CN109098011B - Method for dyeing jean yarns by using natural indigo - Google Patents
Method for dyeing jean yarns by using natural indigo Download PDFInfo
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- 238000004043 dyeing Methods 0.000 title claims abstract description 74
- 235000000177 Indigofera tinctoria Nutrition 0.000 title claims abstract description 45
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229940097275 indigo Drugs 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 41
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 75
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims abstract description 75
- 239000003381 stabilizer Substances 0.000 claims abstract description 36
- 230000003647 oxidation Effects 0.000 claims abstract description 31
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 230000000149 penetrating effect Effects 0.000 claims abstract description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 5
- 229920000742 Cotton Polymers 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 46
- 238000005096 rolling process Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 29
- 239000012452 mother liquor Substances 0.000 claims description 19
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 10
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 10
- 150000004056 anthraquinones Chemical class 0.000 claims description 10
- 239000008103 glucose Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000009970 yarn dyeing Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000000975 dye Substances 0.000 description 125
- 241001062009 Indigofera Species 0.000 description 29
- 230000000052 comparative effect Effects 0.000 description 10
- 239000007788 liquid Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- COHYTHOBJLSHDF-BUHFOSPRSA-N indigo dye Chemical compound N\1C2=CC=CC=C2C(=O)C/1=C1/C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-BUHFOSPRSA-N 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 description 2
- 244000283207 Indigofera tinctoria Species 0.000 description 2
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000334160 Isatis Species 0.000 description 1
- 241000382362 Persicaria tinctoria Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- PZOUSPYUWWUPPK-UHFFFAOYSA-N indole Natural products CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 description 1
- RKJUIXBNRJVNHR-UHFFFAOYSA-N indolenine Natural products C1=CC=C2CC=NC2=C1 RKJUIXBNRJVNHR-UHFFFAOYSA-N 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 231100001081 no carcinogenicity Toxicity 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000000984 vat dye Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- D06P1/22—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 vat dyestuffs including indigo
- D06P1/228—Indigo
-
- 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
- D06P1/445—Use of auxiliary substances before, during or after dyeing or printing
-
- 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
- D06P1/64—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
- D06P1/65112—Compounds containing aldehyde or ketone groups
-
- 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
- D06P1/64—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
-
- 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
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
-
- 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
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
- D06P1/67358—Halides or oxyhalides
-
- 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
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/6025—Natural or regenerated cellulose using vat or sulfur dyes
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Coloring (AREA)
Abstract
The invention discloses a method for dyeing denim yarn by using natural indigo, which is characterized in that the denim cotton yarn is dyed by adopting a leuco body multi-padding oxidation method, dry vat reduction is carried out at 40-50 ℃, the natural indigo is 0.5-2 g/L, sodium hydroxide is 1.5-4.5 g/L, sodium hydrosulfite is 0.75-1.8 g/L, sodium hydrosulfite stabilizer is 0.25-0.6 g/L, accelerating agent sodium chloride or sodium sulfate is 10-15 g/L, and penetrating agent JFC2 g/L, the denim yarn is dyed according to the process of yarn pre-dyeing → oxidation → dyeing → oxidation → post-treatment.
Description
Technical Field
The invention belongs to the technical field of dyeing of fabrics, and particularly relates to a method for dyeing denim yarns by using natural indigo.
Background
The natural pigment is natural, has good compatibility with the environment, can be biodegraded, does not produce toxic substances, does not produce irritation to the skin, and has no carcinogenicity. Natural indigo is prepared by fermenting plant leaves containing indole acid components such as Polygonum tinctorium, Isatis tinctorium, Indigofera tinctoria, and Indigofera tinctoria, is a vat dye, is insoluble in water, and has no affinity to fiber. During dyeing, indigo is reduced into leuco body which can be dissolved in water, has affinity to fiber and can dye the fiber. Examples of the indigo reduction method include a fermentation method, a sodium hydrosulfite method, and a thiourea dioxide method. Among them, the fermentation method is the earliest to be applied, and has the advantages of simple equipment and low production cost; the method has the disadvantages that a large amount of complicated manual operation is needed, the reduction effect is slow, the leuco body can be formed usually in 7-10 days, the production efficiency is low, and continuous production cannot be realized. The thiourea dioxide method has poor stability and is easy to generate over reduction, so that the dye uptake is reduced. The sodium hydrosulfite method is high in reduction speed and simple to operate, but sodium hydrosulfite is poor in stability and violent in reaction when meeting water, a large amount of ineffective decomposition is generated, the sodium hydrosulfite stabilizer is a compound of various reducing agents, sulfur is not contained, the smell is not generated, and the ineffective decomposition of the sodium hydrosulfite can be effectively reduced.
The indigo leuco body has low affinity to cotton fibers and low dye-uptake, and the leuco body is promoted to be dyed by adopting a method for improving the concentration of a dye solution and the dyeing temperature, so that the problems of poor color brilliance, poor dyeing reproducibility, poor color fastness and the like can be caused. Therefore, the denim yarn is dyed by low-concentration normal-temperature dyeing through multiple dipping, rolling and oxidation methods.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for dyeing jean yarns by using natural indigo, which meets the requirements of people on environmental protection and body health.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for dyeing denim yarn by natural indigo adopts a leuco dye liquor to carry out padding oxidation for multiple times to dye denim cotton yarn, and comprises the following steps:
(1) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual rate is 60-65%;
(2) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 10-15 min at the temperature of 20-35 ℃, and then rolling by a padder;
(3) and (3) oxidation: carrying out air oxidation on the dyed jean yarn at the temperature of 20-35 ℃;
(4) repeating the operations (2) and (3) for 5 times;
(5) and (3) post-treatment: and (4) washing, squeezing and drying the oxidized yarn.
The leuco dye solution is prepared from, by weight, 0.5-2 g/L parts of natural indigo, 1.5-4.5 g/L parts of sodium hydroxide, 0.75-1.8 g/L parts of sodium hydrosulfite, 0.25-0.6 g/L parts of sodium hydrosulfite stabilizer, a penetrating agent JFC2 g/L parts of dye and 10-15 g/L parts of accelerating agent.
The sodium hydrosulfite stabilizer is prepared from the following components in parts by weight: 40-50% of glucose, 30-40% of sodium hypophosphite and the balance anthraquinone.
The accelerating agent is sodium chloride or sodium sulfate.
The preparation method of the leuco dye solution comprises the following steps:
a. pre-reduction of dye: putting natural indigo into a beaker, adding a small amount of alcohol and water, uniformly mixing, adding water, stirring to 1/3 of the total amount of leuco dye liquor, adding 2/3 of sodium hydroxide, uniformly stirring, adding 2/3 of sodium hydrosulfite and the total amount of sodium hydrosulfite stabilizer, and fully reducing the dye at 40-50 ℃ to obtain leuco mother liquor;
b. preparing a dye solution: and (b) adding the balance of water into the dyeing cup, adding the balance of sodium hydroxide and sodium hydrosulfite, fully stirring and dissolving, adding a penetrating agent JFC, a dyeing accelerant and the leuco body mother liquor prepared in the step a to reach the total amount of the leuco body dyeing liquor, and uniformly stirring to prepare the leuco body dyeing liquor.
In the step a, the concentration of natural indigo is 1.5-6 g/L (equivalent to the concentration of 0.5-2 g/L in the leuco dye solution), the concentration of sodium hydroxide is 3-9 g/L (equivalent to the concentration of 1-3 g/L in the leuco dye solution), the concentration of sodium hydrosulfite is 1.5-3.6 g/L (equivalent to the concentration of 0.5-1.2 g/L in the leuco dye solution), and the concentration of sodium hydrosulfite stabilizer is 0.75-1.8 g/L (equivalent to the concentration of 0.25-0.6 g/L in the leuco dye solution).
In the step b, when the leuco mother liquor is not added, the concentration of sodium hydroxide is 0.75-2.25 g/L (equivalent to the concentration of 0.5-1.5 g/L in the leuco dye liquor), the concentration of sodium hydrosulfite is 0.375-0.9 g/L (equivalent to the concentration of 0.25-0.6 g/L in the leuco dye liquor), the concentration of a penetrant JFC is 3 g/L (equivalent to the concentration of 2 g/L in the leuco dye liquor), and the concentration of a dyeing accelerant is 15-22.5 g/L (equivalent to the concentration of 10-15 g/L in the leuco dye liquor).
The rolling residual rate in the step (2) of the multiple padding oxidation method for the leuco body is 70% -75%.
And (3) the oxidation time of the leuco body in the step (3) of the multi-time pad-rolling oxidation method is 1.5-2 min.
The water washing temperature in the step (5) of the multiple-time pad-rolling oxidation method for the leuco body is 40-50 ℃, the leuco body is washed for 2-3 times, and the rolling residue rate is 60-65%.
The invention has the beneficial effects that: the dyeing method of soaking, rolling and oxidizing for multiple times can improve the color brightness and dyeing reproducibility of the jean yarn, the dyeing and oxidizing can be carried out under the room temperature condition, heating is not needed, energy is saved, environment is protected, the reduction speed is high, the dyeing effect is stable, the addition of the sodium hydrosulfite stabilizer obviously improves the utilization rate and the reduction capability of the sodium hydrosulfite, the ineffective decomposition of the sodium hydrosulfite is effectively reduced, the using amount of the sodium hydrosulfite can be reduced by 50% by adding a small amount of the sodium hydrosulfite stabilizer, and the dyeing effect which is nearly consistent with that of 100% of the sodium hydrosulfite when the sodium hydrosulfite stabilizer is not added is achieved. The dyeing method is characterized in that the water solution containing the penetrant is padded before dyeing to wet and swell the yarn, so that the dye can be favorably diffused into the fiber when the dye solution is dipped, the dyeing rate is improved, the accelerating agent is added into the dye solution to reduce the repulsive force between a leuco dye and the cellulose fiber, the dyeing rate is improved, the penetrant JFC is added into the dye solution, so that the dye solution can be favorably permeated into the denim yarn, the rubbing fastness is improved, soaping is not needed after the denim yarn is dyed, and the water consumption is greatly reduced. Before dyeing treatment, the penetrant and the accelerating agent in the dyeing solution act synergistically, so that the consumption of natural indigo is greatly reduced, and the effect of obtaining darker color by dyeing with dye with extremely low concentration is realized.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
The method for dyeing the jean yarn by using the natural indigo of the embodiment comprises the following steps:
(1) pre-reducing dye, namely putting natural indigo into a beaker, adding a small amount of alcohol and water, uniformly mixing, adding water, stirring to reach 1/3 of the total liquid amount, adding 3 g/L of sodium hydroxide (equivalent to the concentration of 1 g/L in the leuco dye solution), 1.5 g/L of sodium hydrosulfite (equivalent to the concentration of 0.5 g/L in the leuco dye solution), 0.75 g/L of sodium hydrosulfite stabilizer (equivalent to the concentration of 0.25 g/L in the leuco dye solution), and fully reducing the dye at 40 ℃ to prepare the leuco mother liquor, wherein the sodium hydrosulfite stabilizer is prepared from the following components in parts by weight, namely 40% of glucose, 30% of sodium hypophosphite and the balance anthraquinone;
(2) the dye liquor is prepared by adding the balance of water into a dye cup, adding 0.75 g/L of sodium hydroxide (equivalent to the concentration of 0.5 g/L in the leuco dye liquor), 0.375 g/L of sodium hydrosulfite (equivalent to the concentration of 0.25 g/L in the leuco dye liquor), fully stirring and dissolving, adding a penetrant JFC 3 g/L (equivalent to the concentration of 2 g/L in the leuco dye liquor), a dyeing accelerant sodium chloride 15 g/L (equivalent to the concentration of 10 g/L in the leuco dye liquor) and the leuco mother liquor, and uniformly stirring to obtain the leuco dye liquor;
(3) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual rate is 60%;
(4) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 10min at the temperature of 20 ℃, and then rolling by a padder, wherein the rolling residual rate is 70%;
(5) and (3) oxidation: carrying out air oxidation on the dyed jean yarn for 2min at the temperature of 20 ℃;
(6) repeating the operations (4) and (5) for 5 times;
(7) and (3) post-treatment: and washing the oxidized yarn for 2 times at 40 ℃ with 60% of rolling residue, and drying.
Example 2
The method for dyeing the jean yarn by using the natural indigo of the embodiment comprises the following steps:
(1) the dye is pre-reduced, namely, natural indigo is put into a beaker, a small amount of alcohol and water are added for mixing uniformly, then water is added for stirring to reach 1/3 of the total liquid amount, at the moment, the concentration of the natural indigo is 6 g/L (equivalent to the concentration in a leuco dye solution is 2 g/L), 9 g/L of sodium hydroxide (equivalent to the concentration in the leuco dye solution is 3 g/L), 3.6 g/L of sodium hydrosulfite (equivalent to the concentration in the leuco dye solution is 1.2 g/L), 1.8 g/L of sodium hydrosulfite stabilizer (equivalent to the concentration in the leuco dye solution is 0.6 g/L) are added, and the dye is fully reduced at the temperature of 50 ℃ to prepare leuco dye mother liquor, wherein the sodium hydrosulfite stabilizer is prepared from the following components in weight ratio of 50 percent of glucose, 40 percent of sodium hypophosphite and the balance of anthraquinone;
(2) the dye liquor is prepared by adding the balance of water into a dye cup, adding 2.25 g/L of sodium hydroxide (equivalent to the concentration of 1.5 g/L in the leuco dye liquor), 0.9 g/L of sodium hydrosulfite (equivalent to the concentration of 0.6 g/L in the leuco dye liquor), fully stirring and dissolving, adding a penetrant JFC 3 g/L (equivalent to the concentration of 2 g/L in the leuco dye liquor), a dyeing accelerant sodium sulfate 22.5 g/L (equivalent to the concentration of 15 g/L in the leuco dye liquor) and the leuco mother liquor, and uniformly stirring to obtain the leuco dye liquor;
(3) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual rate is 65%;
(4) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 15min at 35 ℃, and then rolling by a padder, wherein the rolling residual rate is 75%;
(5) and (3) oxidation: carrying out air oxidation on the dyed jean yarn for 1.5min at the temperature of 35 ℃;
(6) repeating the operations (4) and (5) for 5 times;
(7) and (3) post-treatment: and washing the oxidized yarn for 3 times at 50 ℃ with 65% of rolling residue, and drying.
Example 3
The method for dyeing the jean yarn by using the natural indigo of the embodiment comprises the following steps:
(1) pre-reducing dye, namely putting natural indigo into a beaker, adding a small amount of alcohol and water, uniformly mixing, adding water, stirring to reach 1/3 of the total liquid amount, adding 6 g/L of sodium hydroxide (equivalent to the concentration of 2 g/L in the leuco dye solution), 2.4 g/L of sodium hydrosulfite (equivalent to the concentration of 0.8 g/L in the leuco dye solution) and 1.2 g/L of sodium hydrosulfite stabilizer (equivalent to the concentration of 0.4 g/L in the leuco dye solution), and fully reducing the dye at 45 ℃ to prepare leuco mother liquor, wherein the sodium hydrosulfite stabilizer is prepared from the following components in parts by weight, namely 40% of glucose, 40% of sodium hypophosphite and the balance of anthraquinone;
(2) the dye liquor is prepared by adding the balance of water into a dye cup, adding 1.5 g/L of sodium hydroxide (equivalent to the concentration of 1 g/L in the leuco dye liquor), 0.6 g/L of sodium hydrosulfite (equivalent to the concentration of 0.4 g/L in the leuco dye liquor), fully stirring and dissolving, adding a penetrant JFC 3 g/L (equivalent to the concentration of 2 g/L in the leuco dye liquor), a dyeing accelerant sodium chloride 19.5 g/L (equivalent to the concentration of 13 g/L in the leuco dye liquor) and the leuco mother liquor, and uniformly stirring to obtain the leuco dye liquor;
(3) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual ratio is 63 percent;
(4) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 13min at the temperature of 30 ℃, and then rolling by a padder, wherein the rolling residual rate is 73%;
(5) and (3) oxidation: carrying out air oxidation on the dyed jean yarn for 1.8min at the temperature of 30 ℃;
(6) repeating the operations (4) and (5) for 5 times;
(7) and (3) post-treatment: and washing the oxidized yarn for 2 times at 45 ℃ with water, wherein the rolling residue rate is 63%, and then drying.
Example 4
The method for dyeing the jean yarn by using the natural indigo of the embodiment comprises the following steps:
(1) the dye is pre-reduced, namely, natural indigo is put into a beaker, a small amount of alcohol and water are added for mixing evenly, then water is added for stirring to reach 1/3 of the total liquid amount, at the moment, the concentration of the natural indigo is 2.7 g/L (equivalent to the concentration in the leuco dye liquor being 0.9 g/L), sodium hydroxide is added for 4.8 g/L (equivalent to the concentration in the leuco dye liquor being 1.6 g/L), sodium hydrosulfite is added for 1.8 g/L (equivalent to the concentration in the leuco dye liquor being 0.6 g/L), and sodium hydrosulfite stabilizer is added for 0.9 g/L (equivalent to the concentration in the leuco dye liquor being 0.3 g/L), the dye is fully reduced at the temperature of 42 ℃, so as to prepare leuco dye mother liquor, wherein the sodium hydrosulfite stabilizer is prepared from the following components by weight ratio, namely 45% of glucose, 35% of sodium hypophosphite and the balance anthraquinone;
(2) the dye liquor is prepared by adding the balance of water into a dye cup, adding 1.2 g/L of sodium hydroxide (equivalent to the concentration of 0.8 g/L in the leuco dye liquor), 0.45 g/L of sodium hydrosulfite (equivalent to the concentration of 0.3 g/L in the leuco dye liquor), fully stirring and dissolving, adding a penetrant JFC 3 g/L (equivalent to the concentration of 2 g/L in the leuco dye liquor), an accelerating agent sodium sulfate 18 g/L (equivalent to the concentration of 12 g/L in the leuco dye liquor) and the leuco mother liquor, and uniformly stirring to obtain the leuco dye liquor;
(3) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual rate is 62%;
(4) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 12min at 25 ℃, and then rolling by a padder, wherein the rolling residual rate is 72%;
(5) and (3) oxidation: carrying out air oxidation on the dyed jean yarn for 1.5min at the temperature of 25 ℃;
(6) repeating the operations (4) and (5) for 5 times;
(7) and (3) post-treatment: the oxidized yarn is washed for 3 times at the temperature of 43 ℃, the rolling residual rate is 62 percent, and then the yarn is dried.
Example 5
The method for dyeing the jean yarn by using the natural indigo of the embodiment comprises the following steps:
(1) pre-reducing dye, namely putting natural indigo into a beaker, adding a small amount of alcohol and water, uniformly mixing, adding water, stirring to reach 1/3 of the total liquid amount, adding 7.2 g/L of sodium hydroxide (equivalent to the concentration of 2.4 g/L in the leuco dye solution), 3 g/L of sodium hydrosulfite (equivalent to the concentration of 1 g/L in the leuco dye solution), 1.5 g/L of sodium hydrosulfite stabilizer (equivalent to the concentration of 0.5 g/L in the leuco dye solution), and fully reducing the dye at 48 ℃ to prepare the leuco mother liquor, wherein the sodium hydrosulfite stabilizer is prepared from the following components in parts by weight, namely 50% of glucose, 30% of sodium hypophosphite and the balance anthraquinone;
(2) the dye liquor is prepared by adding the balance of water into a dye cup, adding 1.8 g/L of sodium hydroxide (equivalent to the concentration of 1.2 g/L in the leuco dye liquor), 0.75 g/L of sodium hydrosulfite (equivalent to the concentration of 0.5 g/L in the leuco dye liquor), fully stirring and dissolving, adding a penetrant JFC 3 g/L (equivalent to the concentration of 2 g/L in the leuco dye liquor), a dyeing accelerant sodium sulfate 21 g/L (equivalent to the concentration of 14 g/L in the leuco dye liquor) and the leuco mother liquor, and uniformly stirring to obtain the leuco dye liquor;
(3) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual rate is 65%;
(4) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 14min at 32 ℃, and then rolling by a padder, wherein the rolling residual rate is 74%;
(5) and (3) oxidation: carrying out air oxidation on the dyed jean yarn for 1.5min at the temperature of 32 ℃;
(6) repeating the operations (4) and (5) for 5 times;
(7) and (3) post-treatment: and washing the oxidized yarn for 2 times at 48 ℃ with 65% of rolling residue, and drying.
Measurement of apparent color depth K/S value of fabric: each sample was measured 4 times using a CE-7000A SCT high precision colorimeter using a D65 illuminant and a 10 ℃ observation angle, and averaged.
Color fastness to rubbing: the test is carried out according to GB/T3920-2008 ' color fastness to rubbing ' of textile color fastness test '.
Fastness to soaping: the test is carried out according to GB/T3921-2008 'soaping color fastness resistance of textile color fastness test'.
Color fastness to perspiration: the test is carried out according to GB/T3922-.
Color fastness to light: reference GB/T8427-: xenon arc "for testing.
TABLE 1K/S value and color fastness of denim yarn dyed according to example 3
TABLE 2K/S value and color fastness of denim yarn dyed according to example 4
The color fastness of the dyed denim yarn measured in tables 1 to 2 can meet the requirement of the denim fabric.
Comparative example 1
The method for dyeing the jean yarn by using natural indigo according to the formula of the example 4 and without adding the sodium hydrosulfite stabilizer and with 2 times of the sodium hydrosulfite amount comprises the following steps:
(1) pre-reducing the dye, namely putting the natural indigo dye into a beaker, adding a small amount of alcohol and water for mixing uniformly, then adding water, stirring to obtain 1/3 of the total liquid amount, wherein the concentration of the natural indigo dye is 2.7 g/L (equivalent to the concentration in the leuco dye solution is 0.9 g/L), adding 4.8 g/L of sodium hydroxide (equivalent to the concentration in the leuco dye solution is 1.6 g/L) and 3.6 g/L of sodium hydrosulfite (equivalent to the concentration in the leuco dye solution is 1.2 g/L), and fully reducing the dye at 42 ℃ to obtain leuco mother liquor;
(2) the dye liquor is prepared by adding the balance of water into a dye cup, adding 1.2 g/L of sodium hydroxide (equivalent to the concentration of 0.8 g/L in the leuco dye liquor), 0.9 g/L of sodium hydrosulfite (equivalent to the concentration of 0.6 g/L in the leuco dye liquor), fully stirring and dissolving, adding a penetrant JFC 3 g/L (equivalent to the concentration of 2 g/L in the leuco dye liquor), an accelerating agent sodium sulfate 18 g/L (equivalent to the concentration of 12 g/L in the leuco dye liquor) and the leuco mother liquor, and uniformly stirring to obtain the leuco dye liquor;
(3) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual rate is 62%;
(4) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 12min at 25 ℃, and then rolling by a padder, wherein the rolling residual rate is 72%;
(5) and (3) oxidation: carrying out air oxidation on the dyed jean yarn for 1.5min at the temperature of 25 ℃;
(6) repeating the operations (4) and (5) for 5 times;
(7) and (3) post-treatment: the oxidized yarn is washed for 3 times at the temperature of 43 ℃, the rolling residual rate is 62 percent, and then the yarn is dried.
TABLE 1 attached K/S value and color fastness of denim yarn dyed according to comparative example 1
As can be seen from the attached table 1, the amount of the sodium hydrosulfite is increased by 1 time, the sodium hydrosulfite stabilizer is not added, and compared with the sodium hydrosulfite stabilizer (the amount of the sodium hydrosulfite is not increased), the K/S value of the denim yarn obtained by dyeing is very close and the color fastness is consistent. The sodium hydrosulfite stabilizer has the effects of effectively improving the utilization rate and the reducing capability of the sodium hydrosulfite and reducing the ineffective decomposition of the sodium hydrosulfite, so that the using amount of the sodium hydrosulfite is obviously reduced.
Comparative example 2
The method for dyeing the jean yarn by using natural indigo according to the formula of the example 4 and adopting glucose as the sodium hydrosulfite stabilizer comprises the following steps:
(1) pre-reducing dye, namely putting natural indigo into a beaker, adding a small amount of alcohol and water for mixing uniformly, then adding water, stirring to obtain 1/3 of the total liquid amount, wherein the concentration of the natural indigo is 2.7 g/L (equivalent to the concentration of 0.9 g/L in the leuco dye solution), adding 4.8 g/L of sodium hydroxide (equivalent to the concentration of 1.6 g/L in the leuco dye solution), 1.8 g/L of sodium hydrosulfite (equivalent to the concentration of 0.6 g/L in the leuco dye solution), 0.9 g/L of sodium hydrosulfite stabilizer with a single reducing component (equivalent to the concentration of 0.3 g/L in the leuco dye solution), and fully reducing the dye at 42 ℃ to prepare leuco mother liquid;
(2) the dye liquor is prepared by adding the balance of water into a dye cup, adding 1.2 g/L of sodium hydroxide (equivalent to the concentration of 0.8 g/L in the leuco dye liquor), 0.45 g/L of sodium hydrosulfite (equivalent to the concentration of 0.3 g/L in the leuco dye liquor), fully stirring and dissolving, adding a penetrant JFC 3 g/L (equivalent to the concentration of 2 g/L in the leuco dye liquor), an accelerating agent sodium sulfate 18 g/L (equivalent to the concentration of 12 g/L in the leuco dye liquor) and the leuco mother liquor, and uniformly stirring to obtain the leuco dye liquor;
(3) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual rate is 62%;
(4) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 12min at 25 ℃, and then rolling by a padder, wherein the rolling residual rate is 72%;
(5) and (3) oxidation: carrying out air oxidation on the dyed jean yarn for 1.5min at the temperature of 25 ℃;
(6) repeating the operations (4) and (5) for 5 times;
(7) and (3) post-treatment: the oxidized yarn is washed for 3 times at the temperature of 43 ℃, the rolling residual rate is 62 percent, and then the yarn is dried.
TABLE 2 attached K/S value and color fastness of denim yarn dyed according to comparative example 2
Comparative example 3
The formula of example 4 was followed, the sodium hypophosphite stabilizer was used in its entirety, and the dyed denim yarn had a K/S value of 4.8.
Comparative example 4
The formula of example 4 was followed, the all-in-one anthraquinone used as the sodium hydrosulfite stabilizer, and the K/S value of the dyed denim yarn was 5.4.
Comparative example 5
The formula of example 4 was followed, the all sodium hydrosulfite stabilizer used glucose and sodium hypophosphite, and the dyed denim yarn had a K/S value of 6.9.
Comparative example 6
The formula of example 4 was followed, the all-purpose sodium hydrosulfite stabilizer being glucose and anthraquinone, and the dyed denim yarn had a K/S value of 7.1.
Comparative example 7
The formula of example 4 was followed, the sodium hypophosphite stabilizer was used in total with anthraquinone, and the dyed denim yarn had a K/S value of 6.5.
From the dyeing results of comparative examples 2-7, it can be seen that when the sodium hydrosulfite stabilizer is replaced by one or two reducing agent components, the K/S value of the dyed denim yarn is reduced, and the dyed yarn has lighter color. The three reducing agents in the sodium hydrosulfite stabilizer can act synergistically, so that the utilization rate and the reducing capacity of the sodium hydrosulfite are effectively improved, the ineffective decomposition of the sodium hydrosulfite is reduced, and after one or two components are replaced, the synergistic effect of the reducing components cannot be fully exerted, so that the natural indigo is insufficiently reduced, the utilization rate of the dye is reduced, and the dyed yarn is light in color.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A method for dyeing jean yarns by using natural indigo is characterized by comprising the following steps: dyeing the denim cotton yarn by adopting a leuco dye liquor multiple padding oxidation method, comprising the following steps:
(1) the yarn dyeing pretreatment, namely padding with an aqueous solution containing a penetrating agent JFC2 g/L, wherein the rolling residual rate is 60-65%;
(2) dyeing: putting the denim yarn subjected to dyeing pretreatment into a leuco dye solution, soaking for 10-15 min at the temperature of 20-35 ℃, and then rolling by a padder;
(3) and (3) oxidation: carrying out air oxidation on the dyed jean yarn at the temperature of 20-35 ℃;
(4) repeating the operations (2) and (3) for 5 times;
(5) and (3) post-treatment: washing, squeezing and drying the oxidized yarn;
the leuco dye solution comprises, by weight, 0.5-2 g/L parts of natural indigo, 1.5-4.5 g/L parts of sodium hydroxide, 0.75-1.8 g/L parts of sodium hydrosulfite, 0.25-0.6 g/L parts of sodium hydrosulfite stabilizer, 40-50 parts of glucose, 30-40 parts of sodium hypophosphite and the balance anthraquinone, wherein the sodium hydrosulfite stabilizer is a penetrant JFC2 g/L and 10-15 g/L parts of accelerating agent.
2. The method of dyeing denim yarn with natural indigo according to claim 1, characterized in that: the accelerating agent is sodium chloride or sodium sulfate.
3. The method for dyeing denim yarn with natural indigo according to claim 1 or 2, characterized in that: the preparation method of the leuco dye solution comprises the following steps:
a. pre-reduction of dye: putting natural indigo into a beaker, adding a small amount of alcohol and water, uniformly mixing, adding water, stirring to 1/3 of the total amount of leuco dye liquor, adding 2/3 of sodium hydroxide, uniformly stirring, adding 2/3 of sodium hydrosulfite and the total amount of sodium hydrosulfite stabilizer, and fully reducing the dye at 40-50 ℃ to obtain leuco mother liquor;
b. preparing a dye solution: and (b) adding the balance of water into the dyeing cup, adding the balance of sodium hydroxide and sodium hydrosulfite, fully stirring and dissolving, adding a penetrating agent JFC, a dyeing accelerant and the leuco body mother liquor prepared in the step a to reach the total amount of the leuco body dyeing liquor, and uniformly stirring to prepare the leuco body dyeing liquor.
4. The method for dyeing the jean yarn by using the natural indigo according to claim 3, wherein the concentration of the natural indigo in the step a is 1.5-6 g/L, the concentration of sodium hydroxide is 3-9 g/L, the concentration of sodium hydrosulfite is 1.5-3.6 g/L, and the concentration of sodium hydrosulfite stabilizer is 0.75-1.8 g/L.
5. The method for dyeing the denim yarn with the natural indigo according to claim 3, wherein the concentration of sodium hydroxide is 0.75-2.25 g/L, the concentration of sodium hydrosulfite is 0.375-0.9 g/L, the concentration of penetrant JFC is 3 g/L, and the concentration of accelerant is 15-22.5 g/L when leuco mother liquor is not added in the step b.
6. The method of dyeing denim yarn with natural indigo according to claim 1, characterized in that: the rolling residual rate in the step (2) of the leuco dye liquor multiple padding oxidation method is 70-75%.
7. The method of dyeing denim yarn with natural indigo according to claim 1, characterized in that: and (3) carrying out multiple padding oxidation on the leuco dye liquor for 1.5-2 min.
8. The method of dyeing denim yarn with natural indigo according to claim 1, characterized in that: the water washing temperature in the step (5) of the multiple padding oxidation method of the leuco dye liquor is 40-50 ℃, the leuco dye liquor is washed for 2-3 times, and the rolling residue rate is 60-65%.
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| CN110016816A (en) * | 2019-03-13 | 2019-07-16 | 广东前进牛仔布有限公司 | A kind of indigo dyeing method |
| CN110130122B (en) * | 2019-06-14 | 2024-06-28 | 佛山市南海亿棉染织有限公司 | Water-saving dyeing method and device for sulfur dye |
| CN111395013B (en) * | 2020-06-02 | 2020-10-27 | 佛山市南海区今易德纺织有限公司 | Rapid dyeing process of denim fabric |
| CN114086405B (en) * | 2021-12-22 | 2024-02-13 | 中纺院（浙江）技术研究院有限公司 | Biological reducing agent and method for applying biological reducing agent to plant indigo dyed yarns |
| CN114481651B (en) * | 2021-12-31 | 2024-02-02 | 中山市鸿盛生物科技有限公司 | Alkali-resistant penetrating agent and application thereof in sizing |
| CN115538191B (en) * | 2022-09-21 | 2023-12-29 | 南通东屹高新纤维科技有限公司 | Dyeing method of degradable yarn |
| CN116556082B (en) * | 2023-05-22 | 2024-07-02 | 佛山纳纤科技有限公司 | Anhydrous supercritical dyed jean textile and process thereof |
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