CN117188180A - Cellulose fiber and dyeing method thereof - Google Patents
Cellulose fiber and dyeing method thereof Download PDFInfo
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- CN117188180A CN117188180A CN202311387170.5A CN202311387170A CN117188180A CN 117188180 A CN117188180 A CN 117188180A CN 202311387170 A CN202311387170 A CN 202311387170A CN 117188180 A CN117188180 A CN 117188180A
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- dyeing
- vat dye
- vat
- liquid ammonia
- ammonia
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- 238000004043 dyeing Methods 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 45
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 40
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 87
- 239000000984 vat dye Substances 0.000 claims abstract description 87
- 239000000835 fiber Substances 0.000 claims abstract description 37
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 30
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 30
- 239000000975 dye Substances 0.000 claims abstract description 26
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 230000001590 oxidative effect Effects 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 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 38
- 235000000177 Indigofera tinctoria Nutrition 0.000 claims description 37
- 229940097275 indigo Drugs 0.000 claims description 37
- 229920000742 Cotton Polymers 0.000 claims description 24
- 229910021529 ammonia Inorganic materials 0.000 claims description 14
- 239000002585 base Substances 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 229920000297 Rayon Polymers 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000009980 pad dyeing Methods 0.000 claims description 3
- -1 yarn Substances 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
- 235000005607 chanvre indien Nutrition 0.000 claims description 2
- 239000011487 hemp Substances 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 159000000000 sodium salts Chemical class 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 239000012466 permeate Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- JFVXEJADITYJHK-UHFFFAOYSA-L disodium 2-(3-hydroxy-5-sulfonato-1H-indol-2-yl)-3-oxoindole-5-sulfonate Chemical compound [Na+].[Na+].Oc1c([nH]c2ccc(cc12)S([O-])(=O)=O)C1=Nc2ccc(cc2C1=O)S([O-])(=O)=O JFVXEJADITYJHK-UHFFFAOYSA-L 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VIFKLIUAPGUEBV-UHFFFAOYSA-N 2-(3-hydroxy-1h-indol-2-yl)-1h-indol-3-ol Chemical compound N1C2=CC=CC=C2C(O)=C1C1=C(O)C2=CC=CC=C2N1 VIFKLIUAPGUEBV-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 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 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The embodiment of the application discloses a cellulose fiber and a dyeing method thereof. The method comprises the steps of mixing strong alkali and sodium hydrosulfite in strong ammonia water to obtain a reducing solution; adding vat dye into the vat solution, reducing for 10-60min at 30-50 ℃, and cooling to room temperature to obtain vat dye solution; adding liquid ammonia into the reduction dye liquor to obtain liquid ammonia reduction dye liquor; immersing the cellulose fiber into the liquid ammonia vat dye solution for dyeing, and oxidizing and soaping in the air to obtain the dyed cellulose fiber. According to the application, the vat dye liquor prepared by the concentrated ammonia water can be easily mixed with the liquid ammonia in any proportion, the liquid ammonia vat dye liquor with different moisture contents can be easily prepared, and meanwhile, the liquid ammonia vat dye liquor contains moisture, so that strong alkaline conditions exist in the liquid ammonia vat dye liquor, the vat state of vat dye is maintained in dyeing, and the problem that the vat dye is oxidized in the dyeing process to cause fiber undyed is avoided.
Description
Technical Field
The application relates to the technical field of dyeing and finishing, in particular to a cellulose fiber and a dyeing method thereof.
Background
Indigo dye belongs to vat dye, and dyed cotton yarn and fabric are mainly used for jeans clothing. The indigo vat dye is insoluble in water, and needs to be reduced into soluble indigo leuco acid sodium salt under the condition of sodium hydrosulfite and alkaline agent in the dyeing process, then the soluble indigo leuco acid sodium salt permeates into cotton fibers, and then the soluble indigo leuco acid sodium salt is oxidized into the indigo vat dye and fixed in the cotton fibers. As the dye is contacted with oxygen in the air in the dyeing process, when the soluble sodium salt of the leuco indigo is not fully permeated, the soluble sodium salt of the leuco indigo is oxidized by the oxygen in the air and is fixed on the surface of the fiber. Especially, when indigo dyeing yarns, indigo vat dyes adhere to the yarn surface to form ring dyeings. Therefore, the indigo vat dye requires multiple dip-dyeing, i.e., multiple reduction and oxidation times, when dyeing cotton yarn, which increases the production cost.
Disclosure of Invention
Aiming at the defects of the prior art, the application provides a cellulose fiber and a dyeing method thereof, and aims to solve the problems of multiple procedures and high cost caused by repeated dip dyeing of indigo vat dye in the prior art.
In a first aspect, the present application provides a method of dyeing cellulosic fibres comprising:
mixing strong alkali and sodium hydrosulfite in strong ammonia water to obtain a reducing solution;
adding vat dye into the vat solution, reducing for 10-60min at 30-50 ℃, and cooling to room temperature to obtain vat dye solution;
adding liquid ammonia into the reduction dye liquor to obtain liquid ammonia reduction dye liquor;
immersing the cellulose fiber into the liquid ammonia vat dye solution for dyeing, and oxidizing and soaping in the air to obtain the dyed cellulose fiber.
Further, in the method for dyeing cellulose fibers, the ammonia content in the concentrated aqueous ammonia is 20-30%.
Further, in the dyeing method of cellulose fiber, the concentration of the strong alkali dissolved in the strong ammonia water is 10-60g/L; or/and (or)
The concentration of the sodium hydrosulfite dissolved in the concentrated ammonia water is 80-200g/L.
Further, in the dyeing method of the cellulose fiber, the concentration of the vat dye in the vat dye solution is 30-60g/L; or/and (or)
The vat dye includes an indigo vat dye.
Further, in the dyeing method of cellulose fibers, the volume ratio of the vat dye liquid to the liquid ammonia is (1-5): (15-19).
Further, in the dyeing method of cellulose fiber, the cellulose fiber comprises one or more of cotton fiber, fibrilia, viscose fiber and modal fiber.
Further, in the dyeing method of cellulose fiber, the morphological structure of the cellulose fiber is any one of loose fiber, yarn and fabric.
Further, in the dyeing method of cellulose fibers, the dyeing includes any one of dip dyeing and pad dyeing.
Further, in the dyeing method of cellulose fibers, the dyeing time is 1 to 10 minutes.
In a second aspect, the present application also provides a cellulosic fiber prepared by the dyeing process of the cellulosic fiber of the first aspect.
According to the cellulose fiber and the dyeing method thereof, the vat dye liquor prepared by the concentrated ammonia water can be easily mixed with the liquid ammonia in any proportion, so that the liquid ammonia vat dye liquor with different moisture contents can be easily prepared, meanwhile, the liquid ammonia vat dye liquor contains moisture, so that strong alkaline conditions exist in the liquid ammonia vat dye liquor, the vat state of vat dye can be maintained in dyeing, and the problem that the fiber is not dyed thoroughly due to oxidation of the vat dye in the dyeing process is avoided. In addition, the liquid ammonia vat dye liquor can quickly permeate into the fiber, dyeing can be quickly completed, and production time is saved. Meanwhile, the liquid ammonia containing a small amount of water has the functions of mercerizing and crystallizing the fiber, in the dyeing process of the liquid ammonia vat dye liquor, the amorphous area of the fiber is increased, the dye uptake of the dye is improved, namely the dyeing mercerizing is finished synchronously, and the liquid ammonia vat dye liquor contains a small amount of water, so that the stability and reproducibility of the dyeing effect are facilitated. Finally, the water consumption is small in the whole dyeing process, the dyeing amount is small, and the vat dye and the liquid ammonia are easy to recycle.
Detailed Description
The technical solutions of the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in the present specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
In view of the shortcomings in the prior art, the present application provides a method for dyeing cellulosic fibers, comprising:
mixing strong alkali and sodium hydrosulfite in strong ammonia water to obtain a reducing solution;
adding vat dye into the vat solution, reducing for 10-60min at 30-50 ℃, and cooling to room temperature to obtain vat dye solution;
adding liquid ammonia into the reduction dye liquor to obtain liquid ammonia reduction dye liquor;
immersing the cellulose fiber into the liquid ammonia vat dye solution for dyeing, and oxidizing and soaping in the air to obtain the dyed cellulose fiber.
Specifically, the application completes the indigo liquid ammonia vat dye solution by fully dissolving strong alkali, sodium hydrosulfite and indigo vat dye in concentrated ammonia water and then adding the solution into liquid ammonia after vat of the indigo vat dye. The yarn is immersed into indigo liquid ammonia vat dye solution for dyeing, then oxidized in air and soaped, so that the effect that the indigo can be thoroughly dyed and the yarn can be dyed in dark color by one-time dyeing is achieved.
According to the dyeing method of cellulose fibers, the vat dye liquor prepared by the concentrated ammonia water can be easily mixed with the liquid ammonia in any proportion, the liquid ammonia vat dye liquor with different moisture contents can be easily prepared, meanwhile, the liquid ammonia vat dye liquor contains moisture, so that strong alkaline conditions exist in the liquid ammonia vat dye liquor, the vat state of vat dye can be maintained in dyeing, and the problem that the vat dye is oxidized to cause the fiber to be not dyed thoroughly in the dyeing process is avoided.
In addition, the liquid ammonia vat dye liquor can quickly permeate into the fiber, dyeing can be quickly completed, and production time is saved. Meanwhile, the liquid ammonia containing a small amount of water has the functions of mercerizing and crystallizing the fiber, in the process of dyeing with the liquid ammonia vat dye liquor, the amorphous area of the fiber is increased, the dye uptake of the dye is improved, namely the dyeing mercerizing is finished synchronously, and the liquid ammonia vat dye liquor contains a small amount of water, so that the stability and reproducibility of the dyeing effect are facilitated. Finally, the water consumption is small in the whole dyeing process, the dyeing amount is small, and the vat dye and the liquid ammonia are easy to recycle.
In some embodiments, the ammonia content of the concentrated aqueous ammonia is 20-30%. Among them, the ammonia content in the concentrated aqueous ammonia is preferably 25%.
In some embodiments, the strong base is dissolved in concentrated aqueous ammonia at a concentration of 10-60g/L. Wherein the concentration of the strong base dissolved in the strong ammonia water is preferably 40g/L.
In some embodiments, the concentration of the sodium hydrosulfite dissolved in concentrated ammonia is 80-200g/L. Wherein, the concentration of the sodium hydrosulfite dissolved in the concentrated ammonia water is preferably 120g/L.
In some embodiments, the vat dye concentration in the vat dye solution is 30-60g/L. Wherein the concentration of vat dye in the vat dye solution is preferably 40g/L.
In some embodiments, the vat dyes mentioned herein are preferably indigo vat dyes.
In some embodiments, the volume ratio of the vat dye liquid to the liquid ammonia is (1-5): (15-19). Wherein, the volume ratio of the reduction dye liquor to the liquid ammonia is preferably 2:18.
in some embodiments, the cellulosic fibers comprise one or more of cotton fibers, hemp fibers, viscose fibers, modal fibers. Among them, the cellulose fiber is preferably cotton fiber.
In some embodiments, the morphology of the cellulosic fibers includes any of bulk fibers, yarns, fabrics. Among them, the morphology of the cellulose fiber is preferably yarn.
In some embodiments, the dyeing includes any one of dip dyeing and pad dyeing. Among them, the preferred dyeing method of the present application is dip dyeing.
In some embodiments, the staining time is 1-10 minutes. Among them, the dyeing time is preferably 3 minutes.
In some embodiments, the strong base comprises one or more of sodium hydroxide, potassium hydroxide, and the sodium hydrosulfite comprises sodium hydrosulfite.
In some embodiments, the present application also provides a cellulosic fiber prepared by the above-described method of dyeing cellulosic fibers.
The dyeing method of cellulose fibers according to the embodiments of the present application is exemplified by a number of specific examples.
Example 1
Slowly adding 1-6g of NaOH into 100mL of concentrated ammonia water (25% of ammonia content), adding 12g of sodium hydrosulfite, fully dissolving, adding 4g of indigo vat dye, heating to 40 ℃ while stirring, preserving heat for 30 minutes, fully reducing the indigo vat dye, and cooling to room temperature to finish the preparation of 40g/L of indigo ammonia water vat dye liquor.
Respectively taking 2mL of 40g/L indigo ammonia water reduction dye liquor containing different NaOH contents, adding liquid ammonia to 20mL, immersing 1g of cotton yarn into the dye liquor for 3 minutes, taking out the cotton yarn, oxidizing the cotton yarn in air for 10 minutes, and then washing the cotton yarn cleanly by soap, and airing the cotton yarn.
The K/S values of the dyed yarns were measured and the results are shown in Table 1. The cross section of the dyed fiber was observed with an optical microscope and was uniformly permeably dyed.
TABLE 1K/S values of yarn after dyeing with different NaOH contents (40 g/L indigo ammonia vat dye solution)
NaOH content (g) | 1 | 2 | 3 | 4 | 5 | 6 |
K/S value | 8.6 | 11.2 | 12.4 | 13.5 | 12.7 | 12.3 |
Example 2
Slowly adding 4g of NaOH into 100mL of concentrated ammonia water (25% of ammonia content), adding 8-20g of sodium hydrosulfite, fully dissolving, adding 4g of indigo vat dye, heating to 40 ℃ while stirring, preserving heat for 30 minutes, fully reducing the indigo vat dye, and cooling to room temperature to finish the preparation of 40g/L of indigo ammonia water vat dye liquor.
Respectively taking 2mL of 40g/L indigo ammonia water reduction dye liquor containing different sodium hydrosulfite contents, adding liquid ammonia to 20mL, immersing 1g of cotton yarn into the dye liquor for 3 minutes, taking out the cotton yarn, oxidizing the cotton yarn in air for 10 minutes, and then washing the cotton yarn cleanly by soap, and airing the cotton yarn.
The K/S values of the dyed yarns were measured and the results are shown in Table 2. The cross section of the dyed fiber was observed with an optical microscope and was uniformly permeably dyed.
TABLE 2K/S values of dyed yarns with different sodium hydrosulfite content
Sodium hydrosulfite content (g) | 8 | 10 | 12 | 14 | 16 | 20 |
K/S value | 8.9 | 11.3 | 13.5 | 13.1 | 12.8 | 12.2 |
Example 3
Slowly adding 4g of NaOH into 100mL of strong ammonia water (25% of ammonia content), adding 12g of sodium hydrosulfite, fully dissolving, adding 4g of indigo vat dye, heating to 40 ℃ while stirring, preserving heat for 30 minutes, fully reducing the indigo vat dye, and cooling to room temperature to finish the preparation of 40g/L indigo ammonia water vat dye solution.
Respectively taking 2mL of 40g/L indigo ammonia reduction dye liquor, adding liquid ammonia to 20mL, immersing 1g of cotton yarn into the dye liquor for 1-10 minutes, taking out the cotton yarn, oxidizing the cotton yarn in the air for 10 minutes, and then soaping the cotton yarn to be clean and airing the cotton yarn.
The K/S values of the dyed yarns were measured and the results are shown in Table 3. The cross section of the dyed fiber was observed with an optical microscope and was uniformly permeably dyed.
TABLE 3K/S values of yarn after dyeing at different times
Example 4
Slowly adding 4g of NaOH into 100mL of strong ammonia water (25% of ammonia content), adding 12g of sodium hydrosulfite, fully dissolving, adding 4g of indigo vat dye, heating to 40 ℃ while stirring, preserving heat for 30 minutes, fully reducing the indigo vat dye, and cooling to room temperature to finish the preparation of 40g/L indigo ammonia water vat dye solution.
And respectively taking 1-5mL of 40g/L indigo ammonia reduction dye liquor containing different sodium hydrosulfite contents, adding liquid ammonia to 20mL, immersing 1g of cotton yarn for dyeing for 13 minutes, taking out, oxidizing in air for 10 minutes, washing with soap, and airing.
The K/S values of the dyed yarns were measured and the results are shown in Table 4. The cross section of the dyed fiber was observed with an optical microscope and was uniformly permeably dyed.
TABLE 4K/S values of yarn after dyeing with different amounts of indigo ammonia vat dye
40g/L indigo ammonia reduction dye liquor (mL) | 1 | 2 | 3 | 4 | 5 |
K/S value | 6.8 | 13.5 | 13.4 | 13.0 | 12.4 |
Therefore, the application has the following remarkable technical effects due to the adoption of the technical scheme:
1. the reduction dye liquor prepared by the concentrated ammonia water can be easily mixed with the liquid ammonia in any proportion, and the liquid ammonia reduction dye liquor with different moisture contents can be easily prepared;
2. the liquid ammonia vat dye liquor has moisture, so that the liquid ammonia vat dye liquor has strong alkaline conditions, which is favorable for maintaining the vat state of the indigo vat dye in dyeing, and avoids the problem that the indigo vat dye is oxidized in the dyeing process to cause the fiber to be undyed;
3. the liquid ammonia vat dye liquor can quickly permeate into the fiber, can quickly finish dyeing, and saves production time;
4. the liquid ammonia containing a small amount of water still has the effects of mercerizing and crystallizing the fiber, and in the process of dyeing with the indigo liquid ammonia vat dye liquor, the amorphous area of the fiber is increased, and the dye uptake of the dye is improved, namely the dyeing mercerizing is finished synchronously;
5. the liquid ammonia vat dye liquor contains a small amount of water, which is favorable for the stability and reproducibility of dyeing effect;
6. the water consumption is small in the whole dyeing process, the dyeing amount is small, and the indigo vat dye and the liquid ammonia are easy to recycle.
While the application has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the application. Therefore, the protection scope of the application is subject to the protection scope of the claims.
Claims (10)
1. A method of dyeing cellulosic fibers, comprising:
mixing strong alkali and sodium hydrosulfite in strong ammonia water to obtain a reducing solution;
adding vat dye into the vat solution, reducing for 10-60min at 30-50 ℃, and cooling to room temperature to obtain vat dye solution;
adding liquid ammonia into the reduction dye liquor to obtain liquid ammonia reduction dye liquor;
immersing the cellulose fiber into the liquid ammonia vat dye solution for dyeing, and oxidizing and soaping in the air to obtain the dyed cellulose fiber.
2. The method for dyeing cellulose fibers according to claim 1, wherein the ammonia content of the concentrated aqueous ammonia is 20 to 30%.
3. The method for dyeing cellulose fibers according to claim 1, characterized in that the concentration of the strong base dissolved in the strong ammonia water is 10 to 60g/L; or/and (or)
The concentration of the sodium hydrosulfite dissolved in the concentrated ammonia water is 80-200g/L.
4. The method for dyeing cellulose fibers according to claim 1, characterized in that the concentration of vat dye in the vat dye solution is 30-60g/L; or/and (or)
The vat dye includes an indigo vat dye.
5. The method for dyeing cellulose fibers according to claim 1, characterized in that the volume ratio of the vat dye liquid to the liquid ammonia is (1-5): (15-19).
6. The method of dyeing cellulose fibers of claim 1, wherein the cellulose fibers comprise one or more of cotton fibers, hemp fibers, viscose fibers, modal fibers.
7. The method of dyeing cellulose fiber according to claim 6, wherein the morphology of the cellulose fiber is any one of bulk fiber, yarn, and fabric.
8. The method of dyeing cellulose fibers according to claim 1, wherein the dyeing comprises any one of dip dyeing and pad dyeing.
9. The method of dyeing cellulose fibers according to claim 1, wherein the dyeing time is 1 to 10 minutes.
10. Cellulose fiber, characterized in that it is produced by the dyeing method of cellulose fiber according to any one of claims 1 to 9.
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