CN113430843A - Method for dyeing cotton fabric by reactive dye - Google Patents

Method for dyeing cotton fabric by reactive dye Download PDF

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Publication number
CN113430843A
CN113430843A CN202110778467.9A CN202110778467A CN113430843A CN 113430843 A CN113430843 A CN 113430843A CN 202110778467 A CN202110778467 A CN 202110778467A CN 113430843 A CN113430843 A CN 113430843A
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cotton fabric
mixed solution
reactive dye
reactive
btca
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CN113430843B (en
Inventor
姜会钰
张智刚
吴浩能
姚金波
欧阳泽宇
周绚丽
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Yantai Mingyuan Creative Life Technology Co ltd
Wuhan Textile University
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Yantai Mingyuan Creative Life Technology Co ltd
Wuhan Textile University
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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
    • D06P1/38—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 reactive dyes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • 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
    • D06P1/0032—Determining dye recipes and dyeing parameters; Colour matching or monitoring
    • 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
    • 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
    • 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
    • D06P3/66—Natural or regenerated cellulose using reactive dyes

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  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Coloring (AREA)

Abstract

The invention relates to the field of functional finishing of textiles and discloses a method for dyeing cotton fabrics by using reactive dyes. The method comprises the following steps: (1) completely immersing cotton fabrics in BTCA-sodium hypophosphite mixed solution, stirring for 10-15min, wherein the ratio of the cotton fabrics to the BTCA-sodium hypophosphite mixed solution is 3-5g/100mL, then removing redundant solution by rolling, controlling the rolling residual rate of the cotton fabrics to be 96-105 wt%, then drying the cotton fabrics, then curing for 4-12min at the temperature of 140-; (2) and (2) placing the modified cotton fabric obtained in the step (1) into reactive dye liquor with the pH value of 6-8 for dyeing, and then sequentially washing, soaping and drying. The method has simple process flow and good dye-resisting effect.

Description

Method for dyeing cotton fabric by reactive dye
Technical Field
The invention relates to the field of functional finishing of textiles, in particular to a method for dyeing cotton fabrics by using reactive dyes.
Background
Cotton fiber has a long history as a textile raw material, people can use cotton spinning woven fabric for warm keeping as early as thousands of years, and cotton is still one of the most important crops in China so far, and the cotton fiber plays an important role in our daily life. In the past, cotton fibers have been widely used in medical supplies, garment materials, daily production, and the like, due to their excellent wearability. With the continuous increase of the industrial level, a plurality of chemical fiber products expose the corners successively, the synthetic fibers bring certain impact to the cotton fiber industry by virtue of the excellent performance of the synthetic fibers, but with the continuous improvement of the environmental awareness of people, people gradually return the concerned gravity center to the development and application aspects of the cotton fibers, and the cotton fibers are favored by people as a natural fiber by virtue of the excellent qualities of fastness, wear resistance, washing resistance, high-temperature ironing, moisture absorption and dehumidification, softness, no stimulation, comfort, warmth retention, insect damage resistance and the like. In the industrial production process, cotton fibers can be used for not only textile finishing but also fiber dyeing, as is well known, reactive dyes are one of important dyes for dyeing cotton fibers, the dyeing requirements in production are various, sometimes, fabrics need to achieve the effect of different color shades after being dyed, at the moment, most of fabrics are cationized and then dyed, so that the effect is expected to be achieved, but the method has the defects of complex and long treatment process, high cost and the like, and the problem is more obvious when the content of colored fibers is high.
Disclosure of Invention
The invention aims to solve the problems of complex process and high cost of cationic dyeing used for dyeing to obtain fabrics with different colors in the prior art, and provides a method for dyeing cotton fabrics by using reactive dyes.
In order to achieve the aim, the invention provides a method for dyeing cotton fabrics by using reactive dyes, which comprises the following steps:
(1) completely immersing cotton fabrics in BTCA-sodium hypophosphite mixed solution, stirring for 10-15min, wherein the ratio of the cotton fabrics to the BTCA-sodium hypophosphite mixed solution is 3-5g/100mL, then removing redundant solution by rolling, controlling the rolling residual rate of the cotton fabrics to be 96-105 wt%, then drying the cotton fabrics, then curing for 4-12min at the temperature of 140-;
(2) placing the modified cotton fabric obtained in the step (1) in reactive dye liquor with the pH value of 6-8 for dyeing at the temperature of 60-80 ℃ for 25-30min, and then sequentially washing, soaping and drying;
in the step (1), the BTCA-sodium hypophosphite mixed solution contains 8-11 wt% of BTCA, and the BTCA-sodium hypophosphite mixed solution contains 4-12 wt% of sodium hypophosphite;
in the step (2), the dosage of the reactive dye in the reactive dye solution is 0.2-1.1% o.w.f.
Preferably, in the step (1), the stirring temperature is 20-30 ℃, and the stirring speed is 20-180 r/min.
Preferably, in the step (1), the drying temperature is 75-85 ℃, and the drying time is 10-15 min.
Preferably, in the step (1), the cured cotton fabric is washed using an acetic acid-ethanol mixed solution.
Further preferably, the concentration of acetic acid in the acetic acid-ethanol mixed solution is 0.8-1.5g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 0.8-1.5 g/L.
Further preferably, the number of washing is 2 to 4.
Preferably, in the step (1), the drying temperature is 75-85 ℃, and the drying time is 8-12 min.
Preferably, in the step (2), the weight ratio of the modified cotton fabric to the reactive dye liquor is 1: 100;
further preferably, the reactive dye is reactive yellow X-R, reactive orange K-G or reactive brilliant blue KN-R.
Further preferably, the reactive dye is reactive orange K-G or reactive brilliant blue KN-R.
Further preferably, the reactive dye is reactive brilliant blue KN-R.
Preferably, in the step (2), the reactive dye liquor also contains sodium sulfate and sodium carbonate.
Further preferably, the concentration of sodium sulfate in the reactive dye liquor is 8-12g/L, and the concentration of sodium carbonate in the reactive dye liquor is 8-12 g/L.
Preferably, in step (2), the number of washing is 2 to 4.
Preferably, in the step (2), the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1: 100.
preferably, in the step (2), the temperature of the soaping is 70-80 ℃, and the time of the soaping is 15-20 min.
The dyeing method provided by the invention is simple in process flow, low in cost and good in dye-repellent effect.
Drawings
FIG. 1 is an infrared spectrum of a modified cotton fabric obtained in example 1 before dyeing according to the present invention and an unmodified cotton fabric of comparative example 1;
FIG. 2 is an SEM photograph of an unmodified cotton fabric of comparative example 1 prior to dyeing in accordance with the invention;
FIG. 3 is an SEM photograph of an unmodified cotton fabric of comparative example 1 prior to dyeing in accordance with the invention;
FIG. 4 is an SEM photograph of a modified cotton fabric obtained in example 1 before dyeing in accordance with the present invention;
FIG. 5 is an SEM photograph of a modified cotton fabric obtained in example 1 before dyeing in accordance with the present invention;
FIG. 6 is a graph comparing the zeta potential at different pH values of the modified cotton fabric obtained in example 1 before dyeing according to the invention with the unmodified cotton fabric of comparative example 1.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for dyeing cotton fabrics by using reactive dyes, which comprises the following steps:
(1) completely immersing cotton fabrics in BTCA-sodium hypophosphite mixed solution, stirring for 10-15min, wherein the ratio of the cotton fabrics to the BTCA-sodium hypophosphite mixed solution is 3-5g/100mL, then removing redundant solution by rolling, controlling the rolling residual rate of the cotton fabrics to be 96-105 wt%, then drying the cotton fabrics, then curing for 4-12min at the temperature of 140-;
(2) placing the modified cotton fabric obtained in the step (1) in reactive dye liquor with the pH value of 6-8 for dyeing at the temperature of 60-80 ℃ for 25-30min, and then sequentially washing, soaping and drying;
in the step (1), the BTCA-sodium hypophosphite mixed solution contains 8-11 wt% of BTCA, and the BTCA-sodium hypophosphite mixed solution contains 4-12 wt% of sodium hypophosphite;
in the step (2), the dosage of the reactive dye in the reactive dye solution is 0.2-1.1% o.w.f.
In a specific embodiment, the content of BTCA in the BTCA (1, 2, 3, 4-butanetetracarboxylic acid) -sodium hypophosphite mixed solution may be 8 wt%, 8.5 wt%, 9 wt%, 9.5 wt%, 10 wt%, 10.5 wt%, or 11 wt%, and the content of sodium hypophosphite in the BTCA-sodium hypophosphite mixed solution may be 4 wt%, 4.5 wt%, 5 wt%, 5.5 wt%, 6 wt%, 6.5 wt%, 7 wt%, 7.5 wt%, 8 wt%, 8.5 wt%, 9 wt%, 9.5 wt%, 10 wt%, 10.5 wt%, 11 wt%, 11.5 wt%, or 12 wt%.
Specifically, the ratio of the cotton fabric to the BTCA-sodium hypophosphite mixed solution can be 3g/100mL, 3.1g/100mL, 3.2g/100mL, 3.3g/100mL, 3.4g/100mL, 3.5g/100mL, 3.6g/100mL, 3.7g/100mL, 3.8g/100mL, 3.9g/100mL, 4g/100mL, 4.1g/100mL, 4.2g/100mL, 4.3g/100mL, 4.4g/100mL, 4.5g/100mL, 4.6g/100mL, 4.7g/100mL, 4.8g/100mL, 4.9g/100mL, or 5g/100 mL.
In the invention, the cotton fabric is completely immersed in the BTCA-sodium hypophosphite mixed solution, and the stirring time can be 10min, 10.5min, 11min, 11.5min, 12min, 12.5min, 13min, 13.5min, 14min, 14.25min, 14.5min, 14.75min or 15 min.
In particular embodiments, the cotton fabric may have a raffle ratio of 96 wt%, 96.5 wt%, 97 wt%, 97.5 wt%, 98 wt%, 98.5 wt%, 99 wt%, 99.5 wt%, 100 wt%, 100.5 wt%, 101 wt%, 101.5 wt%, 102 wt%, 102.5 wt%, 103 wt%, 103.5 wt%, 104 wt%, 104.5 wt%, or 105 wt%.
In the present invention, the retention is the weight of the liquid carried on the fabric as a percentage of the weight of the fabric itself.
In the present invention, the stirring temperature is 20 to 30 ℃. Specifically, the stirring temperature may be 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃ or 30 ℃.
In the invention, the stirring speed is 20-180 r/min. Specifically, the stirring speed can be 20r/min, 30r/min, 40r/min, 50r/min, 60r/min, 70r/min, 80r/min, 90r/min, 100r/min, 110r/min, 120r/min, 130r/min, 140r/min, 150r/min, 160r/min, 170r/min or 180 r/min.
In the invention, the drying temperature is 75-85 ℃, and the drying time is 10-15 min. In a specific embodiment, the drying temperature may be 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃ or 85 ℃, and the drying time may be 10min, 10.5min, 11min, 11.5min, 12min, 12.5min, 13min, 13.5min, 14min, 14.5min or 15 min.
In the present invention, there is no particular requirement for the equipment for the drying, which may be conventional in the art, and preferably, the drying of the cotton fabric is carried out using an electrically heated forced air drying oven.
In the present invention, in step (1), the cured cotton fabric is washed using an acetic acid-ethanol mixed solution.
Preferably, the concentration of acetic acid in the acetic acid-ethanol mixed solution is 0.8-1.5g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 0.8-1.5 g/L. Specifically, the concentration of acetic acid in the acetic acid-ethanol mixed solution may be 0.8g/L, 0.9g/L, 1g/L, 1.1g/L, 1.2g/L, 1.3g/L, 1.4g/L or 1.5g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution may be 0.8g/L, 0.9g/L, 1g/L, 1.1g/L, 1.2g/L, 1.3g/L, 1.4g/L or 1.5 g/L.
Preferably, the number of washing is 2 to 4. Specifically, the number of washing may be 2, 3, or 4.
In the invention, the drying temperature is 75-85 ℃, and the drying time is 8-12 min. Specifically, the drying temperature can be 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃ or 85 ℃, and the drying time can be 8min, 8.5min, 9min, 9.5min, 10min, 10.5min, 11min, 11.5min or 12 min.
In the present invention, the degree of substitution of the modified cotton fabric obtained in step (1) may be 0.4, 0.41, 0.42, 0.43, 0.44, 0.45, 0.46, 0.47, 0.48, 0.49 or 0.5.
In the invention, the cotton fabric which is modified by polycarboxylic acid has carboxyl in the structure, so that the substitution degree of the modified cotton fabric can be determined by calculating the carboxyl content in the cotton fabric, and the larger the substitution degree is, the larger the modification reaction degree is;
the test method of the carboxyl content (degree of substitution) DS comprises the following steps:
(1) preparation of 100mmol/L NaOH solution
Weighing 1.0g of sodium hydroxide solid, dissolving in 50mL of deionized water, fully stirring, diluting to a constant volume of 250mL, and keeping for later use.
(2) Preparation of 100mmol/L HCl solution
8.3ml of concentrated hydrochloric acid solution is measured by a pipette and poured into a volumetric flask, then deionized water is added into the volumetric flask, the volume is fixed to 1L, the solution is fully shaken up and sealed, and the solution is reserved for later use.
(3) Determination of carboxylic acid group content on modified cotton fabric
A 5cm x 5cm sample of the modified cotton fabric was immersed in 100mL of 0.5% HCl solution for 16 hours and then the fabric was rinsed with deionized water until the HCl was completely removed from the sample, using a silver nitrate drip test to ensure that no chloride residue remained on the surface of the fabric. After rinsing, the samples were dried at room temperature. About 0.25g of sample was weighed and soaked in 50mL of 100mmol/L NaOH solution at room temperature for 4 hours, and the container was sealed to ensure that NaOH did not react with CO in the air2The reaction was run using another 50mL100mmol/LNaOH solution as a blank. After 4 hours, the solution was titrated with 100mmol/L HCl solution. Phenolphthalein is used to determine the endpoint, and to improve the accuracy of the method, the amount of titrant is determined by weighing the remaining titrant and calculating the amount used, the amount of titrant reacted is recorded, three experiments are performed, the average value is taken,
the calculation formula is shown in formula (2.1) and formula (2.2):
QCOOH＝(V1C1-V2C2)/m (2.1)
Figure BDA0003156741640000071
wherein V1、C1Is the volume and concentration of the sodium hydroxide solution used, V2、C2M is the weight of the cotton fabric measured, as is the concentration of hydrochloric acid used and the remaining volume.
In a specific embodiment, in step (2), the pH of the reactive dye liquor may be 6, 6.1, 6.2, 6.3, 6.4, 6.5, 6.6, 6.7, 6.8, 6.9, 7, 7.1, 7.2, 7.3, 7.4, 7.5, 7.6, 7.7, 7.8, 7.9 or 8.
The inventor finds that the cotton fabric modified by the method can hydrolyze ester bonds under acidic or alkaline conditions, and the ester bonds have stronger hydrolytic capability under alkaline conditions, so that the repulsion between the surface of cotton fibers and dye anions in a solution is reduced, the dye repellency is reduced, and the dye repellency is poorer when the acidity or alkalinity is stronger, therefore, the pH value of the active dye liquor is set to be 6-8 in the dyeing process, and the dye repellency is further improved.
In a specific embodiment, in step (2), the amount of the reactive dye in the reactive dye liquor may be 0.2% o.w.f, 0.3% o.w.f, 0.4% o.w.f, 0.5% o.w.f, 0.6% o.w.f, 0.7% o.w.f, 0.8% o.w.f, 0.9% o.w.f, 1% o.w.f or 1.1% o.w.f.
In the invention, in the step (2), the weight ratio of the modified cotton fabric to the reactive dye liquor is 1: 100.
In the invention, the reactive dye is reactive yellow X-R, reactive orange K-G or reactive brilliant blue KN-R.
Preferably, the reactive dye is reactive orange K-G or reactive brilliant blue KN-R.
Further preferably, the reactive dye is reactive brilliant blue KN-R.
In the invention, in the step (2), the reactive dye liquor also contains sodium sulfate and sodium carbonate.
Preferably, the concentration of sodium sulfate in the reactive dye liquor is 8-12g/L, and the concentration of sodium carbonate in the reactive dye liquor is 8-12 g/L. Specifically, the concentration of sodium sulfate in the reactive dye liquor can be 8g/L, 8.25g/L, 8.5g/L, 8.75g/L, 9g/L, 9.25g/L, 9.5g/L, 9.75g/L, 10g/L, 10.25g/L, 10.5g/L, 10.75g/L, 11g/L, 11.25g/L, 11.5g/L, 11.75g/L or 12g/L, the concentration of sodium carbonate in the reactive dye liquor can be 8g/L, 8.25g/L, 8.5g/L, 8.75g/L, 9g/L, 9.25g/L, 9.5g/L, 9.75g/L, 10g/L, 10.25g/L, 10.5g/L, 10.75g/L, 11g/L, 11.25g/L, 11.5g/L or 12g/L, and the concentration of sodium carbonate in the reactive dye liquor can be 8g/L, 8.25g/L, 8.5g/L, 10.75g/L, 11.25g/L, 9.75g/L, 11.25g/L, 9.25g/L, 10.25g/L, 10.5g/L, 10.75g/L, 10.25g/L, 10.5g/L, 10.75g/L, 10.25g/L, 10.75g/L, or 12g/L, 11.5g/L, 11.75g/L or 12 g/L.
In a specific embodiment, the dyeing temperature may be 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃ or 80 ℃, and the dyeing time may be 25min, 25.5min, 26min, 26.5min, 27min, 27.5min, 28min, 28.5min, 29min, 29.5min or 30 min.
The inventor finds that the modified cotton fabric obtained by the invention has poor dye-repellent performance at high temperature in the experimental research process, so that the dyeing temperature is set to be 60-80 ℃ in order to achieve better dye-repellent effect.
In the present invention, in the step (2), the number of washing is 2 to 4. Specifically, the number of washing may be 2, 3, or 4.
In the invention, in the step (2), the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1: 100.
in the invention, in the step (2), the temperature of the soaping is 70-80 ℃, and the time of the soaping is 15-20 min. Specifically, the soaping temperature can be 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃ or 80 ℃, and the soaping time can be 15min, 15.5min, 16min, 16.5min, 17min, 17.5min, 18min, 18.5min, 19min, 19.5min or 20 min.
The method has simple process flow, the cotton fabric obtained by modification can show larger electronegativity in the solution by matching with a proper dyeing process, the cotton fabric can be lightened if dye anions need to overcome larger repulsion force when the modified cotton fabric is dyed, in addition, primary hydroxyl sites of the modified cotton fiber are reduced, and the dye anions mainly react with the primary hydroxyl on the cotton fiber, so that the dye is difficult to dye, and the dyeing cotton fabric is further smaller in K/S value and better in dye-repellent effect by matching with the proper dyeing process, and has lighter color depth after dyeing and better application prospect.
The present invention will be described in detail below by way of examples. The method of the present invention is not limited thereto. The reactive brilliant blue KN-R used in the examples and comparative examples was C.I. reactive blue 19, available from Shanghai Aladdin Biotech Ltd.
Example 1
(1) Completely immersing the cotton fabric in a BTCA-sodium hypophosphite mixed solution (the BTCA-sodium hypophosphite mixed solution contains 10 weight percent of BTCA, the BTCA-sodium hypophosphite mixed solution contains 10 weight percent of sodium hypophosphite), wherein the ratio of the cotton fabric to the BTCA-sodium hypophosphite mixed solution is 4g/100mL, stirring for 15min at 25 ℃, the stirring speed is 100r/min, then removing the redundant solution by rolling, controlling the rolling residual rate of the cotton fabric to be 100 weight percent, then putting the cotton fabric into an electrothermal blowing drying oven, drying for 10min at 80 ℃, then curing for 10min at 150 ℃, then washing the cured cotton fabric for 3 times by using an acetic acid-ethanol mixed solution, wherein the concentration of acetic acid in the acetic acid-ethanol mixed solution is 1g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 1g/L, then placing the cotton fabric in an oven at 80 ℃ for drying for 10min to obtain an anion modified cotton fabric with the substitution degree DS of 0.451;
(2) placing the modified cotton fabric obtained in the step (1) in a reactive dye (reactive brilliant blue KN-R) dye solution with a pH value of 7 for dyeing (the concentration of sodium sulfate in the reactive dye solution is 10g/L, the concentration of sodium carbonate in the reactive dye solution is 10g/L), the using amount of the reactive dye in the reactive dye solution is 1% o.w.f, the weight ratio of the modified cotton fabric to the reactive dye solution is 1:100, the dyeing temperature is 70 ℃, the dyeing time is 30min, then washing is carried out for 3 times, then soaping is carried out in a soaping solution of 0.1g/L, and the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1:100, soaping at the temperature of 70 ℃ for 15min, and finally drying to obtain the dyed cotton fabric A1.
Example 2
(1) Completely immersing the cotton fabric in a BTCA-sodium hypophosphite mixed solution (the BTCA-sodium hypophosphite mixed solution contains 10 weight percent of BTCA, the BTCA-sodium hypophosphite mixed solution contains 10 weight percent of sodium hypophosphite), wherein the ratio of the cotton fabric to the BTCA-sodium hypophosphite mixed solution is 3g/100mL, stirring for 15min at 20 ℃, the stirring speed is 80r/min, then removing the redundant solution by rolling, controlling the rolling residual rate of the cotton fabric to be 102 weight percent, then putting the cotton fabric into an electrothermal blowing drying oven, drying for 15min at 75 ℃, then curing for 5min at 160 ℃, then washing the cured cotton fabric for 3 times by using an acetic acid-ethanol mixed solution, wherein the concentration of acetic acid in the acetic acid-ethanol mixed solution is 1g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 1g/L, then placing the cotton fabric in a drying oven at 75 ℃ for drying for 11min to obtain an anion modified cotton fabric with the degree of substitution DS of 0.441;
(2) placing the modified cotton fabric obtained in the step (1) in a reactive dye (reactive brilliant blue KN-R) dye solution with the pH value of 6.5 for dyeing (the concentration of sodium sulfate in the reactive dye solution is 9g/L, the concentration of sodium carbonate in the reactive dye solution is 10g/L), the using amount of the reactive dye in the reactive dye solution is 0.5% o.w.f, the weight ratio of the modified cotton fabric to the reactive dye solution is 1:100, the dyeing temperature is 60 ℃, the dyeing time is 30min, then washing is carried out for 3 times, then soaping is carried out in a soaping solution of 0.1g/L, and the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1:100, soaping at 73 ℃ for 19min, and finally drying to obtain the dyed cotton fabric A2.
Example 3
(1) Completely immersing the cotton fabric in a BTCA-sodium hypophosphite mixed solution (the BTCA-sodium hypophosphite mixed solution contains 10 weight percent of BTCA, and the BTCA-sodium hypophosphite mixed solution contains 5 weight percent of sodium hypophosphite), wherein the ratio of the cotton fabric to the BTCA-sodium hypophosphite mixed solution is 4g/100mL, stirring for 15min at the temperature of 30 ℃, the stirring speed is 50r/min, then removing the redundant solution by rolling, controlling the rolling residual rate of the cotton fabric to be 98 weight percent, then putting the cotton fabric into an electrothermal blowing drying oven, drying for 11min at the temperature of 75 ℃, then curing for 10min at the temperature of 145 ℃, then washing the cured cotton fabric for 2 times by using an acetic acid-ethanol mixed solution, wherein the concentration of acetic acid in the acetic acid-ethanol mixed solution is 1.5g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 1.5g/L, then placing the cotton fabric in a drying oven at 85 ℃ for drying for 10min to obtain an anion modified cotton fabric with the degree of substitution DS of 0.425;
(2) placing the modified cotton fabric obtained in the step (1) in a reactive dye (reactive brilliant blue KN-R) dye solution with a pH value of 8 for dyeing (the concentration of sodium sulfate in the reactive dye solution is 11g/L, the concentration of sodium carbonate in the reactive dye solution is 10g/L), the using amount of the reactive dye in the reactive dye solution is 1.1% o.w.f, the weight ratio of the modified cotton fabric to the reactive dye solution is 1:100, the dyeing temperature is 78 ℃, the dyeing time is 25min, then washing is carried out for 2 times, then soaping is carried out in a soaping solution of 0.1g/L, and the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1:100, soaping at 75 ℃ for 18min, and finally drying to obtain the dyed cotton fabric A3.
Example 4
(1) Completely immersing the cotton fabric in a BTCA-sodium hypophosphite mixed solution (the BTCA-sodium hypophosphite mixed solution contains 8 weight percent of BTCA, the BTCA-sodium hypophosphite mixed solution contains 10 weight percent of sodium hypophosphite), wherein the ratio of the cotton fabric to the BTCA-sodium hypophosphite mixed solution is 5g/100mL, stirring for 10min at 28 ℃, the stirring speed is 120r/min, then removing the redundant solution by rolling, controlling the residual rolling rate of the cotton fabric to be 96 weight percent, then putting the cotton fabric into an electrothermal blowing drying oven, drying for 10min at 85 ℃, then curing for 10min at 148 ℃, then washing the cured cotton fabric for 2 times by using an acetic acid-ethanol mixed solution, wherein the concentration of acetic acid in the acetic acid-ethanol mixed solution is 1.1g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 1.1g/L, then placing the cotton fabric in an oven at 80 ℃ for drying for 9min to obtain an anion modified cotton fabric with the substitution degree DS of 0.423;
(2) placing the modified cotton fabric obtained in the step (1) in a reactive dye (reactive brilliant blue KN-R) dye solution with a pH value of 6 for dyeing (the concentration of sodium sulfate in the reactive dye solution is 10g/L, the concentration of sodium carbonate in the reactive dye solution is 9g/L), the using amount of the reactive dye in the reactive dye solution is 0.8% o.w.f, the weight ratio of the modified cotton fabric to the reactive dye solution is 1:100, the dyeing temperature is 70 ℃, the dyeing time is 30min, then washing is carried out for 4 times, then soaping is carried out in a soaping solution of 0.1g/L, and the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1:100, soaping at 78 ℃ for 15min, and finally drying to obtain the dyed cotton fabric A4.
Example 5
(1) Completely immersing the cotton fabric in a BTCA-sodium hypophosphite mixed solution (the BTCA-sodium hypophosphite mixed solution contains 8 weight percent of BTCA, the BTCA-sodium hypophosphite mixed solution contains 10 weight percent of sodium hypophosphite), wherein the ratio of the cotton fabric to the BTCA-sodium hypophosphite mixed solution is 3g/100mL, stirring for 10min at the temperature of 30 ℃, the stirring speed is 150r/min, then removing the redundant solution by rolling, controlling the residual rolling rate of the cotton fabric to be 105 weight percent, then putting the cotton fabric into an electrothermal blowing drying oven, drying for 11min at the temperature of 80 ℃, then curing for 5min at the temperature of 158 ℃, then washing the cured cotton fabric for 4 times by using an acetic acid-ethanol mixed solution, wherein the concentration of acetic acid in the acetic acid-ethanol mixed solution is 1.2g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 1.2g/L, then placing the cotton fabric in a drying oven at 77 ℃ for drying for 10min to obtain an anion modified cotton fabric with the degree of substitution DS of 0.419;
(2) placing the modified cotton fabric obtained in the step (1) in a reactive dye (reactive brilliant blue KN-R) dye solution with a pH value of 7 for dyeing (the concentration of sodium sulfate in the reactive dye solution is 10g/L, the concentration of sodium carbonate in the reactive dye solution is 8g/L), the using amount of the reactive dye in the reactive dye solution is 0.2% o.w.f, the weight ratio of the modified cotton fabric to the reactive dye solution is 1:100, the dyeing temperature is 80 ℃, the dyeing time is 25min, then washing is carried out for 4 times, then soaping is carried out in a soaping solution of 0.1g/L, and the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1:100, soaping at 71 ℃ for 15min, and finally drying to obtain the dyed cotton fabric A5.
Example 6
(1) Completely immersing the cotton fabric in a BTCA-sodium hypophosphite mixed solution (the BTCA-sodium hypophosphite mixed solution contains 11 weight percent of BTCA, and the BTCA-sodium hypophosphite mixed solution contains 4 weight percent of sodium hypophosphite), wherein the ratio of the cotton fabric to the BTCA-sodium hypophosphite mixed solution is 5g/100mL, stirring for 15min at the temperature of 23 ℃, the stirring speed is 120r/min, then removing the redundant solution by rolling, controlling the rolling residual rate of the cotton fabric to be 100 weight percent, then putting the cotton fabric into an electrothermal blowing drying oven, drying for 10min at the temperature of 83 ℃, then curing for 12min at the temperature of 140 ℃, then washing the cured cotton fabric for 3 times by using an acetic acid-ethanol mixed solution, wherein the concentration of acetic acid in the acetic acid-ethanol mixed solution is 1.5g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 1.5g/L, then placing the cotton fabric in an oven at 83 ℃ for drying for 8min to obtain an anion modified cotton fabric with the substitution degree DS of 0.433;
(2) placing the modified cotton fabric obtained in the step (1) in a reactive dye (reactive brilliant blue KN-R) dye solution with a pH value of 7 for dyeing (the concentration of sodium sulfate in the reactive dye solution is 10g/L, the concentration of sodium carbonate in the reactive dye solution is 9g/L), the using amount of the reactive dye in the reactive dye solution is 1% o.w.f, the weight ratio of the modified cotton fabric to the reactive dye solution is 1:100, the dyeing temperature is 65 ℃, the dyeing time is 30min, then washing is carried out for 2 times, then soaping is carried out in a soaping solution of 0.1g/L, and the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1:100, soaping at the temperature of 70 ℃ for 20min, and finally drying to obtain the dyed cotton fabric A6.
Example 7
(1) Completely immersing the cotton fabric in a BTCA-sodium hypophosphite mixed solution (the BTCA-sodium hypophosphite mixed solution contains 9 weight percent of BTCA, and the BTCA-sodium hypophosphite mixed solution contains 12 weight percent of sodium hypophosphite), wherein the ratio of the cotton fabric to the BTCA-sodium hypophosphite mixed solution is 4g/100mL, stirring for 15min at 22 ℃, the stirring speed is 125r/min, then removing the redundant solution by rolling, controlling the residual rolling rate of the cotton fabric to be 103 weight percent, then putting the cotton fabric into an electrothermal blowing drying oven, drying for 12min at 76 ℃, then curing for 4min at 157 ℃, then washing the cured cotton fabric for 2 times by using an acetic acid-ethanol mixed solution, wherein the concentration of acetic acid in the acetic acid-ethanol mixed solution is 1.2g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 1.2g/L, then placing the cotton fabric in a drying oven at 75 ℃ for drying for 12min to obtain an anion modified cotton fabric with the substitution degree DS of 0.437;
(2) placing the modified cotton fabric obtained in the step (1) in a reactive dye (reactive brilliant blue KN-R) dye solution with a pH value of 7 for dyeing (the concentration of sodium sulfate in the reactive dye solution is 9g/L, the concentration of sodium carbonate in the reactive dye solution is 11g/L), the using amount of the reactive dye in the reactive dye solution is 0.9% o.w.f, the weight ratio of the modified cotton fabric to the reactive dye solution is 1:100, the dyeing temperature is 70 ℃, the dyeing time is 30min, then washing is carried out for 2 times, then soaping is carried out in a soaping solution of 0.1g/L, and the weight ratio of the modified cotton fabric obtained in the step (1) to the soaping solution is 1:100, soaping at 80 ℃ for 15min, and finally drying to obtain the dyed cotton fabric A7.
Comparative example 1
The procedure was followed as described in example 1, except that the cotton fabric was dyed without modification to give dyed cotton fabric D1.
Comparative example 2
The procedure of example 4 was followed, except that in step (1), 5% by weight of BTCA was contained in the BTCA-sodium hypophosphite mixed solution to obtain a modified cotton fabric having a degree of substitution DS of 0.373, which was then dyed to obtain a dyed cotton fabric D2.
Comparative example 3
The procedure of example 6 was followed, except that in step (1), 14% by weight of BTCA was contained in the BTCA-sodium hypophosphite mixed solution to obtain a modified cotton fabric having a degree of substitution DS of 0.343, which was then dyed to obtain a dyed cotton fabric D3.
Comparative example 4
The procedure of example 6 was followed, except that in step (1), 2% by weight of sodium hypophosphite was contained in the BTCA-sodium hypophosphite mixed solution to obtain a modified cotton fabric having a degree of substitution DS of 0.313, which was then dyed to obtain a dyed cotton fabric D4.
Comparative example 5
The procedure of example 7 was followed, except that in step (1), a modified cotton fabric having a degree of substitution DS of 0.339 was obtained by adding 16 wt% sodium hypophosphite to the BTCA-sodium hypophosphite mixed solution, and then dyeing was carried out to obtain a dyed cotton fabric D5.
Comparative example 6
Carried out as described in example 6, except that in step (1) the curing time was 17min, giving a modified cotton fabric with a degree of substitution DS of 0.335, which was then dyed, giving a dyed cotton fabric D6.
Comparative example 7
Carried out as described in example 7, except that in step (1) the curing time was 2min, giving a modified cotton fabric with a degree of substitution DS of 0.327, which was then dyed, giving a dyed cotton fabric D7.
Comparative example 8
Carried out as described in example 3, except that in step (2) the reactive dye liquor had a pH of 8.5, a dyed cotton fabric D8 was obtained.
Comparative example 9
Carried out as described in example 4, except that in step (2) the reactive dye liquor had a pH of 5, a dyed cotton fabric D9 was obtained.
Comparative example 10
Carried out as described in example 2, except that in step (2) the dyeing temperature was 50 ℃ to obtain a dyed cotton fabric D10.
Comparative example 11
Carried out as described in example 5, except that in step (2) the dyeing temperature was 90 ℃ to obtain a dyed cotton fabric D11.
Test example 1
Respectively carrying out infrared analysis on the modified cotton fabric in the example 1 and the unmodified cotton fabric in the comparative example 1 before dyeing by adopting a Fourier transform infrared spectrometer (Bruker TENSOR-II) (in order to reduce the influence of bound water, the unmodified cotton fabric powder and the modified cotton fabric powder are dried for 2 hours at 100 ℃ before infrared detection), wherein the spectral scanning ranges of samples to be detected are 400-4000 cm--1The number of scanning times: 32 times, resolution: 4cm-1。
The results are shown in FIG. 1 at 1732cm-1Corresponding to the stretching vibration peak of ester carbonyl, 1022cm-1Tensile vibration peak at C-O in C-O-C group, 1596cm-1The peak at position (A) is a stretching vibration peak of carboxyl group not participating in conversion which reacts to become carbonyl group in carboxylate, and is 2900cm-1The peak is the stretching vibration peak of methylene carbon-hydrogen bond in cellulose, and as shown in the figure, the blank cotton fabric is at 1732cm-1No corresponding stretching vibration peak is found nearby, and the modified cotton fabric has the length of 1732cm-1Corresponding stretching vibration peaks are found nearby, which indicates that the polycarboxylic acid molecules (BTCA) are subjected to esterification reaction with hydroxyl groups in cellulose after modification treatment and ester bonds are generated.
Test example 2
The microstructures of the modified cotton fabric of example 1 and the unmodified cotton fabric of comparative example 1 before dyeing were photographed by a scanning electron microscope, SEM photographs of the unmodified cotton fabric were shown in fig. 2 to 3, photographs of the modified cotton fabric were shown in fig. 4 to 5,
as shown in the figure, the modified cotton fibers are swelled, cross-linking exists among the fibers, the fiber surfaces become rough, wrinkles and sediment accumulation occur, the cotton fiber structure is damaged due to the acidity of the BTCA solution, and the BTCA has esterification reaction with a plurality of cotton fiber molecules in the modification process due to the tetracarboxyl structure so as to form a plurality of cross-links.
Test example 3
Determining zeta potentials of the modified cotton fabric of example 1 and the unmodified cotton fabric of comparative example 1 at different pH values before dyeing by using an electric solid surface analyzer SurPASS 3 and a crack method, and setting a temperature parameter to be 20 ℃;
as shown in FIG. 6, the absolute value of the zeta potential of the surface of BTCA modified cotton fabric is the largest at pH 10, and the zeta potential is-32.09 mV because BTCA treated cotton fabric has more carboxyl structures, so the surface of the cotton fabric has more negative charges and is more electronegative.
Test example 4
Determining the K/S values of A1-A7, D1-D11 and the color difference Delta E between A1-A7, D2-D11 and D1;
and (3) testing the dyed cotton fabric by using a color measuring and matching instrument to obtain the L, a, b and K/S values of the dyed cotton fabric, comparing the L, a, b and K/S values with a blank cotton fabric, and calculating the delta E by using a formula (1.1).
Figure BDA0003156741640000181
The results are shown in Table 1.
TABLE 1
Figure BDA0003156741640000182
Figure BDA0003156741640000191
As can be seen from the results in Table 1, the dyed cotton fabric obtained by the method of the invention has a small K/S value and good dye-repelling effect.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (10)

1. A method for dyeing cotton fabrics by reactive dyes is characterized by comprising the following steps:
(1) completely immersing cotton fabrics in BTCA-sodium hypophosphite mixed solution, stirring for 10-15min, wherein the ratio of the cotton fabrics to the BTCA-sodium hypophosphite mixed solution is 3-5g/100mL, then removing redundant solution by rolling, controlling the rolling residual rate of the cotton fabrics to be 96-105 wt%, then drying the cotton fabrics, then curing for 4-12min at the temperature of 140-;
(2) placing the modified cotton fabric obtained in the step (1) in reactive dye liquor with the pH value of 6-8 for dyeing at the temperature of 60-80 ℃ for 25-30min, and then sequentially washing, soaping and drying;
in the step (1), the BTCA-sodium hypophosphite mixed solution contains 8-11 wt% of BTCA, and the BTCA-sodium hypophosphite mixed solution contains 4-12 wt% of sodium hypophosphite;
in the step (2), the dosage of the reactive dye in the reactive dye solution is 0.2-1.1% o.w.f.
2. The method according to claim 1, wherein in the step (1), the stirring temperature is 20-30 ℃ and the stirring speed is 20-180 r/min.
3. The method according to claim 1, wherein in the step (1), the drying temperature is 75-85 ℃ and the drying time is 10-15 min.
4. The method according to claim 1, wherein in the step (1), the cured cotton fabric is washed using an acetic acid-ethanol mixed solution;
preferably, the concentration of acetic acid in the acetic acid-ethanol mixed solution is 0.8-1.5g/L, and the concentration of ethanol in the acetic acid-ethanol mixed solution is 0.8-1.5 g/L;
preferably, the number of washing is 2 to 4.
5. The method as claimed in claim 1, wherein, in the step (1), the temperature of the drying is 75-85 ℃ and the time of the drying is 8-12 min.
6. The method according to claim 1, wherein in step (2), the weight ratio of the modified cotton fabric to the reactive dye liquor is 1: 100;
preferably, the reactive dye is reactive yellow X-R, reactive orange K-G or reactive brilliant blue KN-R;
preferably, the reactive dye is reactive orange K-G or reactive brilliant blue KN-R;
preferably, the reactive dye is reactive brilliant blue KN-R.
7. The method as claimed in claim 1 or 6, wherein in the step (2), the reactive dye liquor further contains sodium sulfate and sodium carbonate;
preferably, the concentration of sodium sulfate in the reactive dye liquor is 8-12g/L, and the concentration of sodium carbonate in the reactive dye liquor is 8-12 g/L.
8. The method according to claim 1, wherein in step (2), the number of washing is 2 to 4.
9. The method according to claim 1 or 8, wherein in step (2), the weight ratio of the modified cotton fabric obtained in step (1) to the soaping solution is 1: 100.
10. the method according to claim 9, wherein in the step (2), the temperature of the soaping is 70-80 ℃ and the time of the soaping is 15-20 min.
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