CN111910452A - Pretreatment process for dyeing wool fabric by using acid dye and dyeing process - Google Patents

Pretreatment process for dyeing wool fabric by using acid dye and dyeing process Download PDF

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Publication number
CN111910452A
CN111910452A CN202010766458.3A CN202010766458A CN111910452A CN 111910452 A CN111910452 A CN 111910452A CN 202010766458 A CN202010766458 A CN 202010766458A CN 111910452 A CN111910452 A CN 111910452A
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Prior art keywords
wool fabric
wool
reducing agent
acid
acid dye
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CN202010766458.3A
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Chinese (zh)
Inventor
陈丽芬
何良
刘丽艳
夏芳芳
许宏
孙喜
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Jiangsu Sunshine Co Ltd
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Jiangsu Sunshine Co Ltd
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Priority to CN202010766458.3A priority Critical patent/CN111910452A/en
Publication of CN111910452A publication Critical patent/CN111910452A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/64General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65168Sulfur-containing compounds
    • D06P1/65181Compounds containing thiol groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/39General 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 acid dyes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/64General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/642Compounds containing nitrogen
    • D06P1/649Compounds containing carbonamide, thiocarbonamide or guanyl groups
    • D06P1/6495Compounds containing carbonamide -RCON= (R=H or hydrocarbons)
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/653Nitrogen-free carboxylic acids or their salts
    • D06P1/6533Aliphatic, araliphatic or cycloaliphatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/667Organo-phosphorus compounds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02Material containing basic nitrogen
    • D06P3/04Material containing basic nitrogen containing amide groups
    • D06P3/14Wool
    • D06P3/16Wool using acid dyes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P5/00Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/22Effecting variation of dye affinity on textile material by chemical means that react with the fibre

Abstract

The invention discloses an acid dye dyeing pretreatment process for wool fabrics, which comprises the following steps: s1: soaking the wool fabric in alkaline reducing solution mainly comprising a first reducing agent, lipoamide and water, heating, carrying out heat preservation reaction, washing with water and drying; s2: soaking the wool fabric obtained in the step S1 in an acidic grafting treatment solution mainly comprising an initiator, an acrylamide monomer and water, and after grafting reaction, soaping, washing and drying to obtain a treated wool fabric; the first reducing agent is tricarboxyethylphosphine and/or mercaptoethanol, and the temperature rise reaction temperature is 55-70 ℃; the pH value of the alkaline reducing solution is 8-9. In the acid dye dyeing pretreatment process of the wool fabric, the reconstruction of disulfide bonds occurs between wool fibers and lipoic acid and/or lipoamide under the reducing agent and alkaline conditions, and then acrylamide is grafted to the surface of wool, so that the dye uptake of the acid dye is further improved.

Description

Pretreatment process for dyeing wool fabric by using acid dye and dyeing process
Technical Field
The invention relates to the technical field of wool fabric production, in particular to an acid dye dyeing pretreatment process and a dyeing process for wool fabric.
Background
The wool fabric is dyed by acid dye or reactive dye. The acid dye has complete chromatogram and bright color, mostly belongs to aromatic sodium sulfonate, contains sulfonic acid group, hydroxyl group and other groups, and a small number of sodium carboxylate are ionized in water to form pigment acid ions which can be combined with amino or amido of wool fibers.
How to further improve the dye uptake of the acid dye is one of the technical problems to be solved by the technical personnel in the field. In the prior art, like in wool spinning science, 2011, volume 1, 3, phase 1, acrylamide grafted weight gain of wool and performance research, acrylamide is used as a wool grafted weight gain monomer, under a hydrogen peroxide/ascorbic acid redox system, primary alcohol groups exist on amino acid residues of wool fiber protein molecules, hydroxyl groups lose protons, and the primary alcohol groups are combined with acrylamide to generate graft copolymerization. As the number of amido bonds on the surface of the wool fiber is increased, and the amino groups are combined with hydrogen ions under acidic conditions to enable the fiber to have positive charges, more acid dye anions can be attracted to be combined by ionic bonds, the dye uptake of the acid dye to the wool fiber is improved, and the apparent color depth of the fabric grafted with acrylamide is improved in the appearance of the fabric.
In the dyeing reaction of the acid dye, the wool fiber and the dye are mainly combined by ionic bonds under the condition of strong acid, and are mainly combined by Van der Waals force and hydrogen bonds under the condition of weak acid, although the integral dye uptake of the grafted wool fabric is improved by the acid dye, the wetting property of the grafted mercerized wool is reduced, the diffusion and permeation of the dye into the fiber are influenced, and the improvement of the dye uptake is not favorable.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the acid dye dyeing pretreatment process for the wool fabric, and the pretreated wool fabric has good wetting property and is beneficial to further improving the dye uptake.
In order to achieve the technical effects, the technical scheme of the invention is as follows: an acid dye dyeing pretreatment process for wool fabrics comprises the following steps:
s1: soaking the wool fabric in alkaline reducing solution mainly comprising a first reducing agent and water, heating and carrying out heat preservation reaction, then adding lipoic acid and/or lipoamide into a reaction system, continuing the heat preservation reaction, washing with water and drying;
s2: soaking the wool fabric obtained in the step S1 in an acidic grafting treatment solution mainly comprising an initiator, an acrylamide monomer and water, performing a grafting reaction, and then washing with hot water and drying to obtain a treated wool fabric;
the first reducing agent is tricarboxyethylphosphine and/or mercaptoethanol, and the temperature rise reaction temperature is 55-70 ℃; the pH value of the alkaline reducing solution is 8-9. And (3) heating for reaction for 3-6 h, and continuing to perform heat preservation reaction for 2-3 h after lipoic acid and/or lipoamide are added. The bath ratio of the wool fabric to the alkaline reducing solution and the acidic grafting treatment solution is 1: (20-30).
In the presence of alkali and a reducing agent, opening a disulfide five-membered ring in a lipoic acid and/or lipoamide molecular structure, reconstructing generated sulfydryl and sulfydryl generated by the breakage of a disulfide bond on the surface of wool fibers, opening the lipoic acid and/or lipoamide to generate an alkyl chain with a sulfydryl branched chain, and carrying out a grafting reaction on acrylamide and hydroxyl and amino on the surface of the wool fibers. Partial sulfydryl is converted into sulfonic group in the fabric drying and grafting process, and the number of amino, carboxyl and the like of hydrophilic groups on the surface of the treated wool fiber is increased, so that the grafted wool is beneficial to dyeing of acid dye.
The preferable technical scheme is that the lipoamide is dropwise added into the reaction system in the S1. The end of the alkyl chain of the lipoamide contains amide, wool fibers can attract more dye negative ions to dye under the acid dyeing condition, and compared with the liponic acid pretreatment, the dyeing rate can be further improved.
The preferable technical scheme is that the initiator consists of an oxidant and a second reducing agent, the oxidant is persulfate, the second reducing agent is selected from sodium sulfite and/or ascorbic acid, and the pH value of the acidic grafting treatment solution is 1-2. The pH value is increased, and the grafting weight gain rate of the wool fabric is reduced.
The preferable technical scheme is that the dosage of the first reducing agent is 7-13% o.w.f. and the dosage of the lipoamide is 1-5% o.w.f. based on the weight of the wool fabric. The usage amount of lipoamide is too large, the quantity of the sulfonic acid groups on the surface of the wool obtained by the first step of drying is increased, the grafting rate of acrylamide can be reduced due to the steric hindrance of the sulfonic acid groups, and the introduction of amino groups and the improvement of the dye uptake are not facilitated.
The preferable technical scheme is that the dosage of the acrylamide monomer is 7-12% o.w.f. based on the weight of the wool fabric. If the dosage of the acrylamide monomer is too large, the grafting weight gain of the wool fibers is increased, which can cause the hand feeling of the wool fabrics to be hard, and the probability of covering hydrophilic groups by the grafted polyacrylamide is increased.
The preferable technical scheme is that the concentration of the oxidant and the concentration of the second reducing agent are both 20-25% based on 100% of the concentration of the acrylamide monomer.
The preferable technical scheme is that the temperature of the grafting reaction is 18-24 ℃, and the grafting reaction time is 3-6 h.
In order to remove residual acrylamide monomer in the wool fabric, the preferable technical scheme is that the heating washing temperature is higher than 75 ℃.
The second purpose of the invention is to provide an acid dye dyeing process for wool fabrics, which comprises the acid dye dyeing pretreatment process for the wool fabrics.
The invention has the advantages and beneficial effects that:
the acid dye dyeing pretreatment process for the wool fabric has reasonable steps, the disulfide bond between the wool fiber and the lipoic acid and/or the lipoamide is reconstructed under the reducing agent and the alkaline condition, then the acrylamide is grafted to the surface of the wool, and the hydrophilic group and the branched chain at the chain end in the molecular structure of the lipoic acid and/or the lipoamide are both beneficial to improving the wettability of the wool fiber, so that the dye uptake of the acid dye is improved.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The specifications of the wool fabric are as follows: full wool yarn knitted fabric, yarn fineness 15.7tex 2, size 50cm, fabric source: jiangsu sunshine group; acid dye: acid scarlet 3R, Tianjin Zhongjin chemical industry.
The dyeing process of the acid dye comprises the following steps: bath ratio of 1:20, soaking the fabric in 50 ℃ water for 15min, adding 2% o.w.f. dye and 4% o.w.f. acetic acid, heating to 95 ℃, keeping the temperature for 45min, washing with 50 ℃ warm water for 1 time, washing with cold water for 2 times, and drying.
Examples
Example 1
The acid dye dyeing pretreatment process for wool fabric of example 1 includes the following steps:
s1: soaking the wool fabric washed with the lanolin in alkaline reducing liquid mainly comprising mercaptoethanol and water at a bath ratio of 1:20, heating to 60-65 ℃, carrying out heat preservation reaction for 4 hours, then adding lipoic acid into the reaction system, continuing the heat preservation reaction for 3 hours, washing with water and drying; based on the weight of the wool fabric, the using amount of the first reducing agent is 7% o.w.f., the using amount of the lipoic acid is 2% o.w.f., and the pH value of the alkaline reducing solution is 9;
s2: soaking the wool fabric obtained in the step S1 in an acidic grafting treatment solution mainly comprising an initiator, an acrylamide monomer and water, wherein the bath ratio is 1:30, the temperature of the grafting reaction is 20-23 ℃, the grafting reaction time is 5 hours, and after the grafting reaction, the wool fabric is washed with water at the temperature of 75-80 ℃ and dried to obtain the treated wool fabric; in S2, the amount of acrylamide monomer is 7% o.w.f. based on the weight of the wool fabric; the initiator consists of an oxidant and a second reducing agent, wherein the oxidant is persulfate, and the second reducing agent is sodium sulfite; the concentration of the oxidant is 23% and the concentration of the second reducing agent is 20% based on the concentration of the acrylamide monomer as 100%; the pH of the acidic graft treatment solution was 1.5.
Example 2
Example 2 is based on example 1, with the difference that lipoamide is added dropwise to the reaction system in S1.
Example 3
Example 3 is based on example 2, with the difference that in S1 a composition of lipoamide and lipoic acid is added dropwise to the reaction system, the mass ratio of the two components being 1: 1.
Example 4
Example 4 is based on example 2, except that the pH of the basic reducing solution in S2 is 10.
Examples 5 to 6
Examples 5-6 are based on example 2 with the difference that example 5 uses 12% o.w.f. of the first reducing agent, 5% o.w.f. of the lipoamide, example 6 uses 12% o.w.f. of the first reducing agent and 8% o.w.f. of the lipoamide.
Examples 7 to 8
Examples 7-8 are based on example 2 except that in example 7 the second reducing agent is ascorbic acid and the oxidizing agent and the second reducing agent are both present at 25% concentration, based on 100% acrylamide monomer concentration; the concentrations of the oxidizing agent and sodium sulfite in example 8 were 30%.
Examples 9 to 10
Examples 9-10 are based on example 2 except that in S2 the acrylamide monomer is used in an amount of 12% o.w.f., based on the weight of the wool fabric; example 10 acrylamide monomer was used at 16% o.w.f.
Comparative example
The comparative example is based on example 1, and is characterized in that wool fabric washed to remove lanolin is soaked in alkaline reducing solution mainly composed of mercaptoethanol and water, the bath ratio is 1:20, the temperature is raised to 60-65 ℃, the reaction is carried out for 4 hours, and the wool fabric is washed and dried.
The results of the tests on the dyebaths and samples of the examples and comparative examples are as follows:
1. weighing the fabric before and after pretreatment, and calculating the grafting weight gain rate of the wool fabric;
2. testing the absorbance of the initial dye solution and the residual liquid by using a UV-3100PC ultraviolet spectrophotometer, and calculating the dye rate;
3. and (3) adopting a standard moisture regain to represent the moisture absorption performance of the fabric, and calculating the standard moisture regain: (W)Dipping in water-WDry matter)/WDry matter*100%。
The test results are given in the following table:
Figure BDA0002614810750000051
Figure BDA0002614810750000061
the amount of acrylamide grafted increases and the number of amino groups increases, but the increased amount of grafting also results in a slight decrease in the hydrophilic properties of the wool fabric, and therefore the dye uptake is affected by both of these factors. Comparative example S1 broke the scale layer and S2 grafted acrylamide.
The standard moisture regain of example 1, example 2, example 8 and example 9 is respectively 13.7%, 12.3%, 14.4% and 10.9%, the amount of acrylamide monomer is too large, the grafting amount is increased, the amino group on the surface of wool fiber is increased, but the moisture absorption performance of wool fabric is reduced, and the dye uptake is slightly increased; the increase of the dosage of the oxidant and the second reducing agent can lead more sulfydryl generated by the ring opening of the lipoic acid and/or the lipoamide to be oxidized into sulfonic group, so that the hydrophilic performance of the wool fabric is improved, but the self-polymerization of the acrylamide is increased, and the grafting rate is slightly reduced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. The acid dye dyeing pretreatment process of the wool fabric is characterized by comprising the following steps of:
s1: soaking the wool fabric in alkaline reducing solution mainly comprising a first reducing agent and water, heating and carrying out heat preservation reaction, then adding lipoic acid and/or lipoamide into a reaction system, continuing the heat preservation reaction, washing with water and drying;
s2: soaking the wool fabric obtained in the step S1 in an acidic grafting treatment solution mainly comprising an initiator, an acrylamide monomer and water, performing a grafting reaction, and then washing with hot water and drying to obtain a treated wool fabric;
the first reducing agent is tricarboxyethylphosphine and/or mercaptoethanol, and the temperature rise reaction temperature is 55-70 ℃; the pH value of the alkaline reducing solution is 8-9.
2. The process of claim 1, wherein S1 is prepared by adding lipoamide dropwise into the reaction system.
3. The acid dye dyeing pretreatment process of wool fabric according to claim 1, wherein the initiator is composed of an oxidant and a second reducing agent, the oxidant is persulfate, the second reducing agent is selected from sodium sulfite and/or ascorbic acid, and the pH value of the acid grafting treatment solution is 1-2.
4. The pretreatment process for dyeing wool fabric according to claim 2, wherein the first reducing agent is used in an amount of 7-13% o.w.f., and the lipoamide is used in an amount of 1-5% o.w.f., based on the weight of the wool fabric.
5. The pretreatment process for dyeing wool fabric according to claim 1, wherein the amount of the acrylamide monomer is 7-12% o.w.f. based on the weight of the wool fabric.
6. The process of claim 1, wherein the concentrations of the oxidizing agent and the second reducing agent are both 20-25% based on 100% acrylamide monomer.
7. The acid dye dyeing pretreatment process for wool fabrics according to claim 1, wherein the temperature of the grafting reaction is 18-24 ℃, and the grafting reaction time is 3-6 h.
8. The wool fabric acid dye pretreatment process according to claim 1, wherein the heated water washing temperature is higher than 75 ℃.
9. A wool fabric acid dye dyeing process, which is characterized by comprising the wool fabric acid dye dyeing pretreatment process according to any one of claims 1 to 8.
CN202010766458.3A 2020-08-03 2020-08-03 Pretreatment process for dyeing wool fabric by using acid dye and dyeing process Pending CN111910452A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1402761A (en) * 1999-10-01 2003-03-12 宝洁公司 Reactive dye compound
CN103582680A (en) * 2011-05-03 2014-02-12 巴斯夫欧洲公司 Disulfide dyes
CN105778556A (en) * 2016-03-29 2016-07-20 济南大学 Violet dye extracting method and dyeing application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1402761A (en) * 1999-10-01 2003-03-12 宝洁公司 Reactive dye compound
CN103582680A (en) * 2011-05-03 2014-02-12 巴斯夫欧洲公司 Disulfide dyes
CN105778556A (en) * 2016-03-29 2016-07-20 济南大学 Violet dye extracting method and dyeing application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈文等: ""羊毛的丙烯酰胺接枝增重及其性能研究"", 《毛纺科技》 *

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