CN105133380A - Method for extracting pigment from walnut green hulls through subcritical water and using pigment for dyeing - Google Patents
Method for extracting pigment from walnut green hulls through subcritical water and using pigment for dyeing Download PDFInfo
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Abstract
The invention relates to a method for extracting natural pigment from walnut green hulls and using the natural pigment for dyeing and belongs to the field of natural product extraction and application. According to the method, subcritical water serves as an extraction solvent, polyphenol, flavone, anthraquinone, naphthoquinone and other natural pigment in the walnut green hulls are extracted, and a natural pigment extraction solution is directly used for dyeing cotton and wool fabric. The method has the advantages that the active ingredient extraction rate is high, no organic solvent is used in the extracting and dyeing process, the process is environmentally friendly, and products are free of pollution, safe, free of toxicity and the like. No toxic and harmful pigment ingredient is contained in dyed fabric obtained through the method, and the method is suitable for dyeing the various cotton and wool fabric and particularly suitable for dyeing infant articles for use, underwear and other articles due to the fact that the natural pigment of the walnut green hulls further has anti-bacterium activity, anti-oxidation activity and the like.
Description
Technical field
The present invention relates to and a kind ofly adopt subcritical water to extract natural colouring matter from green peel of walnut and for method that is cotton, dyeability ofwool fabric, belong to natural plant active component extraction and application field.More specifically, the present invention relates to a kind of is raw material with green peel of walnut, water is Extraction solvent, the method of the active skull cap components such as the polyphenol in green peel of walnut, flavones, anthraquinone and naphthoquinones as natural colouring matter is extracted under undercritical conditions, and by the method for the above-mentioned green peel of walnut nature strength liquid extracted for cotton yarn or COTTON FABRIC and wool, the rabbit hair or its dyeability ofwool fabric.The method technical process is green, not with an organic solvent, the recovery rate of walnut green husk pigment is high, dyeing course is safe, pollution-free, nontoxic, DYED FABRICS can be used for various uses, is particularly suitable for the dyeing of the article such as infant article and underwear.
Background technology
Walnut (
juglansregial.) English walnut, Qiang peach is had another name called, the title having " long live ", " Longevity ", " intelligent promoting fruit ", " Beauty Fruits " among the people, for Juglandaceae walnut, be the precious fruit tree that a kind of nutritive value and economic worth are all very high, with almond, cashew nut, fibert claim the world four large nut.The with a long history of walnut is cultivated by China, and walnut recorded by history records is that Zhang Qian takes back seed plantation by the Western Regions, and then wide-scale distribution is to northern each province.The Xi Rong court of a feudal ruler etc. are according to report both domestic and external in recent years, and in conjunction with the research of archaeology, cytology and zymetology, the original place of production proposing walnut comprises China, think more than 7000 years it, walnut China oneself through there being growth distribution.Walnut nutritious abundant, there is the effect such as kidney-nourishing, stomach invigorating and moistening lung and benefit brain.Compendium of Material Medica is recorded, " walnut kernel, the sweet property of taste is put down, can not only moistening dryness and resolving phlegm, can also invigorating qi and benefiting blood and warm lung ease constipation ".Not only the sweet property of walnut kernel taste is put down, and can be used as medicine, the inner septum etc. of green peel of walnut, Walnut Leaves, root, fruit all has application in China's traditional medicine.
Xinjiang is one of major production areas of China's walnut, Xinjiang in Recent Years walnut cultivated area is in continuous expansion, to the selection and popularization of improved seeds in continuous reinforcement, to the transformation of low production forest also in quickening process, walnut output is riseing year by year, estimates that full boundary walnut output in 2015 will reach more than 400,000 tons.With the collecting season at walnut, producing region there will be a large amount of discarded objects---and green peel of walnut, these discarded objects are seen everywhere, not only welding, the also great waste of precocity.Research shows, containing multiple bioactive ingredients in green peel of walnut, as polyphenol, flavones, anthraquinone, naphthoquinones, alkaloid, polysaccharide etc., uses ancient using green peel of walnut as hair dye.Walnut is comparatively extensive in China's distribution, and there is plantation various places more.At present, existing many researchers are devoted to new purposes and the extracting method of finding green peel of walnut.
As far back as 2007, Chinese patent CN200710017664.9 and CN200710018235.3 just discloses respectively and a kind ofly from green peel of walnut, extracts the method for nucin and the maraniol of essential oil active anticancer and preparation method thereof, mainly utilize organic solvent step by step arithmetic, be separated and active component nucin in refining green peel of walnut and there is the alkyl diaryl compounds of active anticancer, within 2014, CN2014065631.3 reports again diaryl heptane compound separation and preparation method's method in a kind of green peel of walnut, CN201410650315 reports the method for isolating alkaloids from green peel of walnut, CN201410333014 reports a kind of extracting method of green peel of walnut polyphenol, the preparation method of a CN20131024619.5 walnut tanning.These methods are all the methods of the active component adopted in methyl alcohol, ethanol, ethyl acetate, acetone and other organic solvent extraction and isolation green peel of walnut.In recent years, particularly after 2012, about the dejacketer utility model patent quantity of green peel of walnut significantly increases, and about utilizing green peel of walnut also significantly to increase as the patent application of natural hair dye, textile dyeing agent.As the preparation of Chinese patent CN20141066739.5 pericarpium juglandis pigment composition and the preparation method of polychrome system hair dye thereof, CN201410666574 pseudo-ginseng green peel of walnut crow lotion and preparation method thereof, CN201310671464 mono-kind utilizes colouring method green peel of walnut natural dye contaminating cellulose fibre, the application process of CN201210073909 green peel of walnut extract in black is woolen dyed, green peel of walnut dye liquor that CN201110414172 is prepared by green peel of walnut and preparation method thereof and method fabric dyeed with it, the method that CN201010138664 mono-kind utilizes green peel of walnut to prepare growing and blacking hair agent, the patent applications such as CN201310195394 walnut peel extract and preparation method thereof and the purposes as antioxidant all disclose the method adopting different Extraction and separation technology to extract active component wherein and uses thereof from green peel of walnut, said method all has different features separately, but after the leaching process of walnut green husk pigment is all needed first to carry out employing organic solvent extraction, also need to concentrate extract, and then dyeing after carrying out certain preparation, could be used for.
In order to make full use of resource, overcoming in prior art leaching process needs with an organic solvent, extraction step is loaded down with trivial details, the invention provides a kind of is Extraction solvent with subcritical water, the method of the green peel of walnut natural colouring matters such as polyphenol, flavones, anthraquinone and naphthoquinones is extracted, the method environmental protection, to human and environment safety non-toxic from discarded green peel of walnut.Meanwhile, the green peel of walnut extract obtained can be directly used in cotton yarn or its fabric, and wool, the rabbit hair or its fabric dye.In order to increase COLOR FASTNESS and rich colors, after can also adopting adopting the fabric of green peel of walnut extract dyeing, the method for mordant dyeing dyes further process under mordant exists, also can carry out co-bathing dyeing by directly adding a certain proportion of mordant in the extract of green peel of walnut, significantly decreasing the consumption of dyeing water.
Summary of the invention
Raising along with quality of life and the pursuit to health, the physiologically active of natural colouring matter and security are more and more by people are familiar with, and except edible cosmetic product field, textile printing and dyeing field is also increasing year by year to the demand of natural colouring matter.In addition, the problem of environmental pollution that traditional industry causes also has caused each side and has paid close attention to, and the environmental problem that the traditional handicraft of textile printing and dyeing industry is brought also can not be despised.Based on Problems existing in current industry, the object of this invention is to provide the natural colouring matters such as a kind of polyphenol, flavones, anthraquinone and the naphthoquinones that utilize green peel of walnut discarded in walnut plant development wherein to have functional activity for raw material extracts, this extraction raw material is widely distributed in the Xinjiang walnut harvest season, abundance, can not directly use as feed, discarded object bulk deposition also pollutes the environment, and cost of material is extremely low.Meanwhile, be water be Extraction solvent due to what adopt in leaching process, wide material sources, safety non-toxic, meets the developing direction of green chemical industry.The extract of gained can be directly used in textile dyeing, and also can dye in conjunction with mordant according to the requirement of technique and product, selected mordant is that security is high, nontoxic to human and environment, safe metal cations Fe
2+, Fe
3+, Cu
2+, Zn
2+, Ti
2+, Mg
2+, Sn
2+deng sulfate or hydrochloride, whole process does not use any organic solvent, there is technical process be easy to control, without the need to advantages such as fire prevention, technological processing for explosion protection features, dyed safety to fabrics is good, and have certain bacteria resistance function, can be used in various uses, be specially adapted to the dyeing needs of the article such as infant and underwear.
To achieve these goals, the present invention adopts following technical scheme to be achieved:
The natural colouring matter such as polyphenol, flavones and anthraquinone in Subcritical water chromotagraphy green peel of walnut also for a method that is cotton, dyeability ofwool fabric, is characterized in that comprising the following steps:
(1) by after green peel of walnut cleaning, drying, pulverize, inserted in a hydrothermal reaction kettle, water is added with the ratio of solid-liquid ratio 1:1 ~ 1:50, control Extracting temperature 110 DEG C ~ 250 DEG C, extract 5min ~ 100min under remaining on the subcritical state of water, after the extraction time reaching setting, stop heating, and room temperature is quickly cooled to reactor;
(2) opened by the reactor of cool to room temperature in above-mentioned steps (1), filter to isolate Aqueous extracts wherein, a small amount of water washing of filter residue, merges above-mentioned Aqueous extracts and cleaning solution, obtains the nature strength liquid of green peel of walnut;
(3) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2) is controlling dyeing temperature at 20 DEG C ~ 100 DEG C, the dyeing of cotton yarn or COTTON FABRIC is directly used under the condition of dyeing time 30min ~ 150min, after dyeing terminates, through washing with after soaping, drying, obtains dyed cotton yarn or the COTTON FABRIC of pure natural;
(4) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2) is at control dyeing temperature 30 DEG C ~ 90 DEG C, under the condition of dyeing time 30min ~ 240min, be directly used in the dyeing of wool or rabbit hair fabric, after dyeing terminates, through washing with after soaping, drying, obtains the wool of pure natural dyeing, the rabbit hair or its wool fabric;
(5) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2) is controlling dyeing temperature at 20 DEG C ~ 100 DEG C, the dyeing of cotton yarn or COTTON FABRIC is directly used under the condition of dyeing time 30min ~ 150min, after dyeing terminates, wash the dye liquor of remained on surface with water, add the mordant prepared by certain solid-liquid ratio, and control certain temperature and dyeing time dyes, after dyeing terminates, through washing with after soaping, dry, obtain corresponding dyed cotton yarn or COTTON FABRIC;
(6) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2) is controlling dyeing temperature at 30 DEG C ~ 90 DEG C, the dyeing of wool, the rabbit hair or its wool fabric is directly used under the condition of dyeing time 30min ~ 240min, after dyeing terminates, wash the dye liquor of remained on surface with water, the mordant prepared is added by certain solid-liquid ratio, and control certain temperature and dyeing time dyes, after dyeing terminates, through washing with after soaping, drying, obtains corresponding dyeing wool, the rabbit hair or its wool fabric;
(7) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2), the mordant configured is added according to certain ratio, obtain the walnut green husk pigment extract containing mordant, at control dyeing temperature at 20 DEG C ~ 100 DEG C, cotton yarn is directly used in or COTTON FABRIC, wool, the rabbit hair or its wool fabric dye under the condition of dyeing time 30min ~ 240min, after dyeing terminates, through washing with after soaping, drying, obtains corresponding dyed cotton yarn or COTTON FABRIC and dyeing wool, the rabbit hair or its wool fabric.
Described is deionized water, pure water or distilled water for the aqueous solvent extracted and dye.
Main active in the green peel of walnut extract that described Subcritical water chromotagraphy obtains is the natural colouring matters such as polyphenol, flavones and anthraquinone in green peel of walnut, preferred processing condition is solid-liquid ratio is 1:15 ~ 1:30, Extracting temperature 180 DEG C ~ 200 DEG C, extraction time is 50min ~ 60min, and preferred green peel of walnut grinding particle size is 80 orders; Under preferred process conditions, in green peel of walnut extract, total extract yield of polyphenol, flavones and anthraquinone isoreactivity composition is greater than 12%.
When described direct employing green peel of walnut nature strength liquid is to cotton yarn or COTTON FABRIC direct dyeing, preferred dyeing condition be dyeing temperature at 70 DEG C ~ 90 DEG C, dyeing time 100min ~ 150min's.
When described direct employing green peel of walnut nature strength liquid is to cotton yarn or cotton fabric dyeing process, preferred dyeing condition is the pH value of adjustment solution is under the condition of 4.5, and dyeing temperature is 80 DEG C, and dyeing time is 120min.
Described direct employing green peel of walnut nature strength liquid to wool, the rabbit hair or its woolen direct dyeing time, preferred dyeing condition be dyeing temperature at 50 DEG C ~ 70 DEG C, dyeing time 120min ~ 180min.
Described direct employing green peel of walnut nature strength liquid to wool, the rabbit hair or its woolen direct dyeing time, preferred dyeing condition is the pH value of extract when being adjusted to 4.0, and dyeing temperature controls at 60 DEG C, dyeing time 150min.
The mordant of described cotton, wool fabric is and the metal cations Fe that have fewer environmental impacts higher to human safety
2+, Fe
3+, Cu
2+, Zn
2+, Ti
2+, Mg
2+, Sn
2+deng sulfate or hydrochloride, the addition of mordant is 1 ~ 5% of fabric quality, and the dyeing temperature of rear mordant dyeing look is 80 DEG C, and dyeing time is 60min.
The process conditions of described same bath mordant dyeing are treat that the mordant of dyeing and weaving thing 0.5% ~ 5% joins in the extract of the green peel of walnut extracted in advance by being equivalent to, obtain the walnut green husk pigment extract containing mordant, at control dyeing temperature 60 DEG C ~ 90 DEG C, cotton yarn is directly used in or COTTON FABRIC, wool, the rabbit hair or its wool fabric dye under the condition of dyeing time 90min ~ 150min, after dyeing terminates, through washing with after soaping, drying, obtains corresponding dyed cotton yarn or COTTON FABRIC and dyeing wool, the rabbit hair or its wool fabric.
The process conditions of described same bath mordant dyeing are treat that the mordant of dyeing and weaving thing 0.5% ~ 5% joins in the extract of the green peel of walnut extracted in advance by being equivalent to, obtain the walnut green husk pigment extract containing mordant, at control dyeing temperature 60 DEG C ~ 80 DEG C, cotton yarn is directly used in or COTTON FABRIC, wool, the rabbit hair or its wool fabric dye under the condition of dyeing time 120min, after dyeing terminates, through washing with after soaping, drying, obtains corresponding dyed cotton yarn or COTTON FABRIC and dyeing wool, the rabbit hair or its wool fabric.
The DYED FABRICS that described employing said method obtains is the product of environmental protection, whole technical process is not with an organic solvent, the inorganic ions that the mordant used is safety, and the various active pigment composition in green peel of walnut has anti-oxidant and bacteriostasis, the dyeing of the cotton be fit for various uses, wool fabric, is more suitable for the dyeing for the article such as infant article, underwear.
Beneficial effect acquired by the present invention is:
Extraction raw material selected by the present invention is the discarded object green peel of walnut in walnut process, and these materials, usually used as garbage disposal, namely waste the expense that resource turn increases environmental treatment.And in green peel of walnut, be rich in various active skull cap components, not only can use as natural colouring matter, also there is the effects such as anti-oxidant and antibacterial, from the green peel of walnut that these are discarded, extract green peel of walnut natural colouring matter not only can improve utilization of resources value, all right decreasing pollution, promote the whole economic efficiency of Xinjiang walnut plantation and secondary industry, in the development on band one tunnel, play positive effect.
Extraction of the present invention and dyeing simple; extraction efficiency is high; the advantage that energy consumption is low; the raw material Nantural non-toxic used; pollution-free; leaching process does not use any organic solvent; technical process safety; the solvent adopted is water, and the auxiliary material mordant of use is a small amount of metal inorganic salt, and these stock and adjuncts all have safety non-toxic, the nonflammable feature such as explosive to human and environment; whole technical process environmental protection; meet the theory of current back to nature, also meet the requirement of green chemical industry new technology, be easy to accomplish scale production.
The present invention can by the control by technical process such as green peel of walnut natural colouring matter direct dyeing or the dyeing of interpolation mordant, obtain the dyeing product to color needs different from colourity, dyeing production process is convenient to regulable control, can meet the coloration requirements of the cotton of various uses, wool fabric.
Detailed description of the invention
Adopt the mode of specific embodiment to explain the present invention particularly below, but the present invention is not limited to embodiment.
Embodiment 1
Green peel of walnut raw material is pulverized, and crosses 80 mesh sieves, accurately takes 0.5000g and put into 25mL hydrothermal reaction kettle, add 15mL distilled water, airtight, is placed in the baking oven being warming up to 150 DEG C in advance and extracts 50min.After extraction terminates, reactor is taken out from baking oven, is placed in cold water and makes it rapidly cooling to room temperature, suction filtration, and with a small amount of distilled water washing residue, extract is settled to 25mL, measures content wherein.By analysis, total recovery rate of green peel of walnut total polyphenols, flavones, anthraquinone and naphthoquinones is 13.8%.
Embodiment 2
Green peel of walnut raw material is pulverized, and crosses 80 mesh sieves, accurately takes 3.0000g and put into 100mL hydrothermal reaction kettle, add 50mL distilled water, airtight, is placed in the baking oven being warming up to 180 DEG C in advance and extracts 60min.After extraction terminates, reactor is taken out from baking oven, is placed in cold water and makes it rapidly cooling to room temperature, suction filtration, and with a small amount of distilled water washing residue, extract is settled to 100mL, measures content wherein.By analysis, in green peel of walnut, total recovery rate of polyphenol, flavones, anthraquinone and naphthoquinones is 16.5%.
Embodiment 3
Green peel of walnut raw material is pulverized, and accurately takes 100.00g and puts into 5000mL autoclave, add the deionized water that 2500mL boils, and stirs, to guarantee that sample complete wetting is in water, airtight, and system be rapidly heated starts timing after 200 DEG C, extraction 60min.After extraction terminates, heat-exchange system passes into rapidly cooling water and carries out fast cooling, is taken out by extract from reactor, and filter, a small amount of deionized water of filter residue washs, and measures content wherein.By analysis, in green peel of walnut, total recovery rate of polyphenol, flavones, anthraquinone and naphthoquinones is 16.1%.
Embodiment 4
The walnut green husk pigment extract obtained in above-described embodiment 1 is got 20mL, directly puts into and wait to contaminate white cotton 2g, room temperature balneation, warming-in-water to 70 DEG C, insulation 90min.Take out, after clear water rinses fabric, add neutral detergent washing 15min, then clear water is cleaned and is dried.
Embodiment 5
Get the walnut green husk pigment extract obtained in above-described embodiment 2 and get 50mL, directly put into and wait to contaminate white wool 1g, room temperature balneation, warming-in-water to 60 DEG C, insulation 150min.Take out, after clear water rinses fabric, add neutral detergent washing 25min, then clear water is cleaned and is dried.
Embodiment 6
Get the walnut green husk pigment extract obtained in above-described embodiment 3 and get 50mL, directly put into and wait to contaminate white wool 1g, room temperature balneation, warming-in-water to 70 DEG C, insulation 150min.Take out, after clear water rinses, adding concentration is 0.05g/mLFe
3+solution 50mL, 80 DEG C of dyeing 60min, and then add the sodium chloride being equivalent to wait to contaminate cotton quality 3%, continue insulation 60min, take out, clear water rinses, and add neutral detergent washing 20min, then clear water is cleaned and dried.
Embodiment 7
Get the walnut green husk pigment extract obtained in above-described embodiment 3 and get 100mL, the watery hydrochloric acid with 1% adjusts the pH value of solution to be 4.5, puts into and waits to contaminate white cotton 5g, room temperature balneation, warming-in-water to 80 DEG C, insulation 120min.Take out, after clear water rinses fabric, adding concentration is 0.10g/mLTi
2+solution 50mL, 80 DEG C of dyeing 60min, take out, clear water rinses, and add pre-configured neutral detergent washing 20min, then clear water is cleaned and dried.
Embodiment 8
Get the walnut green husk pigment extract obtained in above-described embodiment 3 and get 100mL, the watery hydrochloric acid with 1% adjusts the pH value of solution to be 5.0, puts into and waits to contaminate white rabbit hair fabric 3g, room temperature balneation, warming-in-water to 65 DEG C, insulation 120min.Take out, after clear water rinses fabric, adding concentration is 0.10g/mLFe
2+solution 50mL, 80 DEG C of dyeing 60min, take out, clear water rinses, and add pre-configured neutral detergent washing 20min, then clear water is cleaned and dried.
Embodiment 9
Get the walnut green husk pigment extract obtained in above-described embodiment 3 and get 250mL, the watery hydrochloric acid with 1% adjusts the pH value of solution to be 4.5, adds the pre-configured magnesium sulfate being equivalent to fabric quality 5%, obtains the Mg contained
2+the walnut green husk pigment extract of mordant, puts into and waits to contaminate white cotton 10g, room temperature balneation, warming-in-water to 80 DEG C, insulation 120min.And then add the sodium chloride being equivalent to wait to contaminate cotton quality 3%, continue insulation 60min, take out, clear water rinses, and washs 20min at adding pre-configured neutral detergent 40 DEG C, and then clear water is cleaned and dried.
Embodiment 10
Get the walnut green husk pigment extract obtained in above-described embodiment 3 and get 250mL, the watery hydrochloric acid with 1% adjusts the pH value of solution to be 4.0, adds the pre-configured copper sulphate being equivalent to fabric quality 5%, obtains the Cu contained
2+the walnut green husk pigment extract of mordant, puts into and waits to contaminate white wool fabric 5g, room temperature balneation, warming-in-water to 65 DEG C, insulation 150min.And then add the sodium chloride being equivalent to treat dyeing wool quality 3%, continue insulation 60min, take out, clear water rinses, and washs 20min at adding pre-configured neutral detergent 40 DEG C, and then clear water is cleaned and dried.
Embodiment 11
Get the walnut green husk pigment extract obtained in above-described embodiment 3 and get 200mL, add 0.5g zinc sulfate, obtain the Zn contained
2+the walnut green husk pigment extract of mordant, puts into and treats dye 10g white cotton, room temperature balneation, warming-in-water to 80 DEG C, insulation 120min.Then add the sodium chloride of 0.3g, stir and make it dissolve, continue insulation 60min, then add the tertiary sodium phosphate of 0.5, stirring makes it dissolve, and continues insulation 40min, takes out, clear water rinses, and washs 20min at adding pre-configured neutral detergent 40 DEG C, and then clear water is cleaned and dried.
Claims (10)
1. from green peel of walnut, extract the natural colouring matters such as polyphenol, flavones and anthraquinone and for a method that is cotton, dyeability ofwool fabric, it is characterized in that comprising the following steps:
(1) by after green peel of walnut cleaning, drying, pulverize, inserted in a hydrothermal reaction kettle, water is added with the ratio of solid-liquid ratio 1:1 ~ 1:50, control Extracting temperature 110 DEG C ~ 250 DEG C, extract 5min ~ 100min under remaining on the subcritical state of water, after the extraction time reaching setting, stop heating, and room temperature is quickly cooled to reactor;
(2) opened by the reactor of cool to room temperature in above-mentioned steps (1), filter to isolate Aqueous extracts wherein, a small amount of water washing of filter residue, merges above-mentioned Aqueous extracts and cleaning solution, obtains the nature strength liquid of green peel of walnut;
(3) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2) is controlling dyeing temperature at 20 DEG C ~ 100 DEG C, the dyeing of cotton yarn or COTTON FABRIC is directly used under the condition of dyeing time 30min ~ 150min, after dyeing terminates, through washing with after soaping, drying, obtains dyed cotton yarn or the COTTON FABRIC of pure natural;
(4) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2) is at control dyeing temperature 30 DEG C ~ 90 DEG C, under the condition of dyeing time 30min ~ 240min, be directly used in the dyeing of wool or rabbit hair fabric, after dyeing terminates, through washing with after soaping, drying, obtains the wool of pure natural dyeing, the rabbit hair or its wool fabric;
(5) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2) is controlling dyeing temperature at 20 DEG C ~ 100 DEG C, the dyeing of cotton yarn or COTTON FABRIC is directly used under the condition of dyeing time 30min ~ 150min, after dyeing terminates, wash the dye liquor of remained on surface with water, add the mordant prepared by certain solid-liquid ratio, and control certain temperature and dyeing time dyes, after dyeing terminates, through washing with after soaping, dry, obtain corresponding dyed cotton yarn or COTTON FABRIC;
(6) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2) is controlling dyeing temperature at 30 DEG C ~ 90 DEG C, the dyeing of wool, the rabbit hair or its wool fabric is directly used under the condition of dyeing time 30min ~ 240min, after dyeing terminates, wash the dye liquor of remained on surface with water, the mordant prepared is added by certain solid-liquid ratio, and control certain temperature and dyeing time dyes, after dyeing terminates, through washing with after soaping, drying, obtains corresponding dyeing wool, the rabbit hair or its wool fabric;
(7) the nature strength liquid of the green peel of walnut obtained in above-mentioned steps (2), the mordant configured is added according to certain ratio, obtain the walnut green husk pigment extract containing mordant, at control dyeing temperature at 20 DEG C ~ 100 DEG C, cotton yarn is directly used in or COTTON FABRIC, wool, the rabbit hair or its wool fabric dye under the condition of dyeing time 30min ~ 240min, after dyeing terminates, through washing with after soaping, drying, obtains corresponding dyed cotton yarn or COTTON FABRIC and dyeing wool, the rabbit hair or its wool fabric.
2. method according to claim 1, is characterized in that described is deionized water, pure water or distilled water for the aqueous solvent extracted and dye.
3. method according to claim 1, it is characterized in that the main active in the green peel of walnut extract that described Subcritical water chromotagraphy obtains is the natural colouring matters such as polyphenol, flavones and anthraquinone in green peel of walnut, preferred processing condition is solid-liquid ratio is 1:15 ~ 1:30, Extracting temperature 180 DEG C ~ 200 DEG C, extraction time is 50min ~ 60min, and preferred green peel of walnut grinding particle size is 80 orders; Under preferred process conditions, in green peel of walnut extract, total extract yield of polyphenol, flavones and anthraquinone isoreactivity composition is greater than 12%.
4. method according to claim 1, when it is characterized in that described direct employing green peel of walnut nature strength liquid to cotton yarn or COTTON FABRIC direct dyeing, preferred dyeing condition be dyeing temperature at 70 DEG C ~ 90 DEG C, dyeing time 100min ~ 150min.
5. method according to claim 1, when it is characterized in that described direct employing green peel of walnut nature strength liquid to cotton yarn or cotton fabric dyeing process, preferred dyeing condition is the pH value of adjustment solution is under the condition of 4.5, and dyeing temperature is 80 DEG C, and dyeing time is 120min.
6. method according to claim 1, it is characterized in that described direct employing green peel of walnut nature strength liquid to wool, the rabbit hair or its woolen direct dyeing time, preferred dyeing condition be dyeing temperature at 50 DEG C ~ 70 DEG C, dyeing time 120min ~ 180min.
7. method according to claim 1, it is characterized in that described direct employing green peel of walnut nature strength liquid to wool, the rabbit hair or its woolen direct dyeing time, preferred dyeing condition is that the pH value of extract is when being adjusted to 4.0, dyeing temperature controls at 60 DEG C, dyeing time 150min.
8. method according to claim 1, is characterized in that described cotton, the mordant of wool fabric is and the metal cations Fe that have fewer environmental impacts higher to human safety
2+, Fe
3+, Cu
2+, Zn
2+, Ti
2+, Mg
2+, Sn
2+deng sulfate or hydrochloride, the addition of mordant is 1 ~ 5% of fabric quality, and the dyeing temperature of rear mordant dyeing look is 80 DEG C, and dyeing time is 60min.
9. the method according to claim 1 step (7), it is characterized in that the process conditions optimized are for treating that by being equivalent to described in claim 8 mordant of dyeing and weaving thing 0.5% ~ 5% joins in the extract of the green peel of walnut extracted in advance, obtain the walnut green husk pigment extract containing mordant, at control dyeing temperature 80 DEG C, cotton yarn or COTTON FABRIC is directly used under the condition of dyeing time 120min, wool, the rabbit hair or its wool fabric dye, after dyeing terminates, through washing with after soaping, dry, obtain corresponding dyed cotton yarn or COTTON FABRIC and dyeing wool, the rabbit hair or its wool fabric.
10. method according to claim 1, it is characterized in that the DYED FABRICS adopting the method to obtain is the product of environmental protection, whole technical process is not with an organic solvent, the inorganic ions that the mordant used is safety, and the various active pigment composition in green peel of walnut has anti-oxidant and bacteriostasis, the dyeing of the cotton be fit for various uses, wool fabric, is more suitable for the dyeing for the article such as infant article, underwear.
Priority Applications (1)
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| CN106879577A (en) * | 2017-02-28 | 2017-06-23 | 江苏泗水纺织有限公司 | A kind of store method of walnut green husk pigment |
| CN106946863A (en) * | 2017-02-26 | 2017-07-14 | 浙江峰赫纺织有限公司 | A kind of Kaempferia galanga phenolic antioxidant and its application on bafta |
| CN107841157A (en) * | 2017-10-30 | 2018-03-27 | 潍坊友容实业有限公司 | A kind of Suaeda salsa Betacyanins extraction process |
| CN109953922A (en) * | 2019-04-16 | 2019-07-02 | 中国热带农业科学院南亚热带作物研究所 | A kind of Queensland nut peel extract and its preparation method and application |
| CN111454587A (en) * | 2020-04-24 | 2020-07-28 | 杭州彩润科技有限公司 | Comprehensive processing and utilizing method for dyeing of pericarpium juglandis |
| CN111519453A (en) * | 2020-06-01 | 2020-08-11 | 兰州理工大学 | Dyeing method for dyeing wool fibers by using walnut green husk pigment |
| CN112369433A (en) * | 2020-10-27 | 2021-02-19 | 中国农业大学 | Water-soluble bactericide and preparation method and application thereof |
| CN112593425A (en) * | 2020-12-05 | 2021-04-02 | 浙江灏宇科技有限公司 | Finishing method for improving color fastness of cotton fabric dyed by laccase-catalyzed plant dye |
| CN113863027A (en) * | 2021-09-23 | 2021-12-31 | 天津工业大学 | Method for dyeing cotton fabric by laccase-catalyzed oxidation of walnut green skin powder |
| CN114960230A (en) * | 2022-05-13 | 2022-08-30 | 常州纺织服装职业技术学院 | Preparation method of southern magnolia leaf pigment cotton cloth and southern magnolia leaf pigment cotton cloth with antibacterial property |
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| CN106946863A (en) * | 2017-02-26 | 2017-07-14 | 浙江峰赫纺织有限公司 | A kind of Kaempferia galanga phenolic antioxidant and its application on bafta |
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| CN107841157A (en) * | 2017-10-30 | 2018-03-27 | 潍坊友容实业有限公司 | A kind of Suaeda salsa Betacyanins extraction process |
| CN109953922A (en) * | 2019-04-16 | 2019-07-02 | 中国热带农业科学院南亚热带作物研究所 | A kind of Queensland nut peel extract and its preparation method and application |
| CN111454587B (en) * | 2020-04-24 | 2021-07-13 | 杭州彩润科技有限公司 | Comprehensive processing and utilizing method for dyeing of pericarpium juglandis |
| CN111454587A (en) * | 2020-04-24 | 2020-07-28 | 杭州彩润科技有限公司 | Comprehensive processing and utilizing method for dyeing of pericarpium juglandis |
| CN111519453A (en) * | 2020-06-01 | 2020-08-11 | 兰州理工大学 | Dyeing method for dyeing wool fibers by using walnut green husk pigment |
| CN111519453B (en) * | 2020-06-01 | 2021-04-27 | 兰州理工大学 | Dyeing method for dyeing wool fibers by using walnut green husk pigment |
| CN112369433A (en) * | 2020-10-27 | 2021-02-19 | 中国农业大学 | Water-soluble bactericide and preparation method and application thereof |
| CN112593425A (en) * | 2020-12-05 | 2021-04-02 | 浙江灏宇科技有限公司 | Finishing method for improving color fastness of cotton fabric dyed by laccase-catalyzed plant dye |
| CN113863027A (en) * | 2021-09-23 | 2021-12-31 | 天津工业大学 | Method for dyeing cotton fabric by laccase-catalyzed oxidation of walnut green skin powder |
| CN114960230A (en) * | 2022-05-13 | 2022-08-30 | 常州纺织服装职业技术学院 | Preparation method of southern magnolia leaf pigment cotton cloth and southern magnolia leaf pigment cotton cloth with antibacterial property |
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