CN113652877B - Dyeing method for plants by using dye - Google Patents
Dyeing method for plants by using dye Download PDFInfo
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- CN113652877B CN113652877B CN202111037338.0A CN202111037338A CN113652877B CN 113652877 B CN113652877 B CN 113652877B CN 202111037338 A CN202111037338 A CN 202111037338A CN 113652877 B CN113652877 B CN 113652877B
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- 238000004043 dyeing Methods 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 54
- 239000004744 fabric Substances 0.000 claims abstract description 105
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 65
- 239000000243 solution Substances 0.000 claims abstract description 48
- 239000011259 mixed solution Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052709 silver Inorganic materials 0.000 claims abstract description 36
- 239000004332 silver Substances 0.000 claims abstract description 36
- -1 silver ions Chemical class 0.000 claims abstract description 31
- 239000000284 extract Substances 0.000 claims abstract description 30
- 230000001105 regulatory effect Effects 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000007865 diluting Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 229920000742 Cotton Polymers 0.000 claims description 65
- 241000196324 Embryophyta Species 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 28
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 240000001972 Gardenia jasminoides Species 0.000 claims 1
- 238000010979 pH adjustment Methods 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 7
- 239000004753 textile Substances 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 230000003471 anti-radiation Effects 0.000 abstract description 2
- 239000000975 dye Substances 0.000 description 95
- 244000111489 Gardenia augusta Species 0.000 description 25
- 239000000843 powder Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 20
- 235000013399 edible fruits Nutrition 0.000 description 20
- 235000018958 Gardenia augusta Nutrition 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 238000000967 suction filtration Methods 0.000 description 9
- 241000588724 Escherichia coli Species 0.000 description 6
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 6
- 241000191967 Staphylococcus aureus Species 0.000 description 6
- 235000013311 vegetables Nutrition 0.000 description 6
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 4
- 239000000419 plant extract Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 244000025254 Cannabis sativa Species 0.000 description 3
- 229930182559 Natural dye Natural products 0.000 description 3
- 244000269722 Thea sinensis Species 0.000 description 3
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
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- 239000000978 natural dye Substances 0.000 description 3
- 235000019371 penicillin G benzathine Nutrition 0.000 description 3
- 229940056360 penicillin g Drugs 0.000 description 3
- 230000004224 protection Effects 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 240000001592 Amaranthus caudatus Species 0.000 description 2
- 235000009328 Amaranthus caudatus Nutrition 0.000 description 2
- 244000306301 Caesalpinia sappan Species 0.000 description 2
- 235000015162 Caesalpinia sappan Nutrition 0.000 description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 2
- 235000007516 Chrysanthemum Nutrition 0.000 description 2
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 2
- 240000000691 Houttuynia cordata Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 241000334160 Isatis Species 0.000 description 2
- 241001071917 Lithospermum Species 0.000 description 2
- 244000246386 Mentha pulegium Species 0.000 description 2
- 235000016257 Mentha pulegium Nutrition 0.000 description 2
- 235000004357 Mentha x piperita Nutrition 0.000 description 2
- 206010027439 Metal poisoning Diseases 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 241000972673 Phellodendron amurense Species 0.000 description 2
- 241000219492 Quercus Species 0.000 description 2
- 235000016976 Quercus macrolepis Nutrition 0.000 description 2
- 241001149655 Rubia tinctorum Species 0.000 description 2
- 244000274883 Urtica dioica Species 0.000 description 2
- 235000009108 Urtica dioica Nutrition 0.000 description 2
- 239000004178 amaranth Substances 0.000 description 2
- 235000012735 amaranth Nutrition 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 235000009120 camo Nutrition 0.000 description 2
- 235000012730 carminic acid Nutrition 0.000 description 2
- 239000004106 carminic acid Substances 0.000 description 2
- 235000005607 chanvre indien Nutrition 0.000 description 2
- 229940080423 cochineal Drugs 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 208000010501 heavy metal poisoning Diseases 0.000 description 2
- 239000011487 hemp Substances 0.000 description 2
- 235000001050 hortel pimenta Nutrition 0.000 description 2
- 239000003223 protective agent Substances 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 1
- 241000130781 Arnebia Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 235000013717 Houttuynia Nutrition 0.000 description 1
- 235000013719 Houttuynia cordata Nutrition 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 244000132436 Myrica rubra Species 0.000 description 1
- 240000009235 Rubia cordifolia Species 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- DGQLVPJVXFOQEV-JNVSTXMASA-N carminic acid Chemical compound OC1=C2C(=O)C=3C(C)=C(C(O)=O)C(O)=CC=3C(=O)C2=C(O)C(O)=C1[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O DGQLVPJVXFOQEV-JNVSTXMASA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 108010006161 conchiolin Proteins 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 235000013616 tea Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 235000013799 ultramarine blue Nutrition 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
- D06P1/34—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
-
- 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
-
- 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
- D06P1/90—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 dyes dissolved in organic solvents or aqueous emulsions thereof
- D06P1/908—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 dyes dissolved in organic solvents or aqueous emulsions thereof using specified 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
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Coloring (AREA)
Abstract
The invention relates to the field of textile printing and dyeing, and discloses a dyeing method using dye plants, which comprises the following steps: (1) Adding dye plant into water, regulating pH to 8-12, stirring, and filtering to obtain extract solution; (2) Adding silver ions into the extract solution obtained in the step (1) to obtain a mixed solution, regulating the pH value of the mixed solution to 9-13, and then reacting at 60-90 ℃ for 20-40min to obtain a nano silver dye solution; (3) Diluting the nano silver dye liquor obtained in the step (2) by 5 times, then adjusting the pH value to 7-9, and then placing the fabric into the nano silver dye liquor with the pH value adjusted for dyeing to obtain the dyed fabric. The method disclosed by the invention uses dye plants, silver ions are used as mordants, the dye uptake and color fastness of the plant dye are increased, the dyeing effect can be enhanced, the method is environment-friendly, no reducing agent is added, and the antibacterial performance and the anti-radiation effect of nano silver are utilized to functionalize the fabric.
Description
Technical Field
The invention relates to the field of textile printing and dyeing, in particular to a dyeing method using dye plants.
Background
With the importance of environmental protection, the dye industry has also undergone a great change, and natural dyes with reproducibility and degradability are popular. Natural dyes are generally derived from plants, animals and minerals, and are based on vegetable dyes. The vegetable dye is extracted from the root, stem, leaf and fruit of dye plant, such as: indigo, radix Rubiae, radix Arnebiae, carthami flos, mori fructus, tea, etc. The animal dye has small number and is mainly obtained from conchiolin and cochineal, such as cochineal (purple) gum, cochineal carmine, etc. The mineral dye is a colored inorganic substance extracted from minerals, such as chrome yellow, ultramarine blue, magnesium brown, etc. In recent years, it has been found that pigments produced by microorganisms such as bacteria, fungi, mold and the like can also be used as a source of natural dyes.
The natural vegetable dye has wide sources, is more similar to nature, and has rich colors. However, the natural vegetable dye generally has the problems of low dye-uptake and the like during dyeing. In the dyeing process of the vegetable dye, the metal ions such as copper, chromium, iron, aluminum and the like can be added to serve as mordant for fabrics with poor dyeing performance, so that the dyeing rate is improved, but some heavy metals can cause harm to human bodies, pollute the environment and limit the use in the finishing process of textiles. Therefore, an environment-friendly dyeing method is needed to improve the dyeing performance of the natural plant dye, which has important significance for better development and application of the natural plant dye and environmental protection.
Disclosure of Invention
The invention aims to overcome the following problems in the prior art: (1) The dye-uptake of the natural vegetable dye is generally low during dyeing; (2) Heavy metal ions added in the dyeing process cause harm to human bodies and pollute the environment. A dyeing method using dye plant is provided, which uses the extract of dye plant, silver ion is used as mordant, and the reductive molecule in the extract of dye plant is used to reduce silver into nano silver, and the nano silver is loaded on the surface of fabric. Silver ions and nano silver can increase dye uptake of the dye and can also functionalize the fabric.
In order to achieve the above object, the present invention provides a dyeing method using a dye plant, the method comprising the steps of:
(1) Adding dye plants into water, mixing, regulating pH value to 8-12, stirring at 60-90deg.C, and filtering to obtain extract solution, wherein the weight-volume ratio of the dye plants to water is 30-50g/L;
(2) Adding silver ions into the extract solution obtained in the step (1) to obtain a mixed solution, regulating the pH value of the mixed solution to 9-13, and then reacting at 60-90 ℃ for 20-40min to obtain a nano silver dye solution, wherein the concentration of the silver ions in the mixed solution is 0.5-3.5mmoL/L;
(3) Diluting the nano silver dye solution obtained in the step (2) by 5 times, regulating the pH value, and then placing the fabric into the nano silver dye solution with the pH value regulated for dyeing to obtain the dyed fabric.
Preferably, in step (1), the stirring time is 30-60min.
Preferably, in step (2), the source of silver ions is silver nitrate.
Preferably, in step (2), sodium hydroxide is used to adjust the pH of the mixed solution.
Preferably, in step (3), the fabric is cotton fabric, hemp fabric, wool fabric, silk fabric or chemical fiber fabric.
Preferably, in the step (1), the dye plant is at least one of sappan wood, madder, gardenia, phellodendron bark, peppermint, nettle, red bayberry oak, tea, lithospermum, amaranth, isatis root, chrysanthemum, houttuynia cordata and gallnut.
Further preferably, the dye plant is gardenia.
Preferably, in the step (3), the pH value of the diluted nano silver dye liquor is adjusted to 7-9.
Preferably, in the step (3), the volume weight ratio of the nano silver dye liquor to the fabric after the pH value is adjusted is 40-60mL/g.
Preferably, in step (3), the dyeing temperature is 50-70 ℃.
Preferably, in step (3), the time of the dyeing is 40-60min.
According to the method disclosed by the invention, the dye plants are used, silver ions are used as mordants, the reductive molecules in the dye plant extracts (plant dyes) are utilized to reduce silver into nano silver, the nano silver is loaded on the surface of the fabric, the dye uptake of the dye can be increased by the silver ions and the nano silver, and meanwhile, the dyeing effect can be enhanced by using the dye plant extracts as a protective agent. The dyeing process is green and environment-friendly, no reducing agent is added, the heavy metal poisoning of the fabric and the environmental pollution are avoided, and meanwhile, the fabric is functionalized by utilizing the antibacterial performance and the radiation resistance of the nano silver.
Drawings
FIG. 1 is a photograph of a dyed fabric prepared in example 1 of the invention;
FIG. 2 is a scanning electron micrograph of the dyed fabric prepared in example 1 of the invention;
FIG. 3 is a scanning electron micrograph of the dyed fabric prepared in example 1 of the invention;
FIG. 4 is a scanning electron micrograph of the dyed fabric prepared in example 1 of the invention;
FIG. 5 is a graph showing the antibacterial effect of the dyed fabric prepared in comparative example 13 against E.coli according to example 1 and examples 7 to 9 of the present invention;
FIG. 6 is a graph showing the bacteriostatic effect of the dyed fabric prepared in example 1, examples 7-9, and comparative example 13 on Staphylococcus aureus.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The present invention provides a method for dyeing plants using a dye, the method comprising the steps of:
(1) Adding dye plants into water, mixing, regulating pH value to 8-12, stirring at 60-90deg.C, and filtering to obtain extract solution, wherein the weight-volume ratio of the dye plants to water is 30-50g/L;
(2) Adding silver ions into the extract solution obtained in the step (1) to obtain a mixed solution, regulating the pH value of the mixed solution to 9-13, and then reacting at 60-90 ℃ for 20-40min to obtain a nano silver dye solution, wherein the concentration of the silver ions in the mixed solution is 0.5-3.5mmoL/L;
(3) Diluting the nano silver dye solution obtained in the step (2) by 5 times, regulating the pH value, and then placing the fabric into the nano silver dye solution with the pH value regulated for dyeing to obtain the dyed fabric.
In the present invention, in step (1), the pH value may be adjusted to 8, 8.25, 8.5, 8.75, 9, 9.25, 9.5, 9.75, 10, 10.25, 10.5, 10.75, 11, 11.25, 11.5, 11.75 or 12 after the dye plant is added to the water.
In particular embodiments, the temperature of the agitation may be 60 ℃, 62.5 ℃, 65 ℃, 67.5 ℃, 70 ℃, 72.5 ℃, 75 ℃, 77.5 ℃, 80 ℃, 82.5 ℃, 85 ℃, 87.5 ℃, or 90 ℃.
In the present invention, in the step (1), the stirring time is 30 to 60 minutes. Specifically, the stirring time may be 30min, 32.5min, 35min, 37.5min, 40min, 42.5min, 45min, 47.5min, 50min, 52.5min, 55min, 57.5min or 60min.
In particular cases, in step (1), the weight to volume ratio of dye plant to water may be 30g/L, 32.5g/L, 35g/L, 37.5g/L, 40g/L, 42.5g/L, 45g/L, 47.5g/L, or 50g/L.
In particular cases, in step (2), the concentration of silver ions in the mixed solution may be 0.5 mmole/L, 0.75 mmole/L, 1 mmole/L, 1.25 mmole/L, 1.5 mmole/L, 1.75 mmole/L, 2 mmole/L, 2.25 mmole/L, 2.5 mmole/L, 2.75 mmole/L, 3 mmole/L, 3.25 mmole/L, or 3.5 mmole/L.
In the present invention, in the step (1), the source of silver ions may be selected as usual in the art, and the concentration of silver ions in the mixed solution may be controlled to be 0.5 to 3.5mmoL/L. Preferably, the source of silver ions is silver nitrate.
In the present invention, in step (2), the pH of the mixed solution is adjusted using sodium hydroxide.
Specifically, in step (2), the pH of the mixed solution may be adjusted to 9, 9.25, 9.5, 9.75, 10, 10.25, 10.5, 10.75, 11, 11.25, 11.5, 11.75, 12, 12.25, 12.5, 12.75 or 13.
In particular, in step (2), the temperature of the reaction may be 60 ℃, 62.5 ℃, 65 ℃, 67.5 ℃, 70 ℃, 72.5 ℃, 75 ℃, 77.5 ℃, 80 ℃, 82.5 ℃, 85 ℃, 87.5 ℃ or 90 ℃.
In a specific case, in the step (2), the reaction time may be 20min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min or40 min.
In the present invention, in the step (3), the fabric is a cotton fabric, a hemp fabric, a wool fabric, a silk fabric or a chemical fiber fabric.
The leaves, roots, stems or fruits of the dye plants may be used for extraction staining in the present invention.
In the invention, the dye plant is at least one of sappan wood, madder, gardenia, phellodendron bark, peppermint, nettle, oak, tea, lithospermum, amaranth, isatis root, chrysanthemum, houttuynia and gallnut. Preferably, the dye plant is gardenia.
In the invention, in the step (3), water is added into the nano silver dye liquor obtained in the step (2) for dilution, and the volume of the diluted nano silver dye liquor is 5 times of that of the nano silver dye liquor obtained in the step (2).
In the invention, in the step (3), the pH value of the diluted nano silver dye liquor is adjusted to 7-9. Specifically, the pH of the diluted nano silver dye solution can be adjusted to 7, 7.25, 7.5, 7.75, 8, 8.25, 8.5, 8.75 or 9.
In the step (3), the volume weight ratio of the nano silver dye liquor to the fabric after the pH value is regulated is 40-60mL/g.
Specifically, the volume weight ratio of the nano silver dye solution to the fabric after the pH value is regulated can be 40mL/g, 42.5mL/g, 45mL/g, 47.5mL/g, 50mL/g, 52.5mL/g, 55mL/g, 57.5mL/g or 60mL/g.
In the present invention, in step (3), the dyeing temperature is 50 to 70 ℃. Specifically, the time of the dyeing may be 50 ℃, 52.5 ℃, 55 ℃, 57.5 ℃, 60 ℃, 62.5 ℃, 65 ℃, 67.5 ℃ or 70 ℃.
In the invention, in the step (3), the dyeing time is 40-60min. Specifically, the time of the dyeing may be 40min, 42.5min, 45min, 47.5min, 50min, 52.5min, 55min, 57.5min or 60min.
The method uses dye plants, silver ions are used as mordants, the reductive molecules in the dye plant extracts (plant dyes) are utilized to reduce silver into nano silver, the nano silver is loaded on the surface of the fabric, the silver ions and the nano silver can increase the dye uptake and the color fastness of the dye, and meanwhile, the dye plant extracts are used as protective agents to enhance the dyeing effect. The dyeing process is green and environment-friendly, no reducing agent is added, heavy metal poisoning of the fabric and environmental pollution are avoided, meanwhile, the antibacterial performance and the anti-radiation effect of the nano silver are utilized to functionalize the fabric, and the finished fabric has excellent antibacterial activity and anti-ultraviolet performance on escherichia coli and staphylococcus aureus.
The present invention will be described in detail by way of examples, but the method of the present invention is not limited thereto.
The dye plants used in the examples and comparative examples were all purchased from Hua grass rhyme biotechnology Co., bo, anhua, and the same cotton fabrics were used.
Example 1
(1) Adding 10g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 10, stirring for 45min at 70 ℃, and carrying out suction filtration to obtain an extract solution (the mass-volume ratio of the cape jasmine fruit powder to water is 40 g/L);
(2) Adding silver nitrate into the extract solution obtained in the step (1), fully dissolving to obtain a mixed solution, adjusting the pH value of the mixed solution to 10 (the concentration of silver ions in the mixed solution is 1 mmoL/L) by using sodium hydroxide, and then reacting for 30min at 75 ℃ to obtain a nano silver dye solution;
(3) Diluting the nano silver dye liquor obtained in the step (2) by 5 times, then adjusting the pH value to 8, then placing the cotton fabric into the nano silver dye liquor with the pH value adjusted for dyeing, wherein the volume weight ratio of the nano silver dye liquor with the pH value adjusted to the cotton fabric is 50mL/g, the dyeing temperature is controlled to be 70 ℃ by a constant-temperature water bath, and the dyeing time is 60min, so that the dyed cotton fabric A1 is obtained.
Example 2
(1) Adding 7.5g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 11.5, stirring at 80 ℃ for 40min, and carrying out suction filtration to obtain an extract solution (the mass volume ratio of the cape jasmine fruit powder to water is 30 g/L);
(2) Adding silver nitrate into the extract solution obtained in the step (1), fully dissolving to obtain a mixed solution, adjusting the pH value of the mixed solution to 13 (the concentration of silver ions in the mixed solution is 1.8 mmoL/L) by using sodium hydroxide, and then reacting at 60 ℃ for 40min to obtain a nano silver dye solution;
(3) Diluting the nano silver dye liquor obtained in the step (2) by 5 times, then adjusting the pH value to 8.5, then placing the cotton fabric into the nano silver dye liquor with the pH value adjusted for dyeing, wherein the volume weight ratio of the nano silver dye liquor with the pH value adjusted to the cotton fabric is 40mL/g, the dyeing temperature is controlled to be 65 ℃ by a constant-temperature water bath, and the dyeing time is 45min, so that the dyed cotton fabric A2 is obtained.
Example 3
(1) Adding 10.25g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 12, stirring at 60 ℃ for 60min, and carrying out suction filtration to obtain an extract solution (the mass volume ratio of the cape jasmine fruit powder to water is 41 g/L);
(2) Adding silver nitrate into the extract solution obtained in the step (1), fully dissolving to obtain a mixed solution, adjusting the pH value of the mixed solution to 9 (the concentration of silver ions in the mixed solution is 1.5 mmoL/L) by using sodium hydroxide, and then reacting for 25min at 82 ℃ to obtain a nano silver dye solution;
(3) Diluting the nano silver dye liquor obtained in the step (2) by 5 times, then adjusting the pH value to 9, then placing the cotton fabric into the nano silver dye liquor with the pH value adjusted for dyeing, wherein the volume weight ratio of the nano silver dye liquor with the pH value adjusted to the cotton fabric is 53mL/g, the dyeing temperature is controlled to be 70 ℃ by a constant-temperature water bath, and the dyeing time is 40min, so that the dyed cotton fabric A3 is obtained.
Example 4
(1) Adding 12.5g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 11, stirring for 35min at 85 ℃, and carrying out suction filtration to obtain an extract solution (the mass-volume ratio of the cape jasmine fruit powder to water is 50 g/L);
(2) Adding silver nitrate into the extract solution obtained in the step (1), fully dissolving to obtain a mixed solution, adjusting the pH value of the mixed solution to 10 (the concentration of silver ions in the mixed solution is 2.5 mmoL/L) by using sodium hydroxide, and then reacting for 20min at 90 ℃ to obtain a nano silver dye solution;
(3) Diluting the nano silver dye liquor obtained in the step (2) by 5 times, then adjusting the pH value to 7, then placing the cotton fabric into the nano silver dye liquor with the pH value adjusted for dyeing, wherein the volume weight ratio of the nano silver dye liquor with the pH value adjusted to the cotton fabric is 60mL/g, the dyeing temperature is controlled to be 56 ℃ by a constant-temperature water bath, and the dyeing time is 55min, so that the dyed cotton fabric A4 is obtained.
Example 5
(1) Adding 9.5g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 8, stirring for 30min at 90 ℃, and carrying out suction filtration to obtain an extract solution (the mass volume ratio of the cape jasmine fruit powder to water is 38 g/L);
(2) Adding silver nitrate into the extract solution obtained in the step (1), fully dissolving to obtain a mixed solution, adjusting the pH value of the mixed solution to 11 (the concentration of silver ions in the mixed solution is 3.2 mmoL/L) by using sodium hydroxide, and then reacting for 37min at 65 ℃ to obtain a nano silver dye solution;
(3) Diluting the nano silver dye liquor obtained in the step (2) by 5 times, then adjusting the pH value to 7.5, then placing the cotton fabric into the nano silver dye liquor with the pH value adjusted for dyeing, wherein the volume weight ratio of the nano silver dye liquor with the pH value adjusted to the cotton fabric is 45mL/g, the dyeing temperature is controlled to be 66 ℃ by a constant-temperature water bath, and the dyeing time is 43min, so that the dyed cotton fabric A5 is obtained.
Example 6
(1) Adding 11.75g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 8, stirring for 55min at 65 ℃, and carrying out suction filtration to obtain an extract solution (the mass volume ratio of the cape jasmine fruit powder to water is 47 g/L);
(2) Adding silver nitrate into the extract solution obtained in the step (1), fully dissolving to obtain a mixed solution, adjusting the pH value of the mixed solution to 13 (the concentration of silver ions in the mixed solution is 2.8 mmoL/L) by using sodium hydroxide, and then reacting for 21min at 88 ℃ to obtain a nano silver dye solution;
(3) Diluting the nano silver dye liquor obtained in the step (2) by 5 times, then adjusting the pH value to 8.5, then placing the cotton fabric into the nano silver dye liquor with the pH value adjusted for dyeing, wherein the volume weight ratio of the nano silver dye liquor with the pH value adjusted to the cotton fabric is 50mL/g, and the dyeing temperature is controlled to be 50 ℃ by a constant-temperature water bath, and the dyeing time is 60min, so that the dyed cotton fabric A6 is obtained.
Example 7
The procedure described in example 1 was carried out, except that in step (2), the concentration of silver ions in the mixed solution was 0.5mmoL/L, to obtain a dyed cotton fabric A7.
Example 8
The process of example 1 was carried out, except that in step (2), the concentration of silver ions in the mixed solution was 2mmoL/L, to obtain a dyed cotton fabric A8.
Example 9
The procedure of example 1 was followed, except that in step (2), the concentration of silver ions in the mixed solution was 3mmoL/L, to obtain a dyed cotton fabric A9.
Example 10
The process described in example 1 was carried out, except that in step (2), the concentration of silver ions in the mixed solution was 3.5mmoL/L, to obtain a dyed cotton fabric A10.
Example 11
The procedure described in example 1 was followed, except that the dye plant used was Rubia cordifolia, giving dyed cotton fabric A11.
Example 12
The procedure described in example 1 was followed, except that the dye plant used was arnebia root, resulting in a dyed cotton fabric A12.
Comparative example 1
The process of example 2 was carried out, except that in step (1), 5g of gardenia powder pulverized with a pulverizer was added to 250ml of deionized water at a mass/volume ratio of 20g/L to water, to obtain a dyed cotton fabric D1.
Comparative example 2
The process of example 4 was carried out, except that 16.25g of gardenia powder pulverized with a pulverizer was added to 250ml of deionized water in the step (1), and the mass-to-volume ratio of the gardenia powder to water was 65g/L, to obtain a dyed cotton fabric D2.
Comparative example 3
The process according to example 1 was carried out, except that in step (2), the concentration of silver ions in the mixed solution was 0.2mmoL/L, resulting in a dyed cotton fabric D3.
Comparative example 4
The process according to example 1 was carried out, except that in step (2), the concentration of silver ions in the mixed solution was 4mmoL/L, resulting in a dyed cotton fabric D4.
Comparative example 5
The procedure described in example 3 was carried out, except that in step (2), the pH of the mixed solution was adjusted to 8 to obtain dyed cotton D5.
Comparative example 6
The procedure described in example 2 was followed, except that in step (2), the pH of the mixed solution was adjusted to 13.5 to obtain dyed cotton D6.
Comparative example 7
The process described in example 2 was carried out, except that in step (2), the temperature of the reaction was 50℃to obtain a dyed cotton fabric D7.
Comparative example 8
The process described in example 4 was carried out, except that in step (2), the temperature of the reaction was 95℃to obtain a dyed cotton fabric D8.
Comparative example 9
The process described in example 4 was carried out, except that in step (2), the reaction time was 10 minutes, giving a dyed cotton fabric D9.
Comparative example 10
The process described in example 2 was carried out, except that in step (2), the reaction time was 55min, resulting in dyed cotton D10.
Comparative example 11
The comparative example uses silver ion to pretreat cotton fabric and then dye, and the specific operation steps are as follows:
(1) Adding 10g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 10, stirring for 45min at 70 ℃, and carrying out suction filtration to obtain an extract solution (the mass-volume ratio of the cape jasmine fruit powder to water is 40 g/L);
(2) Placing the cotton fabric into a silver nitrate solution with the volume weight ratio of 1mmoL/L to the cotton fabric of 25mL/g, oscillating at room temperature for 40min, taking out and airing to obtain the silver nitrate pretreated cotton fabric.
(3) Placing the silver nitrate pretreated cotton fabric obtained in the step (2) into the extract solution obtained in the step (1), wherein the volume weight ratio of the extract solution to the silver nitrate pretreated cotton fabric is 50mL/g, the dyeing temperature is controlled to be 70 ℃ by a constant-temperature water bath, and the dyeing time is 60min, so as to obtain the dyed cotton fabric D11.
Comparative example 12
The comparative example uses silver ion post-treatment to dye cotton fabrics, and the specific experimental steps are as follows:
(1) Adding 10g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 10, stirring for 45min at 70 ℃, and carrying out suction filtration to obtain an extract solution (the mass-volume ratio of the cape jasmine fruit powder to water is 40 g/L);
(2) Placing the cotton fabric into the extract solution obtained in the step (1), wherein the volume weight ratio of the extract solution to the cotton fabric is 50mL/g, the dyeing temperature is controlled to be 70 ℃ by a constant-temperature water bath, the dyeing time is 60min, and taking out and airing the cotton fabric to obtain the dye plant dyed cotton fabric;
(3) Placing the dyed cotton fabric on the dye plant obtained in the step (2) into a silver nitrate solution with the volume weight ratio of 1mmoL/L to the dyed cotton fabric on the dye plant of 25mL/g, and carrying out constant-temperature oscillation treatment for 40min at room temperature to obtain the dyed cotton fabric D12.
Comparative example 13
No silver ion was added to this comparative example, and the specific procedure was as follows:
(1) Adding 10g of cape jasmine fruit powder crushed by a crusher into 250ml of deionized water, mixing, adjusting the pH value to 10, stirring for 45min at 70 ℃, and carrying out suction filtration to obtain an extract solution (the mass-volume ratio of the cape jasmine fruit powder to water is 40 g/L);
(2) Adjusting the pH value of the extract solution obtained in the step (1) to 10 by using sodium hydroxide, and then reacting for 30min at 75 ℃ to obtain a dye liquor;
(3) Diluting the dye liquor obtained in the step (2) by 5 times, regulating the pH value to 8, then placing the cotton fabric into the dye liquor with the pH value regulated for dyeing, wherein the volume weight ratio of the dye liquor with the pH value regulated to the cotton fabric is 50mL/g, the dyeing temperature is controlled to be 70 ℃ by a constant-temperature water bath, and the dyeing time is 60min, so as to obtain the dyed cotton fabric D13.
Test example 1
The photo of A1 is shown in figure 1, and the dyed cotton fabric obtained after dyeing by the method of the invention is uniform in dyeing.
Test example 2
And (3) detecting the A1 by using a scanning electron microscope, wherein a scanning electron microscope photo is shown in fig. 2-4, granular substances are gathered on the surface of the dyed cotton fabric and are attached to the surface of the fiber, so that the nano silver particles are attached to the surface of the fabric and are uniformly distributed.
Test example 3
Detecting antibacterial effects of A1, A7, A8, A9 and D13 on staphylococcus aureus and escherichia coli, and additionally arranging a antibacterial control experiment of benzyl penicillin (antibiotics) on the staphylococcus aureus and escherichia coli;
the experimental detection method comprises the following steps: GB/T20944.1-2007 evaluation of antibacterial Properties of textiles part 1: agar plate diffusion method
The antibacterial results of Escherichia coli are shown in FIG. 5, and benzyl penicillin (antibiotic), D13, A7, A1, A8 and A9 correspond to 1-6 in FIG. 5, respectively;
the antibacterial results on Staphylococcus aureus are shown in FIG. 6, and benzyl penicillin (antibiotic), D13, A7, A1, A8 and A9 correspond to 1-6 in FIG. 6, respectively;
as shown in the results of FIGS. 5 and 6, the dyed cotton fabric obtained by adding silver showed inhibition zones against Staphylococcus aureus and Escherichia coli, indicating that the inhibition zones against both colonies were present, and the inhibition zone of the dyed cotton fabric was increased by increasing the silver concentration. The method has the advantage that the dyed cotton fabric obtained by the method has good antibacterial effect.
Test example 4
In order to better illustrate the technical effect of the invention, a blank group 1 is additionally arranged;
blank 1
Blank cotton D14 without any treatment.
K/S values of A1-A12 and D1-D14 are respectively tested, and the color fastness to soaping is achieved;
the test method of the K/S value comprises the following steps: the color depth K/S value of the dyed cotton fabric was measured using a Datecolor400 color meter.
The color fastness testing method comprises the following steps: GB/T3921-2008 "fastness to soaping for textile color fastness test" test.
The results are shown in Table 1.
TABLE 1
As can be seen from the results in Table 1, the dyed cotton fabric obtained by the method of the present invention has a large K/S value, i.e., a good dye-uptake and a high fastness to soaping.
Testing the color difference between A1-A12 and D1-D13 and D14 respectively;
the color difference testing method comprises the following steps: and calculating the chromatic aberration of A1-A12, D1-D13 and D14 respectively by using GB/T7921-2008 standard of uniform color space and chromatic aberration formula.
The results are shown in Table 2.
The color difference with D14 is measured in examples 1-12 and comparative examples 1-13, the data are processed, the larger the numerical value before the (+/-) "in the experimental data is, the larger the average color difference between the dyed cotton fabric and D14 is, namely, the larger the color difference is, the magnitude of the corresponding value after the (+/-)" is used for explaining the repeatability of the dyeing method, and the larger the numerical value is, the worse the repeatability of the dyeing method is.
TABLE 2
The data in Table 2 show that the fabric dyed by the method has good dyeing effect, and the dyeing method has good repeatability and easily controlled chromatic aberration.
UPF, T (UVA) and T (UVB) were tested for A1-A12, D1-D14, respectively;
the method for testing the ultraviolet resistance of the fabric comprises the following steps: GB/T18830-2002 evaluation of ultraviolet resistance of textiles.
The results are shown in Table 3.
TABLE 3 Table 3
As can be seen from the results of Table 3, the dyed fabric obtained by the method of the present invention has good ultraviolet resistance.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (7)
1. A method of dyeing plants with a dye, the method comprising the steps of:
(1) Adding dye plants into water, mixing, regulating pH value to 8-12, stirring at 60-90deg.C, and filtering to obtain extract solution, wherein the weight-volume ratio of the dye plants to water is 30-50g/L;
(2) Adding silver ions into the extract solution obtained in the step (1) to obtain a mixed solution, regulating the pH value of the mixed solution to 9-13, and then reacting at 60-90 ℃ for 20-40min to obtain a nano silver dye solution, wherein the concentration of the silver ions in the mixed solution is 0.5-3.5mmoL/L;
(3) Diluting the nano silver dye liquor obtained in the step (2) by 5 times, regulating the pH value, and then placing the fabric into the nano silver dye liquor with the pH value regulated for dyeing to obtain dyed fabric;
in the step (3), the pH value of the diluted nano silver dye liquor is regulated to 7-9;
the dye plant is gardenia;
the fabric is cotton fabric.
2. The method according to claim 1, wherein in step (1), the stirring time is 30 to 60 minutes.
3. The method of claim 1, wherein in step (2), the source of silver ions is silver nitrate.
4. The method according to claim 1, wherein in step (2), the pH of the mixed solution is adjusted using sodium hydroxide.
5. The method according to claim 1, wherein in the step (3), the volume weight ratio of the nano silver dye solution to the fabric after the pH adjustment is 40-60mL/g.
6. The method according to claim 1, wherein in step (3), the dyeing temperature is 50-70 ℃.
7. The method according to claim 1 or 6, wherein in step (3), the dyeing time is 40-60min.
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| 李岭岭."天然多酚对蚕丝纤维的染色及功能改性".苏州大学硕士学位论文.2018,全文. * |
| 程桐怀."茶梗提取物对天然纤维的染色及功能改性".苏州大学硕士学位论文.2021,52-68. * |
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