CN110344264B - Super-hydrophobic anti-ultraviolet cotton fabric dyeing method - Google Patents

Super-hydrophobic anti-ultraviolet cotton fabric dyeing method Download PDF

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CN110344264B
CN110344264B CN201910704665.3A CN201910704665A CN110344264B CN 110344264 B CN110344264 B CN 110344264B CN 201910704665 A CN201910704665 A CN 201910704665A CN 110344264 B CN110344264 B CN 110344264B
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cotton fabric
dyeing
dye
super
hydrophobic
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CN110344264A (en
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祁珍明
王矿
沈雪婷
钱宽豪
夏思远
张�成
莫年格
王春霞
季萍
马志鹏
高大伟
刘丽
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Zhu Qunyi
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Yancheng Institute of Technology
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/17—Halides of elements of Groups 3 or 13 of the Periodic Table
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46—Compounds containing quaternary nitrogen atoms
    • D06M13/463—Compounds containing quaternary nitrogen atoms derived from monoamines
    • 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
    • D06P1/655—Compounds containing ammonium groups
    • D06P1/66—Compounds containing ammonium groups containing quaternary ammonium groups
    • 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
    • D06P1/67341—Salts or hydroxides of elements different from the alkaline or alkaline-earth metals or with anions containing those elements
    • 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
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Coloring (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a dyeing method of a super-hydrophobic anti-ultraviolet cotton fabric, which comprises the steps of preparing a modified solution and modifying the cotton fabric; adding a dye and a mordant into the modified solution, and dyeing the modified cotton fabric to obtain a dyed cotton fabric; alternately padding the dyed cotton fabric in the mordant and the cross-linking agent for several times; soaking in waterproof finishing agent, cleaning, and padding; drying and baking to obtain the super-hydrophobic anti-ultraviolet dyed cotton fabric; wherein, the preparation modified solution is prepared by using a cation modifier and NaOH; the mordant is lanthanum chloride, the dye is a natural plant dye, the cross-linking agent is phytic acid, and the waterproof finishing agent is YC 560. The contact angle degree of the prepared cotton fabric is more than or equal to 154 degrees, the UPF value is more than or equal to 58, and the cotton fabric is washable and friction-resistant.

Description

Super-hydrophobic anti-ultraviolet cotton fabric dyeing method
Technical Field
The invention belongs to the technical field of spinning, and particularly relates to a method for dyeing super-hydrophobic ultraviolet-resistant cotton fabrics.
Background
In addition, at present, most methods for preparing the super-hydrophobic fabric still have a series of problems that the experimental conditions are harsh, the steps are complicated and the like, and the structural strength between the surface of the carrier and the super-hydrophobic surface layer is low for preparing the super-hydrophobic material on the market at present; the super-hydrophobic surface layer with low strength falls off, so that the hydrophobic capacity is greatly reduced, and the service life is very short.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned technical drawbacks.
Therefore, as one aspect of the invention, the invention overcomes the defects in the prior art and provides a method for dyeing super-hydrophobic ultraviolet-resistant cotton fabrics.
In order to solve the technical problems, the invention provides the following technical scheme: a dyeing method of super-hydrophobic ultraviolet-resistant cotton fabric comprises the steps of preparing a modified solution and modifying the cotton fabric; adding a dye and a mordant into the modified solution, and dyeing the modified cotton fabric to obtain a dyed cotton fabric; alternately padding the dyed cotton fabric in the mordant and the cross-linking agent for several times; soaking in waterproof finishing agent, cleaning, and padding; drying and baking to obtain the super-hydrophobic anti-ultraviolet dyed cotton fabric; wherein, the preparation modified solution is prepared by using a cation modifier and NaOH; the mordant is lanthanum chloride, the dye is a natural plant dye, the cross-linking agent is phytic acid, and the waterproof finishing agent is YC 560.
As a preferred scheme of the super-hydrophobic ultraviolet-resistant cotton fabric dyeing method, the method comprises the following steps: the cationic modifier is 2, 3-epoxypropyl trimethyl ammonium chloride, and the dye is gardenia yellow dye.
As a preferred scheme of the super-hydrophobic ultraviolet-resistant cotton fabric dyeing method, the method comprises the following steps: preparing a modified solution, namely modifying a cotton fabric, wherein the bath ratio is 50:1, the modified solution is prepared by using a cationic modifier with the concentration of 30-50 g/L and NaOH with the concentration of 10-30 g/L, and the cotton fabric is subjected to oscillation for 30-70 min at the temperature of 50-90 ℃.
As a preferred scheme of the super-hydrophobic ultraviolet-resistant cotton fabric dyeing method, the method comprises the following steps: adding a dye and a mordant into the modified solution to dye the modified cotton fabric, wherein the dye and the mordant accounting for 3% of the modified solution by mass are added, dyeing is carried out for 10min at normal temperature, heating to 95 ℃, keeping the temperature for 30-70 min, and washing with water.
As a preferred scheme of the super-hydrophobic ultraviolet-resistant cotton fabric dyeing method, the method comprises the following steps: and alternately padding the dyed cotton fabric in the mordant and the cross-linking agent for several times, wherein the mangling liquor ratio is controlled to be 65-85%, padding the dyed cotton fabric in the mordant, then padding the dyed cotton fabric in the cross-linking agent, and the padding time is more than or equal to 9 times.
As a preferred scheme of the super-hydrophobic ultraviolet-resistant cotton fabric dyeing method, the method comprises the following steps: and soaking in a waterproof finishing agent, cleaning and padding, wherein the step of soaking in 30-50 g/L of the waterproof finishing agent for 30 minutes is to clean and pad once.
As a preferred scheme of the super-hydrophobic ultraviolet-resistant cotton fabric dyeing method, the method comprises the following steps: and drying and baking the cotton fabric after drying, namely drying the cotton fabric for 30 minutes at 65-85 ℃, taking out the cotton fabric, heating the cotton fabric to 100-140 ℃, and baking the cotton fabric for 0.8-2.6 minutes.
In one aspect of the present invention, the present invention overcomes the disadvantages of the prior art and provides a super-hydrophobic ultraviolet-resistant dyed cotton fabric, wherein: the contact angle degree is 154 DEG or more and the UPF value is 58 or more.
The invention has the beneficial effects that:
the dyed cotton fabric prepared by the method has super-hydrophobic and anti-ultraviolet capabilities and is firm in color.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
figure 1 is a process diagram for dyeing cotton fabric.
FIG. 2 is a graph of the effect of modifier concentration on the depth of dye uptake of cotton.
FIG. 3 is the effect of NaOH concentration on the depth of staining of cotton.
FIG. 4 is the effect of modification temperature on the depth of dye uptake of cotton.
FIG. 5 is the effect of modification time on the depth of stain on cotton.
FIG. 6 is a graph showing the effect of lanthanum chloride dosage on the depth of dye uptake of cotton.
FIG. 7 is a graph showing the effect of incubation time on the depth of staining of cotton.
FIG. 8 is a graph showing the effect of dip times on contact angle.
FIG. 9 is a graph showing the effect of the number of impregnations on the UPF value.
FIG. 10 is a graph of the effect of immersion time on contact angle.
FIG. 11 is a graph showing the effect of immersion time on UPF value.
FIG. 12 is a graph showing the effect of lanthanum chloride ion concentration on contact angle.
FIG. 13 is a graph of the effect of lanthanum chloride ion concentration on UPF values.
FIG. 14 is a graph showing the effect of phytic acid solution concentration on the contact angle.
FIG. 15 is a graph showing the effect of concentration of phytic acid solution on UPF values.
FIG. 16 is a graph of the effect of mangle ratio on contact angle.
FIG. 17 is a graph of the effect of mangle ratio on UPF values.
FIG. 18 is a graph showing the effect of the number of soaping on the contact angle.
FIG. 19 is a graph showing the effect of number of soaping on UPF value.
FIG. 20 is a graph of the effect of rubbing times on contact angle.
FIG. 21 is a graph of the effect of friction number on UPF value.
FIG. 22 is an SEM examination of dyed cotton fabric, wherein A and B are cotton fabrics that have not been experimentally treated at two and three thousand times magnification; c and D are detection diagrams of cotton fabrics amplified by two thousand times and three thousand times after experimental treatment.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
1) cationic modification of cotton fabric
According to a bath ratio of 50:1, sucking a cationic modifier (2, 3-epoxypropyltrimethylammonium chloride) solution with the concentration of 30-70 g/L, dripping the cationic modifier solution into a conical flask, and weighing NaOH with the concentration of 10-30 g/L to prepare a modifier solution with a corresponding volume. And (3) putting 2g of pure cotton cloth sample into the prepared solution, putting the pure cotton cloth sample into a normal-temperature oscillation dyeing machine, oscillating for 40min at 50-90 ℃, taking out the cloth sample, fully washing the cloth sample with deionized water, removing the redundant modifier solution on the surface of the cloth sample, and finally putting the cloth sample into an oven for drying.
2) Dyeing cotton fabric
Preparing a dyeing solution: adding 3% of gardenia yellow dye (accounting for the mass fraction of the modifier solution, the same below) and 0.5-2.5% of lanthanum chloride into the modifier solution used in the step 1), mixing, pouring the mixture into a dyeing cup, dyeing by using an IR12SM type infrared rapid color testing machine, and measuring the K/S value of the mixture.
The process curve for dyeing the cotton fabric is as follows, wherein the heat preservation is carried out for 10-50 min at 95 ℃.
The detection method of the dyed cotton fabric comprises the following specific steps:
and (3) rubbing fastness test: shearing a sample of which the length direction is not less than 5cm multiplied by 20cm from the dyed fabric to be detected according to the warp direction or the weft direction; in addition, 5cm multiplied by 5cm of pure cotton bleached plain cloth is cut and used for a circular friction head of a tester; color fastness rating: the crocking fastness was assessed in a standard light box using a staining gray sample card.
(1) And (3) determining dry rubbing fastness: the sample is fixed on the bottom plate of the tester, the length direction of the sample is consistent with the moving direction of the tester, and the sample is tightly pressed by a clamping device. And fixing a 5cm multiplied by 5cm dry bleaching plain cloth on a friction head, wherein the warp and weft directions are straight with the warp and weft directions of the dyed sample. The rubbing head is put down, the power switch is turned on, the start button is pressed, and the rubbing head reciprocates 10 times on the sample fabric. The rubbing head was lifted, the sample and bleached plain cloth were removed, and ready for rating.
(2) Testing wet rubbing fastness: the bleached plain cloth (5cm x 5cm) is soaked and rolled on a roller of a rubbing fastness instrument in advance, and the liquid carrying rate is about 70 percent. Then fixing it on a friction head to carry out friction fastness measurement by the same method as the above. And (4) after the friction is finished, taking down the sample and the bleached plain cloth, and drying the wet cloth at the temperature of below 60 ℃. A rating is prepared.
Soaping color fastness test: according to the experimental method of GB/T3921-2008 'color fastness to soaping of textile color fastness', a dyed fabric sample and a specified lining fabric are sewn together, soap and anhydrous sodium carbonate are put into the fabric sample, mechanical stirring is carried out at a specified time and temperature, then cleaning and drying are carried out, and the color change of the fabric or the staining of the lining fabric is evaluated by using a gray sample card. Conditions are as follows: 5g/L of soap chips. The temperature is 40 ℃, the bath ratio is 50:1, and the time is 30 min.
FIG. 2 shows the effect of the concentration of the modifier on the dyeing depth of cotton, wherein the dyeing liquor is prepared according to the concentration of NaOH of 15g/L, the dye consumption of 3 percent, the lanthanum chloride of 1 percent and the bath ratio of 50:1, and under the condition that other conditions are not changed, when the concentration of the modifier is 50g/L, the dyeing depth of cotton on gardenia yellow is the highest. FIG. 3 shows the effect of NaOH concentration on the dyeing depth of cotton, and analysis shows that the dye liquor is prepared according to the concentration of a modifier of 50g/L, the dye dosage of 3 percent, the lanthanum chloride of 1 percent and the bath ratio of 50:1, and under the condition of no change of other conditions, when the NaOH concentration is 10g/L, the dyeing depth of cotton dyed by gardenia yellow is the highest. FIG. 4 shows the effect of modification temperature on the depth of dyeing of cotton, modified at different temperatures according to the concentration of the modifier 50g/L and the concentration of NaOH 10 g/L. 3% of dye, 1% of lanthanum chloride, and a bath ratio of 50:1, wherein the dye liquor is prepared, and the top dyeing depth of cotton is the highest when the modification temperature is 70 ℃ under the condition that other conditions are not changed. FIG. 5 shows the influence of modification time on the dyeing depth of cotton, wherein the modification is carried out at 70 ℃ for different lengths of time according to the concentration of a modifier of 50g/L and the concentration of NaOH of 10g/L, the dye consumption is 3%, the lanthanum chloride is 1%, and the dyeing liquor prepared according to the bath ratio of 50:1 is unchanged under other conditions, and when the modification time is 30min, the dyeing depth of cotton dyed by gardenia yellow is the highest. FIG. 6 shows the influence of the usage amount of lanthanum chloride on the dyeing depth of cotton, dye liquor is prepared according to the concentration of a modifier of 50g/L, the concentration of NaOH of 15g/L, the usage amount of dye of 3 percent and the bath ratio of 50:1, under the condition that other conditions are not changed, the lanthanum chloride has the dyeing promotion effect on gardenia yellow-dyed cotton fabrics, but after the mass fraction of the lanthanum chloride exceeds 1 percent, the effect is not obviously improved, so that the mass fraction of the mordant lanthanum chloride is 1 percent. FIG. 7 shows the effect of holding time on the depth of dyeing of cotton, according to the concentration of the modifier of 50g/L, NaOH of 10g/L, the modification temperature of 70 ℃ and the modification time of 30 min. 3% of gardenia yellow, 1% of lanthanum chloride and a bath ratio of 50:1, after dyeing for 40min at normal temperature, cooling to 95 ℃, preserving heat and dyeing the fabric, preserving heat for 30min to achieve better dyeing, and through the test of a color fastness tribometer and a color fastness to washing tester, the dry rubbing fastness can reach 3 level, the wet rubbing fastness can reach 3 level, and the color fastness to washing can reach 3.5 level.
Example 2:
1) cationic modification of cotton fabric
According to the bath ratio of 50:1, sucking a cationic modifier (2, 3-epoxypropyltrimethylammonium chloride) solution with the concentration of 50g/L and dripping the solution into a conical flask, and then weighing NaOH with the concentration of 10g/L to prepare a modifier solution with the corresponding volume. And (3) putting 2g of pure cotton cloth sample into the prepared solution, putting the pure cotton cloth sample into a normal-temperature oscillation dyeing machine, oscillating for 30min at 70 ℃, taking out the cloth sample, fully washing the cloth sample with deionized water, removing the redundant modifier solution on the surface of the cloth sample, and finally putting the cloth sample into an oven for drying.
2) Dyeing cotton fabric
Preparing a dyeing solution: adding 3 percent of gardenia yellow dye (accounting for the mass fraction of the modifier solution, the same below) and 1 percent of lanthanum chloride into the modifier solution used in the step 1), mixing, and dyeing the cotton fabric according to the process curve of example 1, wherein the temperature is kept at 95 ℃ for 30 min.
3) Carrying out hydrophobic treatment on cotton fabric:
soaking a dyed cotton fabric of 7 multiplied by 5cm in phytic acid aqueous solution (1-3 mL0.010-0.050 mol/L70 wt% phytic acid solution measured by a pipette is added into 99mL deionized water to prepare the phytic acid solution) for 1-10 minutes, controlling the pressure of a padder by using the padder to enable the cotton fabric to be padded once at a padder rate of about 65% -85%, soaking the cotton fabric in 40 mL0.01-0.035 mol/L LaCl3.7H2O metal ion solution, then padding the cotton fabric by using the padder, repeatedly soaking the cotton fabric in the phytic acid solution for several times, and then soaking the cotton fabric in La metal ion water; after the steps are repeated, the cotton fabric is washed by deionized water and then padded once by using a padder, then the cotton fabric is put into 30-50 g/L waterproof finishing agent YC560 (purchased from Jiaxing silver City Fine chemical Co., Ltd.) to be soaked for 30 minutes and then washed by the deionized water, after washing and then padded once by using the padder, the cotton fabric is put into a constant temperature drying oven with the temperature of 120 ℃ for 30 minutes, then the cotton fabric is taken out, the temperature of the constant temperature drying oven is raised to 100-140 ℃, and then the cotton fabric is put into baking for 0.8-2.6 minutes.
Taking out the product to carry out a performance test,
and (3) testing ultraviolet resistance: the YG (B)912E type textile ultraviolet resistance tester manufactured by Wenzhou Darong textile instruments Co., Ltd is used, and the standard selected during measurement is GB/T18830-.
And (3) testing the super-hydrophobic property: the contact angle measuring instrument produced by the Shanghai morning mathematical technology equipment company Limited is used, and the observation error caused by the uneven surface of the cotton fabric can be greatly reduced by using the angle measurement method for measurement.
Results 1: under the experimental conditions that the concentration and volume of metal ion water are 40mL and 0.01 mol/LLaCl3.7H2O, the specification of phytic acid solution is 100mL0.0095mol/L, the dipping time is 2 minutes, the mangle ratio is 85%, the dosage of yc560 waterproof finishing agent is 30g/L, the baking temperature is 120 ℃, and the baking time is 2 minutes, the influence of the dipping times on the contact angle and the ultraviolet resistance is respectively obtained as shown in figures 8 and 9. As can be seen from the two graphs, the contact angle is maximum when the number of times of the experiment is the ninth, and the ultraviolet protection coefficient reaches the maximum when the number of times of the experiment is the ninth, so that the best effect can be achieved when the number of times of the experiment is repeated when the number of times of the experiment is the ninth.
Results 2: determining that the dipping times are nine times, the concentration and the volume of the metal ion water are 40mL and the concentration and the volume of the metal ion water are 0.01 mol/LLaCl3.7H2O; the specification of the phytic acid solution is 100mL and 0.0095 mol/L; the mangle yield is about 85 percent; the dosage of the yc560 waterproof finishing agent is 30 g/L; baking temperature 120 ℃ baking time 2 minutes, and the measured contact angle number and UPF value after adjusting the dipping time are shown in fig. 10 and 11, respectively. From the two figures, the contact angle reaches the maximum value of 130 degrees after 2min, and the ultraviolet protection coefficient reaches the maximum value of 28.1 degrees after 4min, so that the conclusion is drawn that the best effect can be achieved when the padding time is 4 min.
Results 3: determining the padding times to be nine times; the specification of the phytic acid solution is 100mL and 0.0095 mol/L; the mangle yield is about 85 percent; the soaking time is 4 min; the dosage of the yc560 waterproof finishing agent is 30 g/L; the experiment is carried out by changing the concentration of La ions in metal ion water for 2 minutes at the baking temperature of 120 ℃, the following two figures 12 and 13 are respectively obtained after measuring the contact angle and the UPF value again, the contact angle of the fabric can reach a maximum value of 142 ℃ when the concentration of the metal ion solution is 0.02mol/L, and the peak value of 38+ when the protection coefficient of ultraviolet rays is 0.015mol/L, the contact angle of the fabric is increased, and the superhydrophobic property of the cotton fabric is obviously improved.
Results 4: determining that the padding times are nine times, and the concentration and the volume of the metal ion water are 40mL and are 0.02 mol/LLaCl3.7H2O; changing the concentration of the phytic acid solution by changing the volume of the measured phytic acid; the dosage of the yc560 waterproof finishing agent is 30 g/L; the mangle yield is about 85 percent; the baking temperature is 120 ℃, the baking time is 2 minutes, the concentration of the phytic acid solution is changed by changing the volume of the measured phytic acid for carrying out experiments, and the superhydrophobicity and the uvioresistant performance of the phytic acid solution are continuously measured after finishing, so that the following two figures 14 and 15 are respectively obtained. From the figure, the cotton fabric achieves a contact angle close to 148 degrees when 2mL, namely 100mL of 0.038mol/L phytic acid solution is measured, and the anti-ultraviolet protection coefficient also achieves 52+ to achieve an anti-ultraviolet effect.
Results 5: determining the padding times to be nine times; the soaking time is 4 min; the concentration and volume of the metal ion water are 40mL and are 0.01 mol/LLaCl3.7H2O; the specification of the phytic acid solution is 100mL and 0.038 mol/L; the dosage of the yc560 waterproof finishing agent is 30 g/L; the baking temperature is 120 ℃, the baking time is 2 minutes, the mangle ratio is changed by changing the pressure of a mangle bar of a small padder, and the superhydrophobicity and the uvioresistant performance of the material are continuously tested after the experimental finishing to respectively obtain figures 16 and 17. Through observation of the upper graph, we surprisingly find that at the moment, when the mangle expression is controlled to be 65-70%, the fabric contact angle already achieves a 152 DEG + superhydrophobic effect, the ultraviolet protection coefficient also achieves a good performance of 58+, the mangle expression of the fabric in the experimental finishing process is reduced to enable the cotton fabric to adsorb more metal ions and phytic acid as far as possible, the formed membrane structure on the surface is firmer, and the superhydrophobic and ultraviolet protection effects are better. Through the test of a color fastness tribometer and a color fastness to washing tester, the dry rubbing fastness can reach 4 grades, the wet rubbing fastness can reach 3 grades, and the color fastness to washing can reach 4 grades.
Example 3:
1) cationic modification of cotton fabric
According to the bath ratio of 50:1, sucking a cationic modifier (2, 3-epoxypropyltrimethylammonium chloride) solution with the concentration of 50g/L and dripping the solution into a conical flask, and then weighing NaOH with the concentration of 10g/L to prepare a modifier solution with the corresponding volume. And (3) putting 2g of pure cotton cloth sample into the prepared solution, putting the pure cotton cloth sample into a normal-temperature oscillation dyeing machine, oscillating for 30min at 70 ℃, taking out the cloth sample, fully washing the cloth sample with deionized water, removing the redundant modifier solution on the surface of the cloth sample, and finally putting the cloth sample into an oven for drying.
2) Dyeing cotton fabric
Preparing a dyeing solution: adding 3 percent of gardenia yellow dye (accounting for the mass fraction of the modifier solution, the same below) and 1 percent of lanthanum chloride into the modifier solution used in the step 1), mixing, and dyeing the cotton fabric according to the process curve of example 1, wherein the temperature is kept at 95 ℃ for 30 min.
3) Carrying out hydrophobic treatment on cotton fabric:
soaking 7 multiplied by 5cm dyed cotton fabric in phytic acid aqueous solution (2 mL of 0.019mol/L70 wt% phytic acid solution is measured by a pipette and added into 98mL of deionized water to prepare phytic acid solution) for 4 minutes, controlling the pressure of a padder by using the padder to enable the cotton fabric to be padded once at a padder rate of about 65% -70%, soaking the cotton fabric in 40mL of 0.02mol/L LaCl3.7H2O metal ion solution, then padding the cotton fabric by using the padder, repeatedly soaking the cotton fabric in the phytic acid solution for 8 times, and then padding the cotton fabric in La metal ion water; after the steps are repeated, the cotton fabric is washed by deionized water and then padded once by using a padder, then the cotton fabric is put into a 30g/L waterproof finishing agent to be soaked for 30 minutes and then washed by the deionized water, after the cotton fabric is washed and then padded once by using the padder, the cotton fabric is put into a constant temperature drying oven with the temperature of 120 ℃ for 30 minutes, then the cotton fabric is taken out, the temperature of the constant temperature drying oven is raised to 120 ℃, and then the cotton fabric is put into a baking oven for 1 minute.
The degree of contact angle was measured to be 154.8 ° by an angulometer using a contact angle measuring instrument manufactured by mathematic technology equipment ltd.
The laboratory adopts an ultraviolet-proof tester produced in great honor in Wen, Zhejiang, and the test result shows that the average transmission value of UVA is 1.92 by using the standard GB/T18830-2009; the UVB transmission average is 1.09; the UPF protection factor also achieves a 58+ effect, which indicates that the fabric has good ultraviolet resistance. Through the test of a color fastness tribometer and a color fastness to washing tester, the dry rubbing fastness can reach 4.5 grades, the wet rubbing fastness can reach 4 grades, and the color fastness to washing can reach 5 grades.
And (3) carrying out washing fastness detection on the prepared fabric: measuring 4g of standard soap powder, 1g of soda ash and 1L of distilled water to prepare soap lotion, soaping the treated fabric at room temperature for 5min according to the bath ratio of 1: 15, and respectively testing the super-hydrophobic and uvioresistant performances to obtain figures 18 and 19:
as can be seen from fig. 18, when the fabric is soaped 6 times, compared with the un-soaped fabric, the contact angle and the protection coefficient are actually reduced, but the contact angle still achieves the effect of 150 ° + and the hydrophobic property is still very excellent, the ultraviolet resistance also represents a good effect of 40+ in fig. 19, and the ultraviolet resistance still maintains 45 after 10 times of soaping, which indicates that the surface coating has a certain fastness to washing.
And (3) carrying out rubbing fastness detection on the prepared fabric:
after finishing, the cotton fabric was rubbed 50 times, 100 times, 150 times, 200 times, 250 times, 300 times and then the contact angle and the UPF value were measured as shown in fig. 20 and 21.
From fig. 20 and 21, it can be seen that the cotton fabric after 300 times of rubbing treatment still has a contact angle of more than 140 °, and the UPF value is also 45+, which indicates that the fabric still can maintain good hydrophobic ability and uv resistance after rubbing.
Performing SEM detection on the prepared fabric:
FIGS. 22A and 22B are non-experimentally processed cotton fabrics, which are approximately flat strips with one end thinner and the other thicker, as can be seen by scanning electron microscopy at two and three thousand times magnification; 22C and 22D are detection images of cotton fabrics after experimental treatment, and it can be clearly seen from pictures that nano-scale particles are adsorbed and formed on the surface layer of the cotton fabrics combined with ionic bonds, the rough surface is used as a carrier of the yc560 waterproof finishing agent, so that the yc560 waterproof finishing agent is adsorbed on the surface layer, and the cotton fabrics also achieve good ultraviolet resistance and super-hydrophobic effects.
The lanthanum chloride is utilized to dye plants, through process optimization, lanthanum chloride, phytic acid and yc560 waterproof finishing agent play a synergistic effect, and the dyed fabric is endowed with excellent properties of ultra-hydrophobicity and ultraviolet resistance, firstly, phosphate groups and-OH groups on the surface of the fabric generate complex aggregates with metal ions, secondly, phytic acid molecules can be adsorbed and fixed on a fabric substrate through covalent reaction between the phytic acid molecules and cotton fabrics, so that phytic acid and metal complexes are polymerized on the surface of the fabric to generate a coarse layered structure, then, the phytic acid molecules are modified by the yc560 waterproof finishing agent to form rich alkyl chains, certain surface morphology is generated on fibers, a certain ultra-hydrophobic surface is constructed, and the prepared fabric also has a certain ultraviolet resistance.
Example 4:
1) cationic modification of cotton fabric
According to the bath ratio of 50:1, sucking a cationic modifier (2, 3-epoxypropyltrimethylammonium chloride) solution with the concentration of 50g/L and dripping the solution into a conical flask, and then weighing NaOH with the concentration of 10g/L to prepare a modifier solution with the corresponding volume. And (3) putting 2g of pure cotton cloth sample into the prepared solution, putting the pure cotton cloth sample into a normal-temperature oscillation dyeing machine, oscillating for 30min at 70 ℃, taking out the cloth sample, fully washing the cloth sample with deionized water, removing the redundant modifier solution on the surface of the cloth sample, and finally putting the cloth sample into an oven for drying.
2) Dyeing cotton fabric
Preparing a dyeing solution: adding 3 percent of gardenia yellow dye (accounting for the mass fraction of the modifier solution, the same below) and 1 percent of lanthanum chloride into the modifier solution used in the step 1), mixing, and dyeing the cotton fabric according to the process curve of example 1, wherein the temperature is kept at 95 ℃ for 30 min.
3) Carrying out hydrophobic treatment on cotton fabric:
placing the dyed cotton fabric of 7 multiplied by 5cm into 30g/L of waterproof finishing agent YC560 for soaking for 30 minutes, then washing with deionized water, after washing, padding once with a padder, placing the cotton fabric into a constant temperature drying oven of 120 ℃ for 30 minutes, then taking out the cotton fabric, raising the temperature of the constant temperature drying oven to 120 ℃, then placing the cotton fabric into a baking oven for 1 minute, and then taking out the cotton fabric.
Through detection, the detection method is the same as that of the example 3, the contact angle of the obtained dyed fabric is 102 degrees, the ultraviolet resistance coefficient UPF is 36, the K/S value is 4.6, the contact angle of the fabric reaches 86 degrees when the fabric is soaped for 6 times, and the ultraviolet resistance performance reaches 27; the treated cotton fabric after 100 rubs had a contact angle of 77 ° and a UPF value of 30. Through the test of a color fastness tribometer and a color fastness to washing tester, the dry rubbing fastness can reach 3.5 level, the wet rubbing fastness can reach 2.5 level, and the color fastness to washing can reach 3.5 level.
Example 5:
1) cationic modification of cotton fabric
According to the bath ratio of 50:1, sucking a cationic modifier (2, 3-epoxypropyltrimethylammonium chloride) solution with the concentration of 50g/L and dripping the solution into a conical flask, and then weighing NaOH with the concentration of 10g/L to prepare a modifier solution with the corresponding volume. And (3) putting 2g of pure cotton cloth sample into the prepared solution, putting the pure cotton cloth sample into a normal-temperature oscillation dyeing machine, oscillating for 30min at 70 ℃, taking out the cloth sample, fully washing the cloth sample with deionized water, removing the redundant modifier solution on the surface of the cloth sample, and finally putting the cloth sample into an oven for drying.
2) Dyeing cotton fabric
Preparing a dyeing solution: adding 3% of gardenia yellow dye (accounting for the mass fraction of the modifier solution, the same below) into the modifier solution used in the step 1), mixing, and dyeing the cotton fabric according to the process curve of the embodiment 1, wherein the temperature is kept at 95 ℃ for 30 min.
3) Carrying out hydrophobic treatment on cotton fabric:
soaking 7 multiplied by 5cm dyed cotton fabric in 40mL of 0.02mol/L LaCl 3.7H2O metal ion solution (LaCl 3.7H2O), using a padder, controlling the pressure of the padder to enable the cotton fabric to have a mangling liquor rate of about 65% -70%, soaking the cotton fabric in phytic acid aqueous solution (2 mL0.019mol/L70 wt% phytic acid solution is measured by a pipette and added into 98mL of deionized water to prepare phytic acid solution) for 4 minutes after padding once, using the padder again, and then repeating 8 times of soaking the cotton fabric in La metal ion water and soaking in the phytic acid solution for padding; after the steps are repeated, the cotton fabric is washed by deionized water and then padded for one time by using a padder, then the cotton fabric is put into a 30g/L waterproof finishing agent to be soaked for 30 minutes and then washed by the deionized water, after the cotton fabric is washed and then padded for one time by using the padder, the cotton fabric is put into a constant temperature drying oven with the temperature of 120 ℃ for 30 minutes, then the cotton fabric is taken out, the temperature of the constant temperature drying oven is raised to 120 ℃, and then the cotton fabric is put into a baking oven to be baked for 1 minute and then taken out.
Through detection, the detection method is the same as that of the example 3, the contact angle of the obtained dyed fabric is 115 degrees, the ultraviolet resistance coefficient UPF is 40, the K/S value is only 2.36, the contact angle of the fabric reaches 97 degrees when the fabric is soaped for 6 times, and the ultraviolet resistance performance reaches 34; the treated cotton fabric after 100 rubs had a contact angle of 74 ° and a UPF value of 30. Through the test of a color fastness tribometer and a color fastness to washing tester, the dry rubbing fastness can reach 3.5 grades, the wet rubbing fastness can reach 3 grades, and the color fastness to washing can reach 4 grades.
Example 6:
1) cationic modification of cotton fabric
According to the bath ratio of 50:1, sucking a cationic modifier (2, 3-epoxypropyltrimethylammonium chloride) solution with the concentration of 50g/L and dripping the solution into a conical flask, and then weighing NaOH with the concentration of 10g/L to prepare a modifier solution with the corresponding volume. And (3) putting 2g of pure cotton cloth sample into the prepared solution, putting the pure cotton cloth sample into a normal-temperature oscillation dyeing machine, oscillating for 30min at 70 ℃, taking out the cloth sample, fully washing the cloth sample with deionized water, removing the redundant modifier solution on the surface of the cloth sample, and finally putting the cloth sample into an oven for drying.
2) Dyeing cotton fabric
Preparing a dyeing solution: adding 3 percent of gardenia yellow dye (accounting for the mass fraction of the modifier solution, the same below) and 1 percent of lanthanum chloride into the modifier solution used in the step 1), mixing, and dyeing the cotton fabric according to the process curve of example 1, wherein the temperature is kept at 95 ℃ for 30 min.
3) Carrying out hydrophobic treatment on cotton fabric:
soaking 7 multiplied by 5cm dyed cotton fabric in 40mL of 0.02mol/L LaCl 3.7H2O metal ion solution (LaCl 3.7H2O), using a padder, controlling the pressure of the padder to enable the cotton fabric to have a mangling liquor rate of about 65% -70%, soaking the cotton fabric in phytic acid aqueous solution (2 mL0.019mol/L70 wt% phytic acid solution is measured by a pipette and added into 98mL of deionized water to prepare phytic acid solution) for 4 minutes after padding once, using the padder again, and then repeating 8 times of soaking the cotton fabric in La metal ion water and soaking in the phytic acid solution for padding; after the steps are repeated, the cotton fabric is washed by deionized water and then padded for one time by using a padder, then the cotton fabric is put into a 30g/L waterproof finishing agent to be soaked for 30 minutes and then washed by the deionized water, after the cotton fabric is washed and then padded for one time by using the padder, the cotton fabric is put into a constant temperature drying oven with the temperature of 120 ℃ for 30 minutes, then the cotton fabric is taken out, the temperature of the constant temperature drying oven is raised to 120 ℃, and then the cotton fabric is put into a baking oven to be baked for 1 minute and then taken out.
Through detection, the detection method is the same as that of the example 3, the contact angle of the obtained dyed fabric is 122 degrees, the ultraviolet resistance coefficient UPF is 42, the K/S value is only 2.06, the contact angle of the fabric reaches 105 degrees when the fabric is soaped for 6 times, and the ultraviolet resistance reaches 34; the treated cotton fabric after 100 rubs had a contact angle of 86 ° and a UPF value of 30. Through the test of a color fastness tribometer and a color fastness to washing tester, the dry rubbing fastness can reach 3 grades, the wet rubbing fastness can reach 2.5 grades, and the color fastness to washing can reach 3.5 grades.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (7)

1. A super-hydrophobic ultraviolet-resistant cotton fabric dyeing method is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
preparing a modified solution to modify cotton fabrics;
adding a dye and a mordant into the modified solution, and dyeing the modified cotton fabric to obtain a dyed cotton fabric;
alternately padding the dyed cotton fabric in the mordant and the cross-linking agent for several times, wherein the alternate padding is to pad in the cross-linking agent firstly and then in the mordant, and the alternate padding is to pad for more than or equal to 9 times; the concentration of the padding crosslinking agent is 0.038-0.057 mol/L, the concentration of the mordant is 0.01-0.035 mol/L, and the mangle ratio is controlled to be 65-75%;
soaking in a waterproof finishing agent, cleaning, and padding, wherein the concentration of the waterproof finishing agent is 30-50 g/L;
drying and baking to obtain the super-hydrophobic anti-ultraviolet dyed cotton fabric;
wherein, the preparation modified solution is prepared by using a cation modifier and NaOH; the mordant is lanthanum chloride, the dye is a natural plant dye, the cross-linking agent is phytic acid, and the waterproof finishing agent is YC 560;
and adding a dye and a mordant into the modified solution to dye the modified cotton fabric, wherein the dye and the mordant accounting for 3% of the modified solution by mass are added.
2. The method for dyeing superhydrophobic ultraviolet-resistant cotton fabric according to claim 1, characterized in that: the cationic modifier is 2, 3-epoxypropyl trimethyl ammonium chloride, and the dye is gardenia yellow dye.
3. The dyeing method of super-hydrophobic UV-resistant cotton fabric according to claim 1 or 2, characterized in that: preparing a modified solution, namely modifying a cotton fabric, wherein the bath ratio is 50:1, the modified solution is prepared by using a cationic modifier with the concentration of 30-50 g/L and NaOH with the concentration of 10-30 g/L, and the cotton fabric is subjected to oscillation for 30-70 min at the temperature of 50-90 ℃.
4. The dyeing method of super-hydrophobic UV-resistant cotton fabric according to claim 1 or 2, characterized in that: and adding a dye and a mordant into the modified solution, dyeing the modified cotton fabric, dyeing for 10min at normal temperature, heating to 95 ℃, preserving heat for 30-70 min, and washing with water.
5. The dyeing method of super-hydrophobic UV-resistant cotton fabric according to claim 1 or 2, characterized in that: and soaking in a waterproof finishing agent, cleaning and padding, wherein the step of soaking in 30-50 g/L of the waterproof finishing agent for 30 minutes is to clean and pad once.
6. The dyeing method of super-hydrophobic UV-resistant cotton fabric according to claim 1 or 2, characterized in that: and drying and baking the cotton fabric after drying, namely drying the cotton fabric for 30 minutes at 65-85 ℃, taking out the cotton fabric, heating the cotton fabric to 100-140 ℃, and baking the cotton fabric for 0.8-2.6 minutes.
7. The super-hydrophobic UV resistant dyed cotton fabric made by the method of claim 1, wherein: the contact angle degree of the prepared super-hydrophobic ultraviolet-resistant dyed cotton fabric is more than or equal to 154 degrees, and the UPF value is more than or equal to 58 degrees.
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