CN114086405B - Biological reducing agent and method for applying biological reducing agent to plant indigo dyed yarns - Google Patents
Biological reducing agent and method for applying biological reducing agent to plant indigo dyed yarns Download PDFInfo
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- CN114086405B CN114086405B CN202111577530.9A CN202111577530A CN114086405B CN 114086405 B CN114086405 B CN 114086405B CN 202111577530 A CN202111577530 A CN 202111577530A CN 114086405 B CN114086405 B CN 114086405B
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000004043 dyeing Methods 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- -1 saccharide compound Chemical class 0.000 claims abstract description 25
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 150000007524 organic acids Chemical class 0.000 claims abstract description 8
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 claims description 53
- 238000005406 washing Methods 0.000 claims description 29
- 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 claims description 26
- 241001122767 Theaceae Species 0.000 claims description 25
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 25
- 229930182490 saponin Natural products 0.000 claims description 25
- 150000007949 saponins Chemical class 0.000 claims description 25
- 235000000177 Indigofera tinctoria Nutrition 0.000 claims description 24
- 229940097275 indigo Drugs 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 241000196324 Embryophyta Species 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical group [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 238000004804 winding Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000001502 supplementing effect Effects 0.000 claims description 8
- 235000013311 vegetables Nutrition 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 239000008103 glucose Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 230000002441 reversible effect Effects 0.000 claims description 6
- 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 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- MLIWQXBKMZNZNF-KUHOPJCQSA-N (2e)-2,6-bis[(4-azidophenyl)methylidene]-4-methylcyclohexan-1-one Chemical compound O=C1\C(=C\C=2C=CC(=CC=2)N=[N+]=[N-])CC(C)CC1=CC1=CC=C(N=[N+]=[N-])C=C1 MLIWQXBKMZNZNF-KUHOPJCQSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 229920001661 Chitosan Polymers 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- MUPFEKGTMRGPLJ-RMMQSMQOSA-N Raffinose Natural products O(C[C@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@@H](O[C@@]2(CO)[C@H](O)[C@@H](O)[C@@H](CO)O2)O1)[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 MUPFEKGTMRGPLJ-RMMQSMQOSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- MUPFEKGTMRGPLJ-UHFFFAOYSA-N UNPD196149 Natural products OC1C(O)C(CO)OC1(CO)OC1C(O)C(O)C(O)C(COC2C(C(O)C(O)C(CO)O2)O)O1 MUPFEKGTMRGPLJ-UHFFFAOYSA-N 0.000 claims 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 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 230000002045 lasting effect Effects 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- MUPFEKGTMRGPLJ-ZQSKZDJDSA-N raffinose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO[C@@H]2[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO)O2)O)O1 MUPFEKGTMRGPLJ-ZQSKZDJDSA-N 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims 1
- 235000005985 organic acids Nutrition 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 63
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 229920000742 Cotton Polymers 0.000 description 16
- 238000007254 oxidation reaction Methods 0.000 description 16
- 230000003647 oxidation Effects 0.000 description 15
- 239000004744 fabric Substances 0.000 description 11
- 239000000835 fiber Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 239000003518 caustics Substances 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- JMEVHYCNAPFOAB-UHFFFAOYSA-N 2-(3-hydroxy-5-sulfo-1H-indol-2-yl)-3-oxoindole-5-sulfonic acid Chemical compound Oc1c([nH]c2ccc(cc12)S(O)(=O)=O)C1=Nc2ccc(cc2C1=O)S(O)(=O)=O JMEVHYCNAPFOAB-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- 229920003043 Cellulose fiber Polymers 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009972 garment dyeing Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000004627 regenerated cellulose Substances 0.000 description 2
- 238000007447 staining method Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000000984 vat dye Substances 0.000 description 2
- 238000009970 yarn dyeing Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- QQILFGKZUJYXGS-UHFFFAOYSA-N Indigo dye Chemical compound C1=CC=C2C(=O)C(C3=C(C4=CC=CC=C4N3)O)=NC2=C1 QQILFGKZUJYXGS-UHFFFAOYSA-N 0.000 description 1
- 241000334160 Isatis Species 0.000 description 1
- 229930182559 Natural dye Natural products 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
- 244000152045 Themeda triandra Species 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 150000001719 carbohydrate derivatives Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- QTWZICCBKBYHDM-UHFFFAOYSA-N leucomethylene blue Chemical compound C1=C(N(C)C)C=C2SC3=CC(N(C)C)=CC=C3NC2=C1 QTWZICCBKBYHDM-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000000978 natural dye Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000011909 oxidative ring-opening Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 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
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Coloring (AREA)
Abstract
The application provides a biological reducing agent and a method for applying the biological reducing agent to plant indigo dyed yarns, and belongs to the technical field of dyeing and finishing engineering. Comprises the following components: 30-40% of saccharide compound, 1-6% of inorganic oxide, 2-5% of organic acid, 3-8% of alcohol compound and the balance of deionized water. The reducer can be applied to processing of plant indigo dyed yarns, and has the advantages of strong environmental protection, high stability and the like.
Description
Technical Field
The application relates to a biological reducing agent and a method for applying the biological reducing agent to plant indigo dyed yarns, and belongs to the technical field of dyeing and finishing engineering.
Background
As a dye from blue grass plants such as bluish, polygonum tinctorium, isatis tinctorium, etc., the plant indigo dye is obviously different from the industrial synthetic indigo dye, and the obvious difference is not only in production and preparation, but also in dyeing mode, dyeing effect and functionality. As the only one blue vat dye in a plurality of natural dyes, the dyeing process is more complicated than the conventional dye dyeing process, and mainly three processes are carried out: dye reduction, leuco dye-uptake, leuco oxidation. The key to the quality of indigo dyeing is whether the indigo dye is sufficiently reduced to the leuco form. For this reason, the indigo reduction method is mainly caustic soda-sodium hydrosulfite reduction, caustic soda-glucose reduction and electrochemical reduction at present, and the different methods have advantages and disadvantages.
(1) Caustic soda-sodium hydrosulfite reduction method: the method is the most common dyeing method of vat dye, and the principle is as follows: the vat powder can dissociate the reducibility [ H ] under alkaline condition, the reducibility [ H ] and insoluble indigo react to generate soluble leuco bodies, and then the soluble leuco bodies and fibers are adsorbed and dyed.
But the defects are that: (1) the inorganic salt and the sulfur-containing compound are generated in the acid washing and neutralization processes of a large amount of caustic soda and sodium hydrosulfite used in the reduction process, so that the difficulty of sewage treatment is increased; (2) the caustic soda-sodium hydrosulfite reduction system solution is too alkaline, and can cause irreversible damage to fibers, especially silk fabrics.
(2) Caustic soda-glucose reduction method: the method is characterized in that glucose undergoes an oxidative ring-opening reaction in a caustic soda solution system to generate carboxyl with the end having reducing capability, so that the method can be used for reducing indigo dye. Because glucose is mainly in a closed-loop structure and is assisted by a small amount of open-loop structure in the solution, a large amount of glucose is needed to be added in the reduction process to ensure the full reduction of the indigo dye.
In addition, the biological reduction staining method and the electrochemical reduction staining method have unstable factors such as overlong reduction time and unstable reduction effect, so that the methods cannot realize industrialization.
CN110158329 a discloses a large-scale production method of indigo dye for garment dyeing, which improves garment dyeing device, and adds nitrogen charging device, during dyeing, nitrogen is charged in the device, and air is discharged, so as to prevent excessive oxidation of indigo by air.
CN111270534 a discloses a method for dyeing high-quality bulk fiber plant indigo, which adopts a centrifugal separation method to remove impurities in plant indigo solution, and takes supernatant for dyeing fiber, and the obtained indigo dyed fiber has clean surface, no impurities and high color fastness.
CN112252054 a discloses a method for dyeing pure cotton yarn on line by using vegetable dye, which comprises the steps of winding the pure cotton yarn into loose type cone yarn, dyeing with vegetable dye liquor, and performing yarn steaming fixation and water washing treatment to realize on-line dyeing of the pure cotton yarn by using vegetable dye. The plant dye liquor is added with penetrating agent and ethanol to promote dye to enter the interior of the cone yarn more fully, so that the purpose of full dyeing is achieved.
The patent or the equipment is modified, a nitrogen charging device is added, and nitrogen is used for replacing air, so that excessive oxidation of air to indigo in the dyeing process is avoided; or separating impurities in the indigo stock solution in advance, and using the supernatant for dyeing fabrics; or the space for the indigo dye liquor to enter the cone yarn is enlarged by using a penetrating agent or ethanol or a cone winding mode, the problems of the plant indigo dyeing fabric or yarn are solved only at a single angle, and the core problem of the plant indigo dyeing is not related.
Disclosure of Invention
In view of the above, the present application provides a bioreductive agent, starting from the preparation of the bioreductive agent, using environmentally friendly and low-cost saccharides as raw materials, using inorganic compound sodium periodate or potassium periodate as an oxidant, to prepare a solution for reduction of plant indigo, replacing the traditional and serious-hazard sodium hydrosulfite, realizing the greenization of the plant indigo dyeing process, and realizing indigo dyeing of regenerated cellulose fiber yarns.
Specifically, the application is realized through the following scheme:
a bioreductive agent comprising the following components: 30-40% of saccharide compound, 1-6% of inorganic oxide, 2-5% of organic acid, 3-8% of alcohol compound and the balance of deionized water.
Under the action of organic acid and high temperature, the saccharide compound is converted into plastic fluid from insoluble and water state for reduction of indigo dye, and the saccharide compound with high stability and low cost is used as material and inorganic oxide is used in catalytic decomposition to produce compound with powerful reducing capacity.
Further, as preferable:
the saccharide compound is one or more of raffinose, glucose, chitosan and the like.
The organic acid is any one or a mixture of more of acetic acid, citric acid, tartaric acid and the like.
The alcohol compound is any one or a mixture of more of ethanol, glycol and propanol, and has the main function of promoting the dissolution of saccharide derivatives formed by the reaction in the biological reducing agent; secondly, the solution is maintained in a slightly alkaline environment, so that the substance has a relatively stable state. The addition amount of the alcohol compound is preferably 5 to 6%.
The inorganic oxide is sodium periodate or potassium periodate, and is subjected to oxidation reaction with hydroxyl on the saccharide macromolecular cyclic structure to form a plurality of aldehyde groups with reducibility, so that the reducing capability of saccharide compounds is greatly enhanced. The addition amount of the inorganic oxide is preferably 2 to 5%.
The preparation process of the biological reducing agent comprises the following steps:
(1) Uniformly stirring the saccharide compound with deionized water and organic acid to prepare colloidal liquid;
(2) Adding inorganic oxide into the step (1), uniformly mixing, and reacting at 45-55 ℃ for later use;
(3) Adding alcohol compound according to a certain proportion, continuously stirring and uniformly mixing.
Meanwhile, the application also develops a dyeing method suitable for dyeing regenerated cellulose fiber yarns by using plant indigo, and the dyeing method provides solving paths from multiple angles and multiple layers, establishes a method for dyeing cellulose yarns by using the whole-flow plant indigo, and realizes the application of the biological reducer to the plant indigo dyed yarns.
A method for applying biological reducer to plant indigo dyed yarn comprises the following steps:
(1) Plant indigo dye pre-reduction: fully mixing the biological reducing agent with plant indigo at a concentration of 5-20g/L, adjusting the pH value (preferably adjusting the pH value of the dye liquor by using tea saponin) to 11-12, and measuring and reducing the potential to be more than-800-750 mv to obtain the plant indigo dye liquor; the pH and the reduction potential of the dye bath are respectively adjusted to be more than 11-12 and-800 to-750 mv during dyeing, and the main reasons are that the pH is lower than the interval, the conversion of insoluble indigo to soluble indigo leuco can be influenced, and the too low reduction potential of the dye liquor directly influences the reduction force of the dye liquor, thereby influencing the dyeing of the fiber by the dye.
(2) And (3) dyeing: placing the cone yarn to be treated in a dye vat, adding clear water in a bath ratio of 1:10-20, adding 1-3g/L of tea saponin and 2-5g/L of the biological reducing agent, heating to 20-45 ℃ at 1-3 ℃/min, preserving heat for 20-90min, adding the plant indigo dye liquor in the step (1) in batches for multiple times, supplementing 1-3g/L of tea saponin and 1-3g/L of the biological reducing agent every 10-20min, wherein the proportion of the plant indigo dye liquor added each time is 10-20%, adding for 5-10 times, the pressure of a dye vat cylinder body is 3-5MPa, the power of a main pump is 80-100%, the forward circulation time of the dye liquor is 1-4min, and the reverse circulation time is 3-10min;
(3) Oxidizing: fully discharging dye liquor, pressurizing and introducing air into the cylinder body, wherein the pressurizing interval time is 1-2min, each time lasting time is 8-10min, and cleaning and drying by adding clear water at a ratio of 1:15-25.
Further, as preferable:
since the hydrophobic waxy substances and naturally deposited pigments present on cotton yarn affect the dyeing of vegetable dyes, the cotton yarn is pretreated with the natural alkaline substance tea saponin. Therefore, the cone yarn before dyeing is pretreated: moistening the cone yarn, adding tea saponin, dissolving, increasing the temperature to 60-85 ℃ at 1-3 ℃/min for 10-25min, increasing the temperature to 85-98 ℃ at 1-2 ℃/min for 30-60min, washing with water, pickling, washing with water, and taking out to obtain the cone yarn to be treated. More preferably, the cone yarn pretreatment process is as follows: moistening the cone yarn, dissolving 8-10g/L of tea saponin, introducing the dissolved tea saponin into a cylinder, heating to 80 ℃ at 1-2 ℃/min, preserving heat for 15min, heating to 95 ℃ at 2 ℃/min, preserving heat for 30-60min, washing with clear water, washing with hot water, washing with acid, washing with clear water, and taking out for later use.
The cone yarn is wound by a loose winding machine, so that the cone yarn is fluffy, a large enough space is formed between the yarns, and the dye liquor can flow through the cone yarn fully.
In the step (2), the pressure of the dye vat cylinder body is set to be 3.9-4.0MPa, the power of the main pump is 90-100%, the forward circulation time of the dye liquor is 1-2min, and the reverse circulation time of the dye liquor is 4-6min.
During dyeing, firstly, fully reducing plant indigo dye liquor into a leuco state, and measuring the reduction potential and the pH value of the dye liquor to ensure that the dye liquor is stably kept in a certain range; secondly, adjusting the internal and external circulation time and the pressure of the dye liquor flowing through the cone yarn, so that the dye liquor can fully permeate into the yarn cone, and the difference between the inner layer and the outer layer is reduced; the bath ratio of the dye liquor is improved, the dye liquor is kept to be fully filled in the cylinder body, and excessive oxidation of the indigo dye liquor caused by air brought in by pressurization is reduced; finally, reducing agent (CRT) and tea saponin are added for a plurality of times, so that the dye liquor is always kept in a soluble reduction state, and the excessive adsorption of insoluble indigo on the fiber surface is reduced.
In the step (3), after the dye liquor in the cylinder is fully discharged, the outside air is introduced into the cylinder body in a pressurizing mode, a large amount of air is introduced during pressurizing to oxidize indigo, and air and water remained in the cone yarn are taken away during discharging, wherein the interval is 1-2min, and the period lasts for 8-10min.
In the application, the process flow of the plant indigo yarn dyeing process mainly comprises the following steps: plant indigo dye liquor prereduction-cotton yarn loose winding-cotton yarn cone yarn pretreatment (removing hydrophobic wax and naturally deposited pigment existing on the surface of the fiber, improving the hydrophilicity of the cotton yarn), dyeing (dyeing cotton yarn by a soluble indigo leuco body under the combined action of a reducing agent and tea saponin), oxidation (the oxidation of the soluble indigo is completed under the action of air, so that the insoluble indigo is fixed in the fiber and on the surface), cleaning (under the action of clear water, acetic acid and high temperature, the indigo attached on the surface of the fiber is removed due to too low binding force, and the color fastness of the color yarn is improved).
Further described, the above process solves the above yarn plant indigo dyeing problem by the following three aspects:
(1) The bath ratio is improved, the indigo dye liquor is filled in the cylinder body, the contact area between the dye liquor and air is reduced to the greatest extent, and the over oxidation of the indigo dye liquor is prevented; tea saponin and a reducing agent are supplemented in batches to ensure that the indigo dye liquor is always in a reduced state, so that the problem that the indigo dye is easily oxidized by air is solved;
(2) The dyed yarn is loosely wound, so that the dye liquor has a basic space for dyeing the yarn; pretreating loose type cone yarns, adding natural surfactant to enable the cone yarns to be fully wetted and permeated, and increasing a channel through which dye liquor flows; the internal pressure of the cylinder body is increased, so that the dye liquor fully forms internal flow-external flow circulation in the yarn cylinder, and the problem of uneven yarn cylinder permeation in the dye liquor diffusion process is solved;
(3) The cylinder is internally provided with a plurality of pressurization-discharge cycles, a large amount of air is brought in during pressurization to oxidize indigo, air and water remained in the cone yarn are taken away during discharge, and the interval is 1 to 2 minutes, so that the problem of uneven dyeing caused by insufficient surface oxidation and insufficient internal oxidation is solved.
Detailed Description
Example 1
The main components of the biological reducing agent of the embodiment are as follows:
the balance of deionized water.
The preparation process of the biological reducing agent comprises the following steps:
(1) Uniformly stirring the saccharide compound with deionized water and acetic acid to prepare colloidal liquid;
(2) Adding inorganic oxide sodium periodate into the step (1), uniformly mixing, and reacting at 50 ℃;
(3) Adding alcohol compound according to a certain proportion, continuously stirring and uniformly mixing.
The yarn of the fabric to be treated is 40S pure cotton yarn, and the basic performance index of the fabric is as follows: the rubbing fastness is >3 grade, the soaping fastness is >3 grade, the light fastness is >3 grade, and the washing fastness is >3 grade.
The biological reducing agent is applied to the reduction and dyeing process of the plant indigo fabric to realize the green dyeing of the plant indigo, and the main process is as follows:
cotton cone yarn loose winding, pretreatment of natural alkaline agent, preparation of biological reducing agent, pre-reduction of plant indigo, dyeing, oxidation, water washing and drying winding.
The parameters of the core steps are controlled as follows:
(1) Pre-reduction of plant indigo: fully mixing the prepared biological reducing agent with plant indigo, regulating the pH value of the dye liquor by using tea saponin to ensure that the pH value is stabilized in the range of 11-12, measuring the reduction potential of the dye liquor, and maintaining the reduction potential at-700 to-800 mv, wherein the adding concentration of the biological reducing agent is 5g/L.
(2) And (3) dyeing: putting the cone yarn into a dye vat, feeding clear water in a bath ratio of 1:10, adding a biological reducing agent and tea saponin, providing an environment capable of dyeing, wherein the concentration of the biological reducing agent is 2g/L, and the concentration of the tea saponin is 2g/L.
Heating to 30 ℃ at 1.5 ℃/min, preserving heat for 60min, adding 10% of pre-reduced plant indigo dye liquor, supplementing biological reducing agent and tea saponin every 15min, and supplementing the concentration in the same way as in the step (2).
Setting the technological parameters of a dye vat: the pressure of the dye vat body is set to be 3.9-4.0MPa.s, the power of the main pump is 90-100%, the forward circulation time of the dye liquor is 2min, and the reverse circulation time of the dye liquor is 6min.
(3) Oxidizing: by ventilation oxidation
After the dye liquor in the cylinder is fully discharged, the outside air is introduced into the cylinder body in a pressurizing mode, a large amount of air is brought in during pressurizing to oxidize indigo, air and water remained in the cone yarn are taken away during discharging, the interval between pressurizing and discharging is 1-2 minutes, and the pressurizing lasts for 10 minutes.
Example 2
The main components of the biological reducing agent of this example are as follows:
the balance of deionized water.
The preparation process of the biological reducing agent comprises the following steps:
(1) Uniformly stirring the saccharide compound with deionized water and acetic acid to prepare colloidal liquid;
(2) Adding inorganic oxide sodium periodate into the step (1), uniformly mixing, and reacting at 45 ℃;
(3) Adding alcohol compound according to a certain proportion, continuously stirring and uniformly mixing.
The yarn of the fabric to be treated is 40S pure cotton yarn, and the basic performance indexes are as follows: the rubbing fastness is >3 grade, the soaping fastness is >3 grade, the light fastness is >3 grade, and the washing fastness is >3 grade.
The biological reducing agent is applied to the reduction and dyeing process of the plant indigo fabric to realize the green dyeing of the plant indigo, and the main process is as follows:
cotton cone yarn loose winding, pretreatment of natural alkaline agent, preparation of biological reducing agent, pre-reduction of plant indigo, dyeing, oxidation, water washing and drying winding.
The parameters of the core steps are controlled as follows:
(1) Pre-reduction of plant indigo: fully mixing the prepared biological reducing agent with plant indigo, regulating the pH value of the dye liquor by using tea saponin to ensure that the pH value is stabilized in the range of 11-12, measuring the reduction potential of the dye liquor, and maintaining the reduction potential at-800 to-700 mv, wherein the adding concentration of the biological reducing agent is 20g/L.
(2) And (3) dyeing: putting the cone yarn into a dye vat, feeding clear water in a bath ratio of 1:20, adding a biological reducing agent and tea saponin, providing an environment capable of dyeing, wherein the concentration of the biological reducing agent is 3g/L, and the concentration of the tea saponin is 1g/L.
Heating to 30 ℃ at 1.5 ℃/min, preserving heat for 60min, adding 10% of pre-reduced plant indigo dye liquor, supplementing biological reducing agent and tea saponin every 15min, and supplementing the concentration in the same way as in the step (2).
Setting the technological parameters of a dye vat: the pressure of the dye vat body is set to be 3.9-4.0MPa.s, the power of the main pump is 90-100%, the forward circulation time of the dye liquor is 4min, and the reverse circulation time of the dye liquor is 10min.
(3) Oxidation
Adopts ventilation oxidation: after the dye liquor in the cylinder is fully discharged, the outside air is introduced into the cylinder body in a pressurizing mode, a large amount of air is brought in during pressurizing to oxidize indigo, air and water remained in the cone yarn are taken away during discharging, the interval between pressurizing and discharging is 1-2 minutes, and the pressurizing lasts for 10 minutes.
Example 3
The main components of the biological reducing agent of this example are as follows:
the balance of deionized water.
The preparation process of the biological reducing agent comprises the following steps:
(1) Uniformly stirring the saccharide compound with deionized water and acetic acid to prepare colloidal liquid;
(2) Adding inorganic oxide sodium periodate into the step (1), uniformly mixing, and reacting at 60 ℃;
(3) Adding alcohol compound according to a certain proportion, continuously stirring and uniformly mixing.
The yarn of the fabric to be treated is 40S pure cotton yarn, and the basic performance indexes are as follows: the rubbing fastness is >3 grade, the soaping fastness is >3 grade, the light fastness is >3 grade, and the washing fastness is >3 grade.
The biological reducing agent is applied to the reduction and dyeing process of the plant indigo fabric to realize the green dyeing of the plant indigo, and the main process is as follows:
cotton cone yarn loose winding, pretreatment of natural alkaline agent, preparation of biological reducing agent, pre-reduction of plant indigo, dyeing, oxidation, water washing and drying winding.
The parameters of the core steps are controlled as follows:
(1) Pre-reduction of plant indigo: fully mixing the prepared biological reducing agent with plant indigo, regulating the pH value of the dye liquor by using tea saponin to ensure that the pH value is stabilized in the range of 11-12, measuring the reduction potential of the dye liquor, and maintaining the reduction potential at-700 to-800 mv, wherein the adding concentration of the biological reducing agent is 12g/L.
(2) And (3) dyeing: placing the cone yarn in a dye vat, feeding clear water in a bath ratio of 1:15, adding a biological reducing agent and tea saponin, providing an environment capable of dyeing, wherein the concentration of the biological reducing agent is 5g/L, and the concentration of the tea saponin is 3g/L.
Heating to 30 ℃ at 1.5 ℃/min, preserving heat for 60min, adding 10% of pre-reduced plant indigo dye liquor, supplementing biological reducing agent and tea saponin every 15min, and supplementing the concentration in the same way as in the step (2).
Setting the technological parameters of a dye vat: the pressure of the dye vat body is set to be 3.9-4.0MPa.s, the power of the main pump is 90-100%, the forward circulation time of the dye liquor is 1min, and the reverse circulation time of the dye liquor is 3min.
(3) Oxidizing: after the dye liquor in the cylinder is fully discharged by ventilation oxidation, the outside air is introduced into the cylinder body in a pressurizing mode, a large amount of air is introduced during pressurizing to oxidize indigo, air and water remained in the cone yarn are taken away during pressure discharge, the interval between pressurizing and pressure discharge is 1-2 minutes, and the pressurizing lasts for 10 minutes.
Comparative example 1: conventional caustic soda-sodium hydrosulfite indigo yarn dyeing process
The dyeing process of this comparative example is as follows:
(1) The cotton yarn to be dyed is fully moistened and placed in a dyeing cylinder body, the operation is carried out for 10min, 2g/L sodium hydrosulfite and 1.5g/L caustic soda are added, so that the dyeing bath is in an alkaline environment for the indigo dye to absorb and dye;
(2) Pre-reduction of plant indigo dye liquor: adding clear water into plant indigo powder, sodium hydrosulfite and sodium hydroxide according to the proportion of 1:1.25:1, and fully mixing and dissolving the plant indigo powder, the sodium hydrosulfite and the sodium hydroxide according to the bath ratio of 1:50 to ensure that the solution is yellow-green and the pH value is between 11 and 12 for standby;
(3) Dye-up of plant indigo: and (3) placing the dye liquor with the concentration of 10% of the mother liquor into a secondary cylinder of a dyeing machine, and adding the dye liquor in a circulating reflux way. Reflux to the auxiliary cylinder every 20 minutes, measuring the pH value and the reduction potential, adding 1.25g/L of the protective powder and 1g/L of caustic soda, draining liquid after 3 times, and washing with water;
(4) Washing of the vegetable indigo dyed yarn: washing with clear water overflowed for 10-15min, draining, washing with clear water, adding hydrogen peroxide 1.5g/L, washing with clear water, washing with hot water at 80 ℃ for 30min, washing with clear water, washing with acetic acid 1.5g/L, washing with clear water, deoxidizing enzyme 1.5g/L, washing with two clear water, and drying.
Table 1: performance index comparison Table of indigo yarn for the present example and comparative example
| Numbering device | K/S value | Fastness to washing with soap | Fastness to rubbing | Fastness to light | Fastness to washing |
| Example 1 | 21.25 | 3-4 | 4 | 3 | 4 |
| Example 2 | 23.48 | 3-4 | 4 | 3 | 4 |
| Example 3 | 22.68 | 3-4 | 3-4 | 3-4 | 3-4 |
| Comparative example 1 | 20.67 | 3 | 3 | 3 | 3-4 |
From the comparison of table 1, it can be seen that: the biological reducer provided by the application is adopted to dye yarn indigo, so that the K/S value of the fabric/yarn can be effectively improved, the dyeing effect is good, and the soaping fastness, the rubbing color fastness, the light color fastness and the washing color fastness can basically reach 4 levels.
Claims (4)
1. A method for applying a biological reducing agent to plant indigo dyed yarns, characterized by the steps of:
(1) Plant indigo dye pre-reduction: fully mixing a biological reducing agent with plant indigo at a concentration of 5-20g/L, regulating the pH value to 11-12, and measuring and reducing the potential to be more than-800-750 mv to obtain plant indigo dye liquor;
(2) And (3) dyeing: placing the cone yarn to be treated in a dye vat, feeding clear water at a bath ratio of 1:10-20, adding 1-3g/L of tea saponin and 2-5g/L of biological reducing agent, heating to 20-45 ℃ at 1-3 ℃/min, preserving heat for 20-90min, adding the plant indigo dye liquor in the step (1) in batches, supplementing 1-3g/L of biological reducing agent and 1-3g/L of tea saponin every 10-20min, wherein the pressure of a dye vat cylinder body is 3-5MPa, the power of a main pump is 80-100%, the forward circulation time of the dye liquor is 1-4min, and the reverse circulation time is 3-10min;
(3) Oxidizing: fully discharging dye liquor, pressurizing and introducing air into the cylinder body, wherein the pressurizing interval time is 1-2min, each time lasting time is 8-10min, cleaning and drying,
the biological reducing agent is prepared from 30-40% of saccharide compounds, 1-6% of inorganic oxides, 2-5% of organic acids, 3-8% of alcohol compounds and deionized water by the following steps:
1) Uniformly stirring the saccharide compound with deionized water and organic acid to prepare colloidal liquid;
2) Adding inorganic oxide into the step 1), uniformly mixing, and reacting at 45-55 ℃ for later use;
3) Adding alcohol compound, stirring, mixing to obtain biological reducer,
the saccharide compound is one or a mixture of more of raffinose, glucose and chitosan,
the organic acid is any one or a mixture of more of acetic acid, citric acid and tartaric acid,
the alcohol compound is one or a mixture of more of ethanol, glycol and propanol,
the inorganic oxide is sodium periodate or potassium periodate.
2. A method of applying a bioreductive agent to vegetable indigo dyed yarn according to claim 1, characterized in that: the addition amount of the alcohol compound is 5-6%.
3. The method of applying a bioreductive agent to vegetable indigo dyed yarn according to claim 1, characterized in that the yarn is pre-treated before dyeing: moistening the cone yarn into a cylinder, adding tea saponin, dissolving, increasing the temperature to 60-85 ℃ at 1-3 ℃/min for 10-25min, increasing the temperature to 85-98 ℃ at 1-2 ℃/min for 30-60min, washing with water, pickling, washing with water, and taking out to obtain the cone yarn to be treated.
4. A method of applying a bioreductive agent to vegetable indigo dyed yarn according to claim 1, characterized in that: the cone yarn is obtained by winding by a loose winder.
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