CN113249983B - Method for dyeing black cashmere fiber or fabric by using natural plant pigment - Google Patents
Method for dyeing black cashmere fiber or fabric by using natural plant pigment Download PDFInfo
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- CN113249983B CN113249983B CN202110443651.8A CN202110443651A CN113249983B CN 113249983 B CN113249983 B CN 113249983B CN 202110443651 A CN202110443651 A CN 202110443651A CN 113249983 B CN113249983 B CN 113249983B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—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
- D06P1/673—Inorganic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/14—Wool
Abstract
The invention relates to the technical field of cashmere fiber or fabric dyeing, and discloses a method for dyeing black cashmere fiber or fabric by using natural plant pigment. The method comprises the following steps: (1) extracting walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment and green tea pigment respectively; (2) carrying out pretreatment before dyeing on the cashmere fiber or fabric by adopting pretreatment before dyeing liquid; (3) adding walnut green peel pigment, gallnut pigment, dioscorea cirrhosa pigment, green tea pigment, penetrating agent and nonionic surfactant into the pretreated cashmere fiber or fabric before dyeing according to a bath ratio of 1: 10-20, and dyeing; (4) and (3) washing and drying the dyed cashmere fiber or fabric. The method takes walnut green husks, gallnut, dioscorea cirrhosa and green tea leaves as raw materials to extract natural plant pigments, and the natural plant pigments are adopted to dye cashmere fibers or fabrics, so that environment-friendly black cashmere fibers or fabric products can be obtained.
Description
Technical Field
The invention relates to the technical field of cashmere fiber or fabric dyeing, in particular to a method for dyeing black cashmere fiber or fabric by using natural plant pigment.
Background
The cashmere is a thin fine cashmere layer which is grown on the outer epidermis layer of the goat and covered at the root of the goat coarse hair. Cashmere belongs to rare special animal fibers, is precious, and not only has low yield, but also has excellent quality and characteristics. The cashmere is a thin and curved fiber, and an air layer is arranged in the middle of the fiber, so the cashmere is light and soft in weight; cashmere is much finer than wool, and the cashmere fiber has small and smooth scales; the cashmere has high natural crimpness, compact arrangement in spinning and weaving, good cohesive force and good toughness. The cashmere integrates the advantages of fineness, lightness, thinness, softness, smoothness and warmth.
However, cashmere is more sensitive to acid, alkali and heat than fine wool, and fiber damage is obvious even under the conditions of lower temperature and lower concentration of acid and alkali liquor. At present, chemical synthetic dyes, such as acid dyes, neutral dyes and reactive dyes for protein fibers, are mainly used for dyeing cashmere. Because the dye is used for dyeing the cashmere under the conditions of higher temperature or stronger acid and alkali, the damage of the dyeing to the cashmere is larger. Along with the enhancement of environmental awareness of people, some textiles dyed and processed by chemical synthetic dyes can bring serious influence on human life health and human living environment, and the cashmere products dyed by the chemical synthetic dyes are not more and more in line with the image of high-grade cashmere products. Therefore, researchers begin to research the dyeing of cashmere by natural dyes, but the cashmere dyed by the traditional natural dyes has low dye uptake and cannot be dyed black. For example, chinese patent CN110714341A discloses a method for modifying cashmere fibers and dyeing cashmere with natural vegetable dyes; for another example, chinese patent CN109853257A discloses a natural plant dye dyeing process for cashmere cheese.
The cashmere belongs to high-grade products, and the cashmere is made into high-grade clothes such as winddresses, jackets, western-style clothes and the like, so that the production of cashmere environment-friendly black products becomes more important, and particularly, the cashmere is dyed into environment-friendly black by using natural plant pigments.
Disclosure of Invention
The invention aims to solve the problem that the prior natural plant pigment is difficult to dye the cashmere fiber or fabric into environment-friendly black color in the prior art, and provides a method for dyeing the black cashmere fiber or fabric by using the natural plant pigment.
In order to achieve the above objects, the present invention provides a method for dyeing black cashmere fibers or fabrics with natural plant pigments, comprising the steps of:
(1) respectively extracting walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment and green tea pigment;
(2) carrying out pretreatment before dyeing on cashmere fibers or fabrics by adopting pretreatment before dyeing liquid, wherein the pretreatment liquid contains hydrogen peroxide solution, penetrant, acid protease and anionic surfactant;
(3) adding walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment, green tea leaf pigment, penetrating agent and nonionic surfactant into the pretreated cashmere fiber or fabric before dyeing according to a bath ratio of 1: 10-20, and dyeing;
(4) and (3) washing, soaping, washing and drying the dyed cashmere fiber or fabric.
Preferably, the extraction method of the walnut green husk pigment comprises the following steps:
a1, peeling fresh walnuts to obtain fresh walnut green husks, drying the fresh walnut green husks at 95-105 ℃, and then crushing to obtain walnut green husk powder;
a2, performing cooking extraction on walnut green husk powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
and A3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 60-65 ℃ to obtain the walnut green husk pigment.
Preferably, the extraction method of the Chinese gall pigment comprises the following steps:
b1, drying fresh Chinese gall at 95-105 ℃, and then crushing to obtain Chinese gall powder;
b2, performing cooking extraction on the Chinese gall powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
and B3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at the temperature of 60-65 ℃ to obtain the Chinese gall pigment.
Preferably, the extraction method of dioscorea cirrhosa pigment comprises the following steps:
c1, cleaning and crushing fresh dioscorea cirrhosa to obtain dioscorea cirrhosa blocks;
c2, steaming and extracting the dioscorea cirrhosa blocks and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
c3, after extraction, carrying out vacuum filtration to obtain the dioscorea cirrhosa pigment.
Preferably, the extraction method of green tea leaf pigment comprises the following steps:
d1, drying the crude tea leaves at 95-105 ℃, and then crushing to obtain green tea powder;
d2, performing cooking extraction on the green tea powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
d3, after extraction, carrying out suction filtration under reduced pressure to obtain the green tea pigment.
Preferably, the method for pretreating cashmere fibers or fabrics before dyeing in the step (2) comprises the following steps:
s1, injecting a pre-dyeing pretreatment liquid into a dye vat according to a bath ratio of 1: 10-20, wherein the pre-dyeing pretreatment liquid contains 6-10 g/L of 27-28 mass% hydrogen peroxide solution, 1-2 g/L of penetrating agent, 2-4% (o.w.f) of acid protease and 2-3 g/L of anionic surfactant;
s2, adjusting the pH value of the pretreatment solution before dyeing to 5.5-6.5 by adopting an acetic acid-sodium acetate buffer solution;
s3, pretreating the cashmere loose fibers at room temperature, heating the cashmere loose fibers at the same time, and treating the cashmere fibers or the fabrics in the pretreatment solution before dyeing for 45-50 min after the temperature is increased from the room temperature to 50-55 ℃;
and S4, discharging liquid after the pretreatment before dyeing is finished, and washing the cashmere fibers or fabrics pretreated before dyeing by using clear water.
Preferably, in step S1, the penetrant is JFC and the anionic surfactant is OEP-98.
Preferably, the temperature rise rate in step S3 is 0.5-1.5 ℃/min.
Preferably, the method for dyeing the cashmere fiber or fabric in the step (3) comprises the following steps:
m1, adding 5-8% (o.w.f) of walnut green husk pigment, 2-5% (o.w.f) of Chinese gall pigment, 1-3% (o.w.f) of dioscorea cirrhosa natural plant pigment, 1-3% (o.w.f) of green tea pigment, 1-2% (o.w.f) of penetrating agent and 1-2% (o.w.f) of nonionic surfactant into a dye vat according to a bath ratio of 1: 10-20 to prepare a dye;
m2, adjusting the pH value of the dye to 5-6 by adopting an acetic acid-sodium acetate buffer solution;
m3, dyeing the pretreated cashmere fibers or fabrics at room temperature, simultaneously heating, and dyeing the pretreated cashmere fibers or fabrics in the dye for 20-30 min after the temperature is raised from the room temperature to 50-55 ℃;
m4, adding 2-3% (o.w.f) of mordant into the dye, then heating the temperature to 65-70 ℃, dyeing for 20-30 min, then heating the temperature to 85-95 ℃, and dyeing for 20-30 min;
m5, after dyeing is finished, cooling the temperature to 50-55 ℃, and washing, soaping, washing and drying.
Preferably, in step M1, the penetrant is JFC and the non-ionic surfactant is peregal O.
Preferably, in step M4, the mordant is ferrous sulfate and/or ferric sulfate.
Preferably, the heating and cooling rates in the steps M3-M5 are both 0.8-1.2 ℃/min.
Preferably, the method for washing the cashmere fibers or fabrics in the step (4) comprises the following steps: washing the dyed cashmere fibers or fabrics in clear water at 50-55 ℃ for 10-20 min, adding a soaping agent of 1.8-2.2g/L for soaping at 60-70 ℃ for 10-20 min, and then washing in clear water at 50-55 ℃ for 5-10 min.
The invention has the following beneficial effects:
1) the invention provides a method for dyeing environment-friendly black cashmere fiber or fabric by using natural plant pigment;
2) the walnut green husk natural plant pigment extracted by the invention is used for dyeing cashmere fibers or fabrics, so that waste can be changed into valuable, and the effect of protecting the ecological environment is achieved while resources are reasonably developed and utilized;
3) the walnut green seedcase natural plant pigment extracted by the invention is used for dyeing cashmere fibers or fabrics, and can be matched with natural plant pigments such as gallnut, dioscorea cirrhosa, green tea leaves and the like to dye the cashmere fibers or fabrics into environment-friendly black;
4) the invention uses natural plant pigment to dye environment-friendly black cashmere fiber or fabric, the pollution is small, and the pollution is controlled at the front end;
5) the invention uses natural plant pigment to dye the environment-friendly black cashmere fiber or fabric, can be used for cashmere fiber or fabric high-grade clothes, and has high added value of products.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for dyeing black cashmere fiber or fabric by using natural plant pigment, which is characterized by comprising the following steps:
(1) respectively extracting walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment and green tea pigment;
(2) carrying out pretreatment before dyeing on cashmere fibers or fabrics by adopting pretreatment before dyeing liquid, wherein the pretreatment liquid contains hydrogen peroxide solution, penetrant, acid protease and anionic surfactant;
(3) adding walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment, green tea leaf pigment, penetrating agent and nonionic surfactant into the pretreated cashmere fiber or fabric before dyeing according to a bath ratio of 1: 10-20, and dyeing;
(4) and (3) washing, soaping, washing and drying the dyed cashmere fiber or fabric.
According to the method, the cashmere fiber or fabric is pretreated in the pretreatment liquid before dyeing containing specific components, and then the cashmere fiber or fabric is dyed in the dye containing walnut green husk pigment, nutgall pigment, dioscorea cirrhosa pigment, green tea leaf pigment, penetrating agent and nonionic surfactant according to a specific bath ratio, so that the environment-friendly black cashmere fiber or fabric product can be dyed. The penetrant used in step (2) and step (3) may be the same or different.
In particular embodiments, the bath ratio used in the dyeing process may be 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, or 1: 20.
In the method of the invention, the extraction of the walnut green seedcase pigment, the gallnut pigment, the dioscorea cirrhosa pigment and the green tea pigment can be carried out according to the method conventionally adopted in the field.
In a preferred embodiment, in order to sufficiently extract the pigment and the effective components in the pigment, the extraction of the pigment from the walnut green husk can be carried out according to the following steps:
a1, peeling fresh walnuts to obtain fresh walnut green husks, drying the fresh walnut green husks at 95-105 ℃, and then crushing to obtain walnut green husk powder;
a2, performing cooking extraction on walnut green husk powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
and A3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 60-65 ℃ to obtain the walnut green husk pigment.
In a preferred embodiment, in order to sufficiently extract the pigment and the effective components in the pigment, the extraction of the gallnut pigment can be carried out according to the following steps:
b1, drying fresh Chinese gall at 95-105 ℃, and then crushing to obtain Chinese gall powder;
b2, performing cooking extraction on the Chinese gall powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
and B3, after the cooking is finished, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at the temperature of 60-65 ℃ to obtain the Chinese gall pigment.
In a preferred embodiment, in order to sufficiently extract the pigment and the effective components in the pigment, the extraction of the dioscorea cirrhosa pigment can be performed according to the following steps:
c1, cleaning and crushing fresh dioscorea cirrhosa to obtain dioscorea cirrhosa blocks;
c2, steaming and extracting the dioscorea cirrhosa blocks and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
c3, after extraction, carrying out vacuum filtration to obtain the dioscorea cirrhosa pigment.
In a preferred embodiment, in order to sufficiently extract the pigments and the effective components in the pigments, the extraction of the green tea leaf pigments may be performed according to the following steps:
d1, drying the crude tea leaves at 95-105 ℃, and then crushing to obtain green tea powder;
d2, performing cooking extraction on the green tea powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
d3, after extraction, carrying out suction filtration under reduced pressure to obtain the green tea pigment.
In the method, the pretreatment before dyeing is carried out on the cashmere fiber or fabric, and the method has the following functions: improve the dyeing performances of the cashmere fiber or fabric, such as dye uptake, level dyeing property and the like. The pretreatment before dyeing of the cashmere fiber or fabric can be carried out according to a specific method or a conventional method in the field, and the pretreatment before dyeing only contains a hydrogen peroxide solution, a penetrating agent, an acid protease and an anionic surfactant.
In a preferred embodiment, in order to improve the pretreatment effect, it is necessary to control the bath ratio, the usage ratio of the hydrogen peroxide solution, the penetrant, the acidic protease and the anionic surfactant in the pretreatment liquid before dyeing, the pH of the pretreatment liquid before dyeing, and the pretreatment temperature and time reasonably. The pretreatment before dyeing of the cashmere fiber or fabric in the step (2) can be carried out according to the following steps:
s1, injecting a pre-dyeing pretreatment liquid into a dye vat according to a bath ratio of 1: 10-20, wherein the pre-dyeing pretreatment liquid contains 6-10 g/L of 27-28 mass% hydrogen peroxide solution, 1-2 g/L of penetrating agent, 2-4% (o.w.f) of acid protease and 2-3 g/L of anionic surfactant;
s2, adjusting the pH value of the pretreatment solution before dyeing to 5.5-6.5 by adopting an acetic acid-sodium acetate buffer solution;
s3, pretreating the cashmere loose fibers at room temperature, heating the cashmere loose fibers at the same time, and treating the cashmere fibers or the fabrics in the pretreatment solution before dyeing for 45-50 min after the temperature is increased from the room temperature to 50-55 ℃;
and S4, discharging liquid after the pretreatment before dyeing is finished, and washing the cashmere fibers or fabrics pretreated before dyeing by using clear water.
In particular embodiments, the bath ratio of the pre-dye pretreatment may be 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, or 1: 20.
In particular embodiments, the pH of the pre-dye pretreatment liquor may be adjusted to 5.5, 5.6, 5.7, 5.8, 5.9, 6, 6.1, 6.2, 6.3, 6.4, or 6.5.
In the methods of the present invention, the osmotic and anionic surfactants may be conventional in the art. In a preferred embodiment, in step S1, the penetrant is JFC and the anionic surfactant is OEP-98.
In step S3, the temperature rise needs to be maintained at a low temperature rise rate. In a preferred embodiment, the temperature increase rate in step S3 is 0.5 to 1.5 ℃/min, and may be, for example, 0.5 ℃/min, 0.7 ℃/min, 0.9 ℃/min, 1 ℃/min, 1.1 ℃/min, 1.2 ℃/min, 1.3 ℃/min, or 1.5 ℃/min. In a more preferred embodiment, the temperature increase rate in step S3 is 1 ℃/min.
In the method of the present invention, dyeing of cashmere fibers or fabrics may be performed according to conventional methods in the art.
In a preferred embodiment, in order to improve the dyeing effect, the dyeing of the cashmere fiber or fabric in the step (3) may be performed according to the following steps:
m1, adding 5-8% (o.w.f) of walnut green husk pigment, 2-5% (o.w.f) of Chinese gall pigment, 1-3% (o.w.f) of dioscorea cirrhosa pigment, 1-3% (o.w.f) of green tea pigment, 1-2% (o.w.f) of penetrating agent and 1-2% (o.w.f) of nonionic surfactant into a dye vat according to a bath ratio of 1: 10-20 to prepare a dye;
m2, adjusting the pH value of the dye to 5-6 by adopting an acetic acid-sodium acetate buffer solution;
m3, dyeing the pretreated cashmere fibers or fabrics at room temperature, simultaneously heating, and dyeing the pretreated cashmere fibers or fabrics in the dye for 20-30 min after the temperature is raised from the room temperature to 50-55 ℃;
m4, adding 2-3% (o.w.f) of mordant into the dye, then heating the temperature to 65-70 ℃, dyeing for 20-30 min, then heating the temperature to 85-95 ℃, and dyeing for 20-30 min;
m5, after dyeing is finished, cooling the temperature to 50-55 ℃, and washing, soaping, washing and drying.
In the preferred embodiment, the dyeing effect is improved by reasonably controlling the use amounts of the walnut green husk pigment, the Chinese gall pigment, the dioscorea cirrhosa pigment, the green tea pigment, the penetrating agent and the nonionic surfactant, controlling the pH value of the dye and adopting a sectional heating dyeing mode.
In the method of the present invention, in step M1, the penetrant and the non-ionic surfactant may be selected conventionally in the art.
In a preferred embodiment, in step M1, the penetrant is JFC and the non-ionic surfactant is peregal O.
In the method of the present invention, in step M4, the mordant may be a conventional choice in the art. In a specific embodiment, in step M4, the mordant may be ferrous sulfate and/or ferric sulfate.
During the dyeing process, the temperature rise and the temperature fall are required to be kept at a slower temperature rise and temperature fall rate every time. In a preferred embodiment, the temperature rising and lowering rates in the steps M3-M5 are both 0.8-1.2 ℃/min, such as 0.8 ℃/min, 0.9 ℃/min, 1 ℃/min, 1.1 ℃/min or 1.2 ℃/min.
In the method of the present invention, the washing of the dyed cashmere fibers or fabrics with water may be performed according to the conventional procedures in the art. In a preferred embodiment, in order to wash the residual dye in the cashmere fiber or fabric clean without greatly affecting the dyeing effect, the washing of the cashmere fiber or fabric in the step (4) may be performed according to the following operations: washing the dyed cashmere fibers or fabrics in clear water at 50-55 ℃ for 10-20 min, adding a soaping agent of 1.8-2.2g/L for soaping at 60-70 ℃ for 10-20 min, and then washing in clear water at 50-55 ℃ for 5-10 min.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
The method described in each of the examples and comparative examples comprises dyeing cashmere woven fabric and cashmere loose fiber, respectively.
Example 1
(1) Respectively extracting walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment and green tea pigment;
(2) carrying out pretreatment before dyeing on cashmere fibers or fabrics by adopting pretreatment before dyeing liquid, wherein the pretreatment liquid contains hydrogen peroxide solution, penetrant, acid protease and anionic surfactant;
(3) adding walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment, green tea leaf pigment, penetrating agent and nonionic surfactant into the pretreated cashmere fiber or fabric according to the bath ratio of 1:20, and dyeing;
(4) washing, soaping, washing and drying the dyed cashmere fiber or fabric;
the extraction method of the walnut green husk pigment comprises the following steps:
a1, peeling fresh walnuts to obtain fresh walnut green husks, drying the fresh walnut green husks at 98 ℃, and then crushing to obtain walnut green husk powder;
a2, performing cooking extraction on walnut green husk powder and deionized water according to the ratio of 1:20, wherein the extraction temperature is 98 ℃, and the extraction time is 3 hours;
a3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 63 ℃ to obtain walnut green husk pigment;
the extraction method of the Chinese gall pigment comprises the following steps:
b1, drying fresh gallnut at 98 ℃, and then crushing to obtain gallnut powder;
b2, cooking and extracting the nutgall powder and deionized water according to the ratio of 1:20, wherein the extraction temperature is 98 ℃, and the extraction time is 3 hours;
b3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 63 ℃ to obtain Chinese gall pigment;
the method for extracting dioscorea cirrhosa pigment comprises the following steps:
c1, cleaning and crushing fresh dioscorea cirrhosa to obtain dioscorea cirrhosa blocks;
c2, steaming and extracting the dioscorea cirrhosa blocks and deionized water according to the ratio of 1:20, wherein the extraction temperature is 99 ℃, and the extraction time is 3 hours;
c3, after extraction, carrying out vacuum filtration to obtain dioscorea cirrhosa pigment;
the extraction method of the green tea pigment comprises the following steps:
d1, drying the crude tea leaves at 98 ℃, and then crushing to obtain green tea powder;
d2, performing cooking extraction on the green tea powder and deionized water according to the ratio of 1:20, wherein the extraction temperature is 99 ℃, and the extraction time is 3 hours;
d3, after extraction, carrying out vacuum filtration to obtain green tea pigment;
the method for pretreating cashmere fibers or fabrics before dyeing in the step (2) comprises the following steps:
s1, injecting a pre-dyeing pretreatment liquid into a dye vat according to a bath ratio of 1:20, wherein the pre-dyeing pretreatment liquid contains 8g/L of 27.5 mass% hydrogen peroxide solution, 2g/L of penetrating agent JFC, 3% (o.w.f) of acid protease and 2g/L of anionic surfactant OEP-98;
s2, adjusting the pH value of the pretreatment solution before dyeing to 6 by adopting acetic acid-sodium acetate buffer solution;
s3, pretreating the cashmere loose fibers at room temperature, heating at the rate of 1 ℃/min, and treating the cashmere fibers or fabrics in pretreatment liquid before dyeing for 50min after the temperature is increased from the room temperature to 50 ℃;
s4, discharging liquid after the pretreatment before dyeing is finished, and washing the cashmere fibers or fabrics after the pretreatment before dyeing with clear water;
the method for dyeing the cashmere fiber or fabric in the step (3) comprises the following steps:
m1, adding 5% (o.w.f) of walnut green husk pigment, 2% (o.w.f) of nutgall pigment, 2% (o.w.f) of dioscorea cirrhosa natural plant pigment, 3% (o.w.f) of green tea pigment, 2% (o.w.f) of penetrating agent JFC and 2% (o.w.f) of nonionic surfactant peregal O into a dye vat according to a bath ratio of 1:20 to prepare a dye;
m2, adjusting the pH value of the dye to 5 by adopting acetic acid-sodium acetate buffer solution;
m3, dyeing the pretreated cashmere fiber or fabric at room temperature, simultaneously heating at the speed of 1 ℃/min, and dyeing the pretreated cashmere fiber or fabric in a dye for 30min after the temperature is raised from the room temperature to 50 ℃;
m4, adding 3% (o.w.f) of mordant ferrous sulfate into the dye, then raising the temperature to 65 ℃ at the speed of 1 ℃/min, dyeing for 30min, then raising the temperature to 85 ℃ at the speed of 1 ℃/min, and dyeing for 30 min;
m5, after dyeing is finished, reducing the temperature to 50 ℃ at the speed of 1 ℃/min, washing, soaping, washing and drying;
the method for washing the cashmere fibers or the fabrics in the step (4) comprises the following steps: washing the dyed cashmere fiber or fabric in 50 deg.C clear water for 20min, adding 2g/L soaping agent, soaping at 60 deg.C for 20min, and washing in 50 deg.C clear water for 10 min.
Example 2
(1) Respectively extracting walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment and green tea pigment;
(2) carrying out pretreatment before dyeing on cashmere fibers or fabrics by adopting pretreatment before dyeing liquid, wherein the pretreatment liquid contains hydrogen peroxide solution, penetrant, acid protease and anionic surfactant;
(3) adding walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment, green tea leaf pigment, penetrating agent and nonionic surfactant into the pretreated cashmere fiber or fabric according to the bath ratio of 1:15, and dyeing;
(4) washing, soaping, washing and drying the dyed cashmere fiber or fabric;
the extraction method of the walnut green husk pigment comprises the following steps:
a1, peeling fresh walnuts to obtain fresh walnut green husks, drying the fresh walnut green husks at 103 ℃, and then crushing to obtain walnut green husk powder;
a2, performing cooking extraction on walnut green husk powder and deionized water according to the ratio of 1:30, wherein the extraction temperature is 99 ℃, and the extraction time is 5 hours;
a3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 60 ℃ to obtain walnut green husk pigment;
the extraction method of the Chinese gall pigment comprises the following steps:
b1, drying fresh gallnut at 95 ℃, and then crushing to obtain gallnut powder;
b2, cooking and extracting the nutgall powder and deionized water according to the ratio of 1:25, wherein the extraction temperature is 100 ℃, and the extraction time is 5 hours;
b3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 65 ℃ to obtain Chinese gall pigment;
the method for extracting dioscorea cirrhosa pigment comprises the following steps:
c1, cleaning and crushing fresh dioscorea cirrhosa to obtain dioscorea cirrhosa blocks;
c2, steaming and extracting the dioscorea cirrhosa blocks and deionized water according to the ratio of 1:25, wherein the extraction temperature is 100 ℃, and the extraction time is 4 hours;
c3, after extraction, carrying out vacuum filtration to obtain dioscorea cirrhosa pigment;
the extraction method of the green tea pigment comprises the following steps:
d1, drying the crude tea leaves at 105 ℃, and then crushing to obtain green tea powder;
d2, steaming and extracting the green tea powder and deionized water according to the ratio of 1:30, wherein the extraction temperature is 98 ℃, and the extraction time is 4 h;
d3, after extraction, carrying out vacuum filtration to obtain green tea pigment;
the method for pretreating cashmere fibers or fabrics before dyeing in the step (2) comprises the following steps:
s1, injecting a pre-dyeing pretreatment liquid into a dye vat according to a bath ratio of 1:15, wherein the pre-dyeing pretreatment liquid contains 6g/L of 27 mass% hydrogen peroxide solution, 1g/L of penetrating agent JFC, 4% (o.w.f) of acid protease and 2.5g/L of anionic surfactant OEP-98;
s2, adjusting the pH value of the pretreatment solution before dyeing to 5.5 by adopting acetic acid-sodium acetate buffer solution;
s3, pretreating cashmere loose fibers at room temperature, heating at the speed of 0.7 ℃/min, and treating the cashmere fibers or fabrics in pretreatment liquid before dyeing for 45min after the temperature is increased from the room temperature to 55 ℃;
s4, discharging liquid after the pretreatment before dyeing is finished, and washing the cashmere fibers or fabrics after the pretreatment before dyeing with clear water;
the method for dyeing the cashmere fiber or fabric in the step (3) comprises the following steps:
m1, adding 8% (o.w.f) of walnut green husk pigment, 5% (o.w.f) of nutgall pigment, 1% (o.w.f) of dioscorea cirrhosa natural plant pigment, 2% (o.w.f) of green tea pigment, 1% (o.w.f) of penetrating agent JFC and 1.5% (o.w.f) of nonionic surfactant peregal O into a dye vat according to a bath ratio of 1:15 to prepare a dye;
m2, adjusting the pH value of the dye to 5.5 by adopting acetic acid-sodium acetate buffer solution;
m3, dyeing the pretreated cashmere fiber or fabric at room temperature, simultaneously heating at the speed of 1.2 ℃/min, and dyeing the pretreated cashmere fiber or fabric in a dye for 25min after the temperature is raised from the room temperature to 55 ℃;
m4, adding 2% (o.w.f) of mordant iron sulfate into the dye, then raising the temperature to 68 ℃ at the speed of 0.8 ℃/min, dyeing for 20min, and then raising the temperature to 90 ℃ at the speed of 1.2 ℃/min, and dyeing for 25 min;
m5, after dyeing is finished, reducing the temperature to 53 ℃ at the speed of 0.8 ℃/min, washing with water, soaping, washing with water, and drying;
the method for washing the cashmere fibers or the fabrics in the step (4) comprises the following steps: washing the dyed cashmere fiber or fabric in 55 deg.C clear water for 15min, adding 2.2g/L soaping agent, soaping at 65 deg.C for 10min, and washing at 53 deg.C for 8 min.
Example 3
(1) Respectively extracting walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment and green tea pigment;
(2) carrying out pretreatment before dyeing on cashmere fibers or fabrics by adopting pretreatment before dyeing liquid, wherein the pretreatment liquid contains hydrogen peroxide solution, penetrant, acid protease and anionic surfactant;
(3) adding walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment, green tea leaf pigment, penetrating agent and nonionic surfactant into the pretreated cashmere fiber or fabric according to the bath ratio of 1:10, and dyeing;
(4) washing, soaping, washing and drying the dyed cashmere fiber or fabric;
the extraction method of the walnut green husk pigment comprises the following steps:
a1, peeling fresh walnuts to obtain fresh walnut green husks, drying the fresh walnut green husks at 95 ℃, and then crushing to obtain walnut green husk powder;
a2, performing cooking extraction on walnut green husk powder and deionized water according to the ratio of 1:25, wherein the extraction temperature is 100 ℃, and the extraction time is 4 hours;
a3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 65 ℃ to obtain walnut green husk pigment;
the extraction method of the Chinese gall pigment comprises the following steps:
b1, drying fresh gallnut at 105 ℃, and then crushing to obtain gallnut powder;
b2, cooking and extracting the nutgall powder and deionized water according to the ratio of 1:30, wherein the extraction temperature is 99 ℃, and the extraction time is 4 hours;
b3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 60 ℃ to obtain Chinese gall pigment;
the method for extracting dioscorea cirrhosa pigment comprises the following steps:
c1, cleaning and crushing fresh dioscorea cirrhosa to obtain dioscorea cirrhosa blocks;
c2, steaming and extracting the dioscorea cirrhosa blocks and deionized water according to the ratio of 1:30, wherein the extraction temperature is 99 ℃, and the extraction time is 5 hours;
c3, after extraction, carrying out vacuum filtration to obtain the dioscorea cirrhosa pigment. (ii) a
The extraction method of the green tea pigment comprises the following steps:
d1, drying the tea leaves at 95 ℃ and then crushing to obtain green tea powder;
d2, performing cooking extraction on the green tea powder and deionized water according to the ratio of 1:25, wherein the extraction temperature is 100 ℃, and the extraction time is 5 hours;
d3, after extraction, carrying out vacuum filtration to obtain green tea pigment;
the method for pretreating cashmere fibers or fabrics before dyeing in the step (2) comprises the following steps:
s1, injecting a pre-dyeing pretreatment liquid into a dye vat according to a bath ratio of 1:10, wherein the pre-dyeing pretreatment liquid contains 10g/L of 28 mass% hydrogen peroxide solution, 1.5g/L of penetrating agent JFC, 2% (o.w.f) of acid protease and 3g/L of anionic surfactant OEP-98;
s2, adjusting the pH value of the pretreatment solution before dyeing to 6.5 by adopting acetic acid-sodium acetate buffer solution;
s3, pretreating the cashmere loose fibers at room temperature, heating at the speed of 0.5-1.3 ℃/min, and treating the cashmere fibers or fabrics in pretreatment liquid before dyeing for 47min after the temperature is increased from room temperature to 53 ℃;
s4, discharging liquid after the pretreatment before dyeing is finished, and washing the cashmere fibers or fabrics after the pretreatment before dyeing with clear water;
the method for dyeing the cashmere fiber or fabric in the step (3) comprises the following steps:
m1, adding 7% (o.w.f) of walnut green husk pigment, 3% (o.w.f) of nutgall pigment, 3% (o.w.f) of dioscorea cirrhosa natural plant pigment, 1% (o.w.f) of green tea pigment, 1.5% (o.w.f) of penetrating agent JFC and 1% (o.w.f) of nonionic surfactant peregal O into a dye vat according to a bath ratio of 1:10 to prepare a dye;
m2, adjusting the pH value of the dye to 6 by adopting acetic acid-sodium acetate buffer solution;
m3, dyeing the pretreated cashmere fibers or fabrics at room temperature, simultaneously heating at the speed of 0.8 ℃/min, and dyeing the pretreated cashmere fibers or fabrics in the dye for 20min after the temperature is raised from the room temperature to 52 ℃;
m4, adding 2.5% (o.w.f) mordant ferrous sulfate and ferric sulfate into the dye, then raising the temperature to 70 ℃ at the speed of 1.2 ℃/min, dyeing for 25min, and then raising the temperature to 95 ℃ at the speed of 0.8 ℃/min, and dyeing for 20 min;
m5, after dyeing is finished, reducing the temperature to 55 ℃ at the speed of 1.2 ℃/min, washing with water, soaping, washing with water, and drying;
the method for washing the cashmere fibers or the fabrics in the step (4) comprises the following steps: washing the dyed cashmere fiber or fabric in clean water at 53 deg.C for 10min, adding 1.8g/L soaping agent, soaping at 70 deg.C for 15min, and washing at 55 deg.C for 5 min.
Comparative example 1
The procedure of example 3 was followed except that no walnut green husk pigment was added during the dyeing in step (3).
Comparative example 2
The procedure of example 3 was followed except that no Galla chinensis pigment was added during the dyeing in step (3).
Comparative example 3
The procedure of example 3 was followed except that, in the dyeing of step (3), dioscorea cirrhosa pigment was not added.
Comparative example 4
The procedure of example 3 was followed except that, in the dyeing of step (3), green tea leaf pigment was not added.
Comparative example 5
The procedure of example 3 was followed except that the dyeing process was carried out directly without pre-dyeing treatment as described in step (2).
Comparative example 6
The procedure is as in example 3 except that after the mordant is added in step M4, the temperature is raised to 95 ℃ directly at a rate of 0.8 ℃/min for 45min without two stepwise increases.
Test example
The color and color fastness of cashmere products dyed according to the methods of examples 1 to 3 and comparative examples 1 to 6 were measured, and the results are shown in tables 1 and 2.
TABLE 1 dyed Fabric color parameters
TABLE 2 fastness test results of dyed fabrics
The results in table 1 show that the environment-friendly black cashmere fiber or fabric product can be obtained by dyeing the cashmere fiber or fabric by the method of the invention under the condition that the fastness of the dyed fabric is not changed.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (12)
1. A method for dyeing black cashmere fiber or fabric by using natural plant pigment is characterized by comprising the following steps:
(1) respectively extracting walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment and green tea pigment;
(2) pretreating cashmere fibers or fabrics before dyeing by adopting pretreatment liquid before dyeing, wherein the pretreatment liquid contains hydrogen peroxide solution, penetrant, acid protease and anionic surfactant OEP-98;
(3) adding walnut green seedcase pigment, gallnut pigment, dioscorea cirrhosa pigment, green tea leaf pigment, penetrating agent and nonionic surfactant into the pretreated cashmere fiber or fabric before dyeing according to a bath ratio of 1: 10-20, and dyeing;
(4) washing, soaping, washing and drying the dyed cashmere fiber or fabric;
the method for dyeing the cashmere fiber or fabric in the step (3) comprises the following steps:
m1, adding 5-8% (o.w.f) of walnut green husk pigment, 2-5% (o.w.f) of Chinese gall pigment, 1-3% (o.w.f) of dioscorea cirrhosa natural plant pigment, 1-3% (o.w.f) of green tea pigment, 1-2% (o.w.f) of penetrating agent and 1-2% (o.w.f) of nonionic surfactant into a dye vat according to a bath ratio of 1: 10-20 to prepare a dye;
m2, adjusting the pH value of the dye to 5-6 by adopting an acetic acid-sodium acetate buffer solution;
m3, dyeing the pretreated cashmere fibers or fabrics at room temperature, simultaneously heating, and dyeing the pretreated cashmere fibers or fabrics in the dye for 20-30 min after the temperature is raised from the room temperature to 50-55 ℃;
m4, adding 2-3% (o.w.f) of mordant into the dye, then heating the temperature to 65-70 ℃, dyeing for 20-30 min, then heating the temperature to 85-95 ℃, and dyeing for 20-30 min;
m5, after dyeing is finished, cooling the temperature to 50-55 ℃, and washing, soaping, washing and drying.
2. The method as claimed in claim 1, wherein the extraction method of the pigment from the green husk of walnut comprises the following steps:
a1, peeling fresh walnuts to obtain fresh walnut green husks, drying the fresh walnut green husks at 95-105 ℃, and then crushing to obtain walnut green husk powder;
a2, performing cooking extraction on walnut green husk powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
and A3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at 60-65 ℃ to obtain the walnut green husk pigment.
3. The method according to claim 1, wherein the extraction method of the Chinese gall pigment comprises the following steps:
b1, drying fresh Chinese gall at 95-105 ℃, and then crushing to obtain Chinese gall powder;
b2, performing cooking extraction on the Chinese gall powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
and B3, after cooking, filtering and collecting supernatant, and then concentrating the supernatant under reduced pressure at the temperature of 60-65 ℃ to obtain the Chinese gall pigment.
4. The method according to claim 1, wherein the method for extracting dioscorea cirrhosa pigment comprises the following steps:
c1, cleaning and crushing fresh dioscorea cirrhosa to obtain dioscorea cirrhosa blocks;
c2, steaming and extracting the dioscorea cirrhosa blocks and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
c3, after extraction, carrying out vacuum filtration to obtain the dioscorea cirrhosa pigment.
5. The method according to claim 1, wherein the extraction method of the green tea leaf pigment comprises the steps of:
d1, drying the crude tea leaves at 95-105 ℃, and then crushing to obtain green tea powder;
d2, performing cooking extraction on the green tea powder and deionized water according to the ratio of 1: 20-30, wherein the extraction temperature is 98-100 ℃, and the extraction time is 3-5 hours;
d3, after extraction, carrying out suction filtration under reduced pressure to obtain the green tea pigment.
6. The method according to any one of claims 1 to 5, wherein the method for pre-dyeing the cashmere fibres or fabrics in step (2) comprises the following steps:
s1, injecting a pre-dyeing pretreatment liquid into a dye vat according to a bath ratio of 1: 10-20, wherein the pre-dyeing pretreatment liquid contains 6-10 g/L of 27-28 mass% hydrogen peroxide solution, 1-2 g/L of penetrating agent, 2-4% (o.w.f) of acid protease and 2-3 g/L of anionic surfactant;
s2, adjusting the pH value of the pretreatment solution before dyeing to 5.5-6.5 by adopting an acetic acid-sodium acetate buffer solution;
s3, pretreating the cashmere loose fibers at room temperature, heating the cashmere loose fibers at the same time, and treating the cashmere fibers or the fabrics in the pretreatment solution before dyeing for 45-50 min after the temperature is increased from the room temperature to 50-55 ℃;
and S4, discharging liquid after the pretreatment before dyeing is finished, and washing the cashmere fibers or fabrics pretreated before dyeing by using clear water.
7. The method of claim 6, wherein in step S1, the osmotic agent is JFC.
8. The method according to claim 6, wherein the temperature increase rate in step S3 is 0.5-1.5 ℃/min.
9. The method of claim 1, wherein in step M1, the penetrating agent is JFC and the non-ionic surfactant is peregal O.
10. The method according to claim 1, wherein in step M4, the mordant is ferrous sulfate and/or ferric sulfate.
11. The method of claim 1, wherein the temperature increase and decrease in the steps M3-M5 are at a rate of 0.8-1.2 ℃/min.
12. The method according to any one of claims 1 to 5, wherein the method for washing the cashmere fibres or fabrics in step (4) comprises: washing the dyed cashmere fibers or fabrics in clear water at 50-55 ℃ for 10-20 min, adding a soaping agent of 1.8-2.2g/L for soaping at 60-70 ℃ for 10-20 min, and then washing in clear water at 50-55 ℃ for 5-10 min.
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