitable for high-temperature extraction, and is easy to sublimate during high-temperature dyeing due to the sublimation property of the juglone, so that the coloring rate is low.
Example 4:
the comprehensive processing and utilizing method of the Qinglongyi for dyeing comprises the following steps:
the first step is as follows: selecting the Qinglongyi produced in the current year;
the second step is that: the preparation method comprises the following steps of (1) taking 10 parts of pericarpium juglandis, 90 parts of ethyl acetate solution, 10 parts of chitosan subjected to ultrasonic degradation and 90% of ethyl acetate solution in percentage by mass, adding the pericarpium juglandis into a mixed solution of the ethyl acetate solution and the chitosan subjected to ultrasonic degradation, carrying out first extraction at 28 ℃ for 60 minutes to obtain a mixed solution of chitosan and juglone and the pericarpium juglandis subjected to first extraction, and recovering ethyl acetate, wherein the mixed solution of chitosan and juglone is used as an additive of a plant dye or used for plant dyeing; the mixed solution of chitosan and juglone is used for plant dyeing of chinlon and polyester textiles, 2 parts of the mixed solution of chitosan and juglone extracted during dyeing are added into 98 parts of water according to parts by weight, the dyeing temperature is 100 ℃, the temperature is kept for 50 minutes, 0.15 part of ferric acetate is added when the temperature is reduced to 80 ℃, the temperature is kept for 28 minutes at 80 ℃, then the liquor is discharged and washed, and the dyed grey is bright.
The third step: the method comprises the following steps of carrying out secondary extraction on the exocarpium Juglandis Immaturum extracted for the first time by adopting a two-aqueous-phase high-temperature method to obtain a solution containing flavone and polyphenol, carrying out reduced pressure distillation on the solution containing flavone and polyphenol to prepare a concentrated solution, wherein the concentrated solution is used for plant dyeing, the concentrated solution is used for plant dyeing of cellulose, protein fibers, yarns, fabrics and clothes such as cotton, hemp, tencel, modal, wool and silk, and different mordant can be used for dyeing gray according to a conventional dyeing method.
The ultrasonic degradation of chitosan comprises the following steps:
step a 1: weighing 2 parts of chitosan with the molecular weight of more than 80 ten thousand and the deacetylation degree of more than 80 percent and 98 parts of formic acid solution according to the parts by weight, wherein the mass percentage concentration of the formic acid solution is 0.3 percent;
step a 2: starting 40KHZ ultrasonic wave, running for 1 minute, then stopping running for 1 minute, and reacting for 80 minutes at 45 ℃ to obtain the chitosan degraded by ultrasonic wave.
The method for extracting the exocarpium Juglandis Immaturum for the first time comprises the following steps:
step s 1: weighing 0.8 part of tween, 0.7 part of monoglyceride and 1.5 parts of Turkey red oil in parts by weight, and mixing the components to obtain a double aqueous phase solution, wherein the mass percent concentration of the Turkey red oil is 60%;
step s 2: weighing 10 parts by weight of first-extracted pericarpium juglandis and 88 parts by weight of purified water, and adding the materials into the aqueous two-phase solution;
step s 3: the second extraction was carried out at 78 ℃ for 100 minutes.
The pigment components of the black dragon clothes are extracted step by step, the concentrated solution extracted for the second time by a double aqueous phase high-temperature method can be used for plant dyeing of cellulose such as cotton, hemp, tencel, modal, wool, silk and the like, protein fibers, yarns, fabrics and clothes, the juglone solution extracted for the first time is used for plant dyeing of chemical fibers such as modified polyester, chinlon, regenerated terylene and the like, yarns, fabrics and clothes, and the juglone solution extracted for the first time can also be used as an additive of plant dye; the green dragon's clothes are extracted into different products in different extraction modes, the additional performance is greatly improved after comprehensive utilization, and meanwhile, the harm of the waste green dragon's clothes after processing in agriculture and forestry, food enterprises and beverage enterprises to soil is reduced; the juglone has small molecular weight, has sublimation property, is not suitable for high-temperature extraction, and is easy to sublimate during high-temperature dyeing due to the sublimation property of the juglone, so that the coloring rate is low.
It should be noted that the above list is only one specific embodiment of the present invention. It is clear that the invention is not limited to the embodiments described above, but that many variations are possible, all of which can be derived or suggested directly from the disclosure of the invention by a person skilled in the art, and are considered to be within the scope of the invention.
Claims (9)
1. The comprehensive processing and utilizing method of the pericarpium juglandis for dyeing is characterized by comprising the following steps:
the first step is as follows: selecting the pericarpium juglandis;
the second step is that: adding the pericarpium juglandis into a mixed solution of an ethyl acetate solution and chitosan subjected to ultrasonic degradation for primary extraction to obtain a mixed solution of chitosan and juglone and the pericarpium juglandis subjected to primary extraction, and recovering the ethyl acetate, wherein the mixed solution of chitosan and juglone is used as an additive of a plant dye or used for plant dyeing;
the third step: and (3) carrying out secondary extraction on the exocarpium Juglandis Immaturum subjected to the primary extraction by adopting a two-aqueous-phase high-temperature method to obtain a solution containing flavone and polyphenol, and carrying out reduced pressure distillation on the solution containing flavone and polyphenol to prepare a concentrated solution, wherein the concentrated solution is used for plant dyeing.
2. The comprehensive processing and utilization method for dyeing of the pericarpium juglandis as claimed in claim 1, wherein the ultrasonic degradation of chitosan comprises the following steps:
step a 1: weighing 2 parts of chitosan with the molecular weight of more than 80 ten thousand and the deacetylation degree of more than 80 percent and 98 parts of formic acid solution according to the parts by weight;
step a 2: starting 40KHZ ultrasonic wave, running for 1 minute, then stopping running for 1 minute, and reacting for 60-90 minutes at 45 ℃ to obtain the chitosan degraded by ultrasonic wave.
3. The comprehensive processing and utilization method of pericarpium juglandis for dyeing according to claim 1, wherein in the second step, the weight parts of pericarpium juglandis are 8-16, the weight parts of ethyl acetate solution is 90, and the weight parts of chitosan degraded by ultrasonic wave is 10.
4. The comprehensive processing and utilizing method for dyeing of pericarpium juglandis as claimed in claim 1, wherein the temperature of the first extraction is 25-30 ℃, and the time of the first extraction is 40-70 minutes.
5. The comprehensive processing and utilization method for dyeing of the pericarpium juglandis according to claim 2, wherein the mass percent concentration of the formic acid solution is between 0.1 and 0.5%.
6. The comprehensive processing and utilization method for dyeing of the pericarpium juglandis according to claim 1, wherein the concentration of the ethyl acetate solution is 90% by mass.
7. The comprehensive processing and utilization method for dyeing of pericarpium juglandis according to claim 1, wherein the step of performing the second extraction of the primarily extracted pericarpium juglandis by using a two-aqueous-phase high-temperature method comprises the following steps:
step s 1: weighing 0.2-1 part of tween, 0.5-1 part of monoglyceride and 1-2 parts of turkey red oil in parts by weight, and mixing to obtain a double aqueous phase solution;
step s 2: weighing 8-16 parts of first-extracted pericarpium juglandis and 80-91 parts of purified water in parts by weight, and adding the materials into the aqueous two-phase solution;
step s 3: performing second extraction at 70-80 deg.C for 60-120 min.
8. The comprehensive processing and utilization method for dyeing according to claim 1, characterized in that the concentration of turkish red oil is 60% by mass.
9. The method for comprehensively utilizing the exocarpium Juglandis Immaturum for dyeing according to claim 1, wherein in the first step, the exocarpium Juglandis Immaturum produced in the current year is selected.
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