CN113005795B - Method for preparing cationic dye dyeable polyamide fiber - Google Patents
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- CN113005795B CN113005795B CN202110337543.2A CN202110337543A CN113005795B CN 113005795 B CN113005795 B CN 113005795B CN 202110337543 A CN202110337543 A CN 202110337543A CN 113005795 B CN113005795 B CN 113005795B
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- 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
- D06P1/653—Nitrogen-free carboxylic acids or their salts
- D06P1/6533—Aliphatic, araliphatic or cycloaliphatic
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- 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
- D06P1/41—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 basic dyes
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- 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
- D06P1/653—Nitrogen-free carboxylic acids or their salts
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- 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
- D06P1/67375—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341 with sulfur-containing anions
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- 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
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/24—Polyamides; Polyurethanes
- D06P3/242—Polyamides; Polyurethanes using basic dyes
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- Textile Engineering (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
本发明公开了一种制备阳离子染料可染的锦纶纤维的方法，属于纺织材料技术领域。旨在通过醋酸进行锦纶纤维制品预处理，结合接枝硫辛酸、二硫键还原和氧化聚合反应，在锦纶纤维上引入较多羧基，提升锦纶纤维染色性能。具体步骤包括：(1)锦纶预处理；(2)纤维接枝硫辛酸；(3)硫辛酸还原处理；(4)氧化聚合和干燥处理。与传统碱法进行锦纶纤维改性引入负电性基团、实现阳离子染料染羊毛相比，本发明述及的改性方法生产能耗低、锦纶纤维损伤小，阳离子染料对纤维的可染性改善明显。The invention discloses a method for preparing cationic dye-dyeable nylon fiber, which belongs to the technical field of textile materials. The purpose is to pretreat nylon fiber products with acetic acid, and combine grafted lipoic acid, disulfide bond reduction and oxidative polymerization to introduce more carboxyl groups on nylon fibers to improve the dyeing properties of nylon fibers. The specific steps include: (1) nylon fiber pretreatment; (2) fiber grafting lipoic acid; (3) lipoic acid reduction treatment; (4) oxidative polymerization and drying treatment. Compared with the traditional alkali method for modifying nylon fibers to introduce negatively charged groups and dyeing wool with cationic dyes, the modification method described in the present invention has low production energy consumption, less damage to nylon fibers, and improved dyeability of fibers by cationic dyes. obvious.
Description
Technical Field
The invention relates to a method for preparing cationic dye dyeable polyamide fiber, and belongs to the technical field of textile materials.
Background
The most common dyes used in dyeing nylon fiber products comprise weak acid dyes, acid mordant-containing dyes, reactive dyes and the like. Wherein, the faintly acid dye has bright color, complete chromatogram and good level-dyeing property, and is widely applied to nylon dyeing; on the other hand, the weak acid dye and the polyamide fiber are mainly combined through hydrogen bonds and Van der Waals force, and belong to non-covalent bond combination, the dye is easy to fall off from the surface of the fiber during washing, and the wet treatment fastness of the dyed material is easy to reduce. In order to improve the color fastness of the polyamide fiber product, 1: the type 2 acid mordant-containing dye (also called neutral dye) is applied to dyeing. Compared with weakly acidic dyes, the neutral dye has a larger molecular structure and a larger affinity between the dye and the fiber, so that when the neutral dye is applied to dyeing of nylon fibers, the color depth and the color fastness of dyed materials are increased, but the color brightness is not enough, and the potential risk that the extractable heavy metal in the fiber products exceeds the standard exists to different degrees. In addition, the reactive dye is also applied to dyeing of the nylon fiber product, and the wet treatment fastness of the nylon fiber product can be improved by forming a covalent bond between the active group of the reactive dye and the amino group in the fiber; however, because the number of reactive amino groups in the nylon fiber is limited and only a small amount of amino groups are contained at the chain ends of macromolecules of the fiber, the nylon fiber has the defects of light color and low dye utilization rate when dyed by reactive dyes.
Compared with the dye, the cationic dye has the advantages of bright color, good washing fastness and light fastness, and the like, can be ionized to generate colored ions with positive charges after being dissolved in water, and can be used for dyeing fibers such as acrylic fibers containing electronegative groups, cationic dyeable terylene and the like. The cationic dye is rarely applied to nylon dyeing at present because the quantity of electronegative carboxyl groups in nylon fibers is small. In order to dye the nylon fiber by the cationic dye, more electronegative groups can be introduced into the nylon fiber by means of modification processing. Research shows that a certain amount of carboxyl can be introduced by hydrolyzing amido bonds in the polyamide fiber macromolecules, but the strength of the fibers is reduced easily due to improper control.
Disclosure of Invention
[ problem ] to provide a method for producing a semiconductor device
The technical problems to be solved in practice by the invention are as follows: provides a nylon fiber which has small fiber strength damage, can realize dyeability of cationic dye and has higher dyeing depth and color fastness.
[ technical solution ] A
In order to solve the problems, the invention firstly treats the polyamide fiber under a mild condition by virtue of acetic acid which has a hydrolysis effect on amido bonds in the polyamide fiber, so that the macromolecular surface of the polyamide fiber is hydrolyzed to generate a certain amount of amino groups; then, by taking newly added amino groups on the fiber as reaction anchor points, forming a reticular cross-linked structure containing more electronegative groups on the fiber through grafting and further polymerization reaction with carboxyl-containing micromolecules, increasing the electronegativity of the surface of the fiber, and realizing the modification processing of the cationic dye-dyeable polyamide fiber. Specifically, firstly, carrying out hydrolysis pretreatment on nylon fibers by virtue of acetic acid; then lipoic acid is grafted on the nylon fiber by means of 1-ethyl-3- (3-dimethylaminopropyl) -carbodiimide and N-hydroxysuccinimide; finally, lipoic acid grafted on fibrils and lipoic acid added in the system are reduced by sodium bisulfate, and after oxidative polymerization, a polymer which is connected by disulfide bonds and contains more carboxyl groups is formed on the surface of the nylon fiber, so that the modification processing of the nylon fiber which can be dyed by cations is realized. Compared with the method that only the amido bond in the chinlon is hydrolyzed to generate the electronegative group, the modification has small influence on the fiber strength, the introduction efficiency of the electronegative group is higher, and the dyeing depth of the cationic dye on the chinlon fiber is increased more obviously.
The first purpose of the invention is to provide a method for preparing cationic dye dyeable nylon fiber, which comprises the steps of pretreating the nylon fiber by using acetic acid, grafting lipoic acid on the nylon fiber under the condition of a cross-linking agent, adding a reducing agent and the lipoic acid into the nylon fiber grafted with the lipoic acid, and finally carrying out oxidative polymerization to obtain the cationic dye dyeable nylon fiber.
In one embodiment of the invention, the method comprises the steps of:
(1) pretreatment of nylon: pretreating a nylon fiber product by using acetic acid to hydrolyze fiber macromolecules to generate amino;
(2) fiber-grafted lipoic acid: after the nylon fiber product treated in the step (1) is washed, lipoic acid is grafted;
(3) and (3) lipoic acid reduction treatment: soaking the nylon fiber product treated in the step (2) in a mixed solution of a reducing agent and sodium lipoate for disulfide bond reduction treatment;
(4) oxidative polymerization and drying treatment: and (4) carrying out oxidative polymerization on the nylon fiber product treated in the step (3) in the air or by adopting an oxidant to obtain the cationic dye-dyeable nylon fiber.
In one embodiment of the present invention, the acetic acid pretreatment process recipe and conditions are as follows: acetic acid is 1-2.5 g/L, the temperature is 40-60 ℃, and the time is 0.5-1 hour.
In one embodiment of the invention, the crosslinking agent is 1-ethyl-3- (3-dimethylaminopropyl) -carbodiimide and N-hydroxysuccinimide.
In one embodiment of the present invention, the grafting process conditions in step (2): 2-5 g/L of 1-ethyl-3- (3-dimethylaminopropyl) -carbodiimide, 2-5 g/L of N-hydroxysuccinimide, 5-10 g/L of sodium lipoate, 20-30 ℃, 4.5-5.5 of pH value and 6-24 hours;
in one embodiment of the invention, the reducing agent comprises sodium sulfite and sodium borohydride.
In one embodiment of the present invention, the reduction treatment conditions are: 5-10 g/L of reducing agent, 15-30 g/L of sodium lipoate, 20-40 ℃, 6.5-8.5 of pH value and 0.5-1 hour of time.
In one embodiment of the invention, the oxidative polymerization conditions are: 0.2-0.5 g/L of hydrogen peroxide, 20-30 ℃ and 2-12 hours.
The second purpose of the invention is to provide a cationic dyeable fiber prepared by the method.
The third purpose of the invention is to provide a dyeing method of the nylon fiber dyeable by the cationic dye, the dyeing method is to dye the nylon fiber dyeable by the cationic dye by adopting the cationic dye, and the dyeing conditions are as follows: the cationic dye is 0.5-1 g/L, the dyeing temperature is 80-100 ℃, the pH is 4.0-6.0, and the dyeing time is 30-90 min.
A fourth object of the invention is to provide a fiber dyed by the above method.
It is a fifth object of the present invention to provide a textile product comprising the above cationic dyeable fiber or the above dyed fiber.
In one embodiment of the present invention, the textile includes any one of a conjugate fiber, a yarn, a carpet-like fabric, a woven fabric, a knitted fabric, a thermal wadding, a filling material, a nonwoven fabric, a garment, a clothing accessory, a home textile, a decoration, a medical hygienic article, or a special work garment.
The invention has the beneficial effects that:
according to the invention, the nylon fiber product is pretreated by acetic acid, grafting lipoic acid, disulfide bond reduction and oxidative polymerization are combined, more carboxyl groups are introduced on the nylon fiber, and the dyeing property of the nylon fiber is improved. Compared with the traditional modification method for realizing dyeability of cationic dyes by introducing electronegative carboxyl into polyamide fiber through hydrolysis by an alkaline method, the method has the following advantages:
(1) the production energy consumption is low. The steps (1) to (4) of the dyeable nylon fiber cationic dye modification processing are all carried out under the conditions of low temperature and near neutrality, and the method has the characteristic of low production energy consumption.
(2) The fiber damage is small. After lipoic acid is grafted on the surface of the nylon fiber, covalent crosslinking based on disulfide bond interconnection can be formed at different sites in fiber macromolecules or among molecules by combining disulfide bond reduction and oxidative polymerization, so that the strength of the fiber is increased to a certain extent and is increased by 2-2.5% compared with that of an untreated sample after dyeing;
(3) the dyeing property is obviously improved, after the nylon fiber product is modified by the method, the affinity to cationic dye is increased, the dyeing depth K/S of the nylon fiber product is increased by 3.5-4.5 compared with that of an untreated sample, and the color fastness is improved by 0.5 level.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
The dyeing depth K/S value (color measuring condition: D65 light source, 10 degree visual field) of the nylon fiber product is measured by adopting a color measuring instrument, the wet rubbing fastness of the dyed fiber product is measured by referring to GB/T3920-.
Example 1:
the nylon 6 filament woven fabric is modified by the process and the method of the invention in steps (1) to (4), and finally, the sample is dyed by cationic dye according to the step (5) described below.
(1) Pretreatment of nylon: pretreating a sample by using acetic acid to generate amino on the fiber; the pretreatment process formula and conditions are as follows: 1g/L of acetic acid, 0.5g/L of penetrating agent and 0.5 hour of treatment at 40 ℃;
(2) fiber-grafted lipoic acid: washing the sample treated in the step (1) with water and grafting lipoic acid; the grafting process formula and conditions are as follows: 2g/L of 1-ethyl-3- (3-dimethylaminopropyl) -carbodiimide, 2g/L of N-hydroxysuccinimide, 5g/L of sodium lipoate, 20 ℃ of temperature and 4.5 of pH value, and treating for 6 hours;
(3) and (3) lipoic acid reduction: dipping the sample treated in the step (2) in a mixed solution of sodium sulfite and sodium lipoate for reduction treatment; reduction treatment recipe and conditions: 5g/L of sodium sulfite, 15g/L of sodium lipoate, 20 ℃ of temperature, 6.5 of pH value and 0.5 hour of treatment;
(4) oxidative polymerization and drying treatment: soaking the sample treated in the step (3) in hydrogen peroxide solution for oxidative polymerization, washing with water, and drying at 60 ℃; oxidative polymerization formula and conditions: 0.2g/L of hydrogen peroxide, 20 ℃ and 2 hours of treatment.
(5) Dyeing with cationic dye: and (4) dyeing the sample treated in the step (4) by using cationic red X-GRL (red-dye for 1 hour, washing the sample with water and drying the sample after dyeing.
Example 2
The nylon 66 filament knitted fabric is modified by the process and the method of the invention in the steps (1) to (4), and finally, the sample is dyed by cationic dye according to the step (5).
(1) Pretreatment of nylon: pretreating a sample by using acetic acid to generate amino on the fiber; the pretreatment process formula and conditions are as follows: 2.5g/L of acetic acid and 1.5g/L of penetrating agent, and treating for 1 hour at 60 ℃;
(2) fiber-grafted lipoic acid: washing the sample treated in the step (1) with water and grafting lipoic acid; the grafting process formula and conditions are as follows: 5g/L of 1-ethyl-3- (3-dimethylaminopropyl) -carbodiimide, 5g/L of N-hydroxysuccinimide, 10g/L of sodium lipoate, 30 ℃ of temperature and 5.5 of pH value, and treating for 24 hours;
(3) and (3) lipoic acid reduction: immersing the sample treated in the step (2) in a mixed solution of sodium borohydride and sodium lipoate for reduction treatment; reduction treatment recipe and conditions: 10g/L of sodium borohydride, 30g/L of sodium lipoate, 40 ℃ of temperature and 8.5 of pH value, and treating for 1 hour;
(4) oxidative polymerization and drying treatment: soaking the sample treated in the step (3) in hydrogen peroxide solution for oxidative polymerization, washing with water, and drying at 60 ℃; oxidative polymerization formula and conditions: 0.5g/L of hydrogen peroxide, 30 ℃ and 12 hours of treatment.
(5) Dyeing with cationic dye: and (3) washing the sample treated in the step (2) with water, and dyeing with cationic brilliant blue RL, wherein the cationic brilliant blue RL is 0.6g/L, the leveling agent is 0.25g/L, the temperature is 95 ℃, the pH value is 5.5, and washing and drying the sample after dyeing for 1 hour.
Comparative example 1:
the treatment in example 1 was not conducted in steps (1) to (4), and the other conditions and parameters were the same as those in example 1.
Comparative example 2:
the process of example 1 was not conducted through steps (3) and (4), and the other conditions or parameters were the same as those of example 1.
Comparative example 3:
the sodium lipoate was not added in step (3) of example 1, and the other conditions or parameters were the same as those of example 1.
Comparative example 4:
the treatment in example 2 was not conducted in steps (1) to (4), and the other conditions or parameters were the same as those in example 2.
Comparative example 5:
the process of example 2 was not conducted through the steps (3) and (4), and the other conditions or parameters were the same as those of example 2.
Comparative example 6:
the sodium lipoate was not added in step (3) of example 2, and the other conditions or parameters were the same as those of example 2.
The dyeing depth, wet rubbing fastness and the strength change rate of the nylon fabrics in examples 1 to 3 and comparative examples 1 to 6 relative to an untreated sample were measured to obtain data in table 1.
TABLE 1
As can be seen from Table 1:
a. the samples (examples 1 and 2) modified by the method of the invention before dyeing have greatly increased color depth and increased sample strength compared with untreated samples, which shows that after the lipoic acid grafted on the nylon fiber and the lipoic acid added in the system are reduced, the sulfhydryl groups which can be reduced in oxidation can be mutually polymerized, and the reticular macromolecules with disulfide bonds which are mutually connected and contain more carboxyl groups on the branched chains are formed on the surface of the fiber. The lipoic acid grafted at different sites on the fiber can be mutually connected through polymerization, so that the breaking or bursting strength of the fabric is improved. Therefore, the method for modifying the polyamide fiber can increase the dye uptake of cationic dye, obtain higher color depth and color fastness and obviously improve the strength of the sample.
b. The K/S values of the samples without any treatment before dyeing (comparative example 1, comparative example 4) were lower, and the fabric strength was not significantly changed from that of the untreated samples;
c. the K/S value of the sample (comparative example 2 and comparative example 5) which is only treated by acetic acid before dyeing is similar to the color depth of the untreated sample, but the strength of the sample is slightly reduced, which shows that the acetic acid pretreatment has a certain hydrolysis effect on the polyamide fiber;
d. when the sodium lipoate is not added during the reduction in the step (3) of the example, the K/S value of the sample is not increased significantly and the strength is reduced compared with that of the untreated sample from the comparison examples 3 and 6, which shows that the processing effect is different from the example. The reason is that if sodium lipoate is not added in the reduction process, the nylon fiber can only be reduced to show that the grafted lipoic acid generates sulfydryl, and if the intermolecular distance of the grafted lipoic acid is far, the reduction product can not form connection between lipoic acids at different sites in the oxidation process, so that the lipoic acid is added in the reduction solution, a polymerization structure can be formed between the lipoic acid reduction products grafted on the fiber in the oxidation process, the formation of a network structure containing more lipoic acid is gradually shown, and the strength of the fabric can also be obviously improved.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
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