CN110735331A - Preparation of cotton fiber anion modifier, anion modifier and dyeing process - Google Patents
Preparation of cotton fiber anion modifier, anion modifier and dyeing process Download PDFInfo
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- CN110735331A CN110735331A CN201911025126.3A CN201911025126A CN110735331A CN 110735331 A CN110735331 A CN 110735331A CN 201911025126 A CN201911025126 A CN 201911025126A CN 110735331 A CN110735331 A CN 110735331A
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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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/42—One nitrogen atom
- C07D251/44—One nitrogen atom with halogen atoms attached to the two other ring carbon atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/48—Two nitrogen atoms
- C07D251/50—Two nitrogen atoms with a halogen atom attached to the third ring carbon atom
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/445—Use of auxiliary substances before, during or after dyeing or printing
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/62—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 using compositions containing low-molecular-weight organic compounds with sulfate, sulfonate, sulfenic or sulfinic groups
- D06P1/628—Compounds containing nitrogen
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/653—Nitrogen-free carboxylic acids or their salts
- D06P1/6533—Aliphatic, araliphatic or cycloaliphatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
Abstract
The invention provides a preparation method of a cotton fiber anionic modifier, an anionic modifier and a dyeing process, belonging to the field of cotton fabric modified dyeing and solving the problems of heavy pollution caused by the modification of cotton fabric by using the existing cotton fiber cationic modifier, and the like, and the preparation method of cotton fiber anionic modifiers is characterized by comprising the following steps of adding water, crushed ice and cyanuric chloride into a beaker, stirring for 1-2 hours, adding water and sulfanilic acid into a second beaker, regulating the pH value to be 5-6 by using hydrochloric acid, enabling the solution to be transparent, dripping sulfanilic acid hydrochloride into the second beaker into a beaker, finishing dripping for 1-2 hours, keeping the temperature below 5 ℃, carrying out condensation reaction until the reaction is finished, regulating the pH value to be 7-8 by using sodium bicarbonate, adding 25-40% of neutral salt according to volume, salting out, stirring for 1-2 hours, carrying out filter pressing, drying a filter cake, and obtaining the advantages of small pollution and the like.
Description
Technical Field
The invention belongs to the field of cotton cloth modified dyeing, and particularly relates to a preparation method of cotton fiber anionic modifiers, a cotton fiber anionic modifier and a cotton cloth modified dyeing process thereof.
Background
Cationic dyes (Cationic dyes) are kinds of textile dyes, also called basic dyes and basic dyes.
At present, the cotton cloth is dyed by mainly using reactive dyes, but when the reactive dyes are in dip dyeing, a large amount of neutral salt needs to be added to promote dyeing, the dye-uptake and the color fixation rate are not high, about 70 percent of the dye-uptake and the color fixation rate are , the hydrolytic dyes and the neutral salt in dyeing residual liquid are mixed, the concentration is high, great pressure is brought to the subsequent dyeing sewage treatment, and the method does not accord with the clean and environment-friendly production concept advocated by the country.
In order to solve the serious problems, the dyeing experts reduce the use of a large amount of neutral salt by replacing neutral salt with substitute salt, and do not use or use little neutral salt by using a cotton fiber cationic modifier, but the obtained effect is , the former has limited salt reduction range, but the production cost is increased by using the cotton fiber cationic modifier, the phenomena of uneven dyeing, colored patterns and the like are easy to occur, the key is that the chroma in dyeing residual liquid is high, the COD of the residual liquid is high, and the cationic modified working solution becomes a new dyeing sewage source after being used.
Disclosure of Invention
The th object of the invention is to solve the above problems in the prior art and provide a preparation method of cotton fiber anionic modifiers, the th object of the invention is to provide a modified dyeing process of cotton cloth.
The th object of the invention can be realized by the following technical scheme that the preparation method of cotton fiber anion modifiers is characterized by comprising the following steps:
s01, adding water, crushed ice and cyanuric chloride into a beaker, stirring for 1-2 hours, adding water and sulfanilic acid into a second beaker, and adjusting the pH value to 5-6 by hydrochloric acid to ensure that the solution is transparent;
s02, dripping sulfanilic acid hydrochloride in the second beaker into the beaker, finishing dripping within 1-2 hours, keeping the temperature below 5 ℃, and carrying out condensation reaction until the reaction is finished;
s03: adjusting the pH value of the system to 7-8 by using sodium bicarbonate; adding 25-40% neutral salt by volume for salting out; stirring for 1-2 hours, carrying out filter pressing, and drying a filter cake to obtain the filter cake.
Preferably, the molar ratio of cyanuric chloride to sulfanilic acid is 0.8-1.2: 0.8-1.2, in step S01, cyanuric chloride and sulfanilic acid are mixed in a molar ratio of 0.8-1.2: adding in the ratio of 0.8-1.2.
Preferably, the molar ratio of cyanuric chloride to sulfanilic acid is 0.5-1.1: 0.9-2.4, the cyanuric chloride and sulfanilic acid are added according to the molar ratio of 0.5-1.1: 0.45-1.2 in step S01, and step S04 is further included between step S02 and step S03, S04: adding the rest sulfanilic acid into a th beaker, adjusting the pH value to 6-6.5 by using sodium bicarbonate, standing overnight, heating to 20-25 ℃ the next day, adjusting the pH value to 5-6 by using sodium bicarbonate, and reacting for 6 hours.
Preferably, in step S01, stirring is performed for 1 hour; in step S02, the dropping is completed within 1 hour; in step S03, the mixture was stirred for 1 hour.
Preferably, in step S03, the filter cake is dried at 85 ℃.
The second object of the invention can be realized by the following technical scheme that cotton fiber anion modifiers prepared by the preparation method are characterized in that the structural formula of the cotton fiber anion modifier is shown as the formula (I):
r is-Cl or
cotton cloth modified dyeing process adopting the cotton fiber anionic modifier is characterized by comprising the following steps:
(1) preparing a modified working solution from a cotton fiber anion modifier and neutral salt; wetting and squeezing cotton cloth, putting into a modified working solution, treating for 10-20 minutes, heating to 20-30 ℃, adding sodium carbonate, performing modification treatment for 30-60 minutes, taking out the cotton cloth, washing with cold water until the pH value of the cloth surface is neutral, and obtaining the modified cotton cloth;
(2) preparing a dyeing working solution from a cationic dye, glacial acetic acid, sodium acetate and a leveling agent, putting the modified cotton cloth obtained in the step S02 into the dyeing working solution, heating to 90-100 ℃, dyeing for 30-60 minutes, taking out the cotton cloth, washing with cold water, soaping, washing with cold water, and drying.
Preferably, in step S01, the cotton fiber anion modifier 1-3% (o.w.f), the neutral salt 20-40g/L, the sodium carbonate 10-15g/L, the bath ratio 10: 1.
preferably, in step S02, the cationic dye is 1-3% (o.w.f), the glacial acetic acid is 1-3% (o.w.f), the sodium acetate is 1-3% (o.w.f), the leveling agent is 0.5-1% (o.w.f), the bath ratio is 10: 1.
the working principle of the invention is as follows:
when the total molar ratio of the cyanuric chloride to the sulfanilic acid is 0.8-1.2: 0.8-1.2, the cyanuric chloride and the sulfanilic acid are all added in step S01, and then step S02 and step S03 are sequentially carried out, so that low-temperature cotton fiber anion modifiers are obtained, as shown in formula (I-1), and the chemical reaction formula is as follows:
when the total molar ratio of cyanuric chloride to sulfanilic acid is 0.5-1.1: 0.9-2.4, in step S01, cyanuric chloride and sulfanilic acid are added in a molar ratio of 0.5-1.1: 0.45-1.2, i.e. half of sulfanilic acid is added, in step S02, SO4 and SO3 are sequentially carried out, in step S04, the beaker is added with the rest half sulfanilic acid, the pH value is adjusted to 6-6.5 by sodium bicarbonate, the temperature is raised to 20-25 ℃ the next day, the pH value is adjusted to 5-6 by sodium bicarbonate, and the reaction is carried out for 6 hours, finally high-temperature type cotton fiber anion modifiers are obtained, as shown in formula (I-2), and the chemical reaction is as follows:
selecting 1-3% (o.w.f) of low-temperature cotton fiber anion modifier (I-1) or high-temperature cotton fiber anion modifier (I-2), preparing a modified working solution with neutral salt, wetting and squeezing cotton cloth, then putting the cotton cloth into the modified working solution, treating for 10-20 minutes, heating to 20-30 ℃, adding sodium carbonate, performing modification treatment for 30-60 minutes, taking out the cotton cloth, washing the cotton cloth with cold water until the pH value of the cloth surface is neutral, and obtaining the modified cotton cloth, wherein the neutral salt is 20-40g/L, the sodium carbonate is 10-15g/L, and the bath ratio is 10: 1 (o.w.f), which is words in the printing and dyeing process, and refers to the concentration unit and the weight ratio of dye to the weight of the fabric.
And preparing a dyeing working solution from the cationic dye, glacial acetic acid, sodium acetate and a leveling agent, putting the modified cotton cloth into the dyeing working solution, slowly heating to 90-100 ℃, dyeing for 30-60 minutes, taking out the cotton cloth, washing with cold water, soaping, washing with cold water, and drying. 1-3% (o.w.f) of cationic dye, 1-3% (o.w.f) of glacial acetic acid, 1-3% (o.w.f) of sodium acetate, 0.5-1% (o.w.f) of leveling agent, and bath ratio of 10: 1.
compared with the prior art, the invention has the following advantages:
1. the invention adopts cyanuric chloride and sulfanilic acid to prepare two cotton fiber anionic modifiers, and the anionic modifiers are used for carrying out anionic modification on cotton fibers to ensure that the cotton fibers contain sulfonic anionic groups and then are dyed by cationic dyes, so that the cotton cloth can obtain bright dyeing effect in aspects, and the cotton cloth has good fastness to washing and sunlight, and in addition, aspect can obtain very high dyeing rate which is far higher than the dyeing rate and the fixation rate of the cotton cloth dyed by direct dyes and reactive dyes, so that the dyeing residual liquid is clear, almost contains no dyes and has lower COD (chemical oxygen demand) residual liquid.
2. The low-temperature modification process for modifying cotton cloth into cotton cloth by using the low-temperature cotton fiber anionic modifier has the advantages of energy conservation; the high-temperature modification process for modifying cotton cloth into cotton cloth by using the high-temperature cotton fiber anionic modifier has the advantages of deeper and thicker dyeing and brighter color light. The modified working solution is neutralized after being used, water is added for dilution to adjust the concentration of neutral salt, and then the cotton fiber anion modifier is added, so that the modified working solution can be used as the next modified working solution.
2. The preparation process is simple and can be completed in a common reaction kettle.
Detailed Description
The following are specific examples of the present invention, and the technical solution of the present invention is further described in , but the present invention is not limited to these examples.
Example 1
1. Laboratory preparation formula of low-temperature cotton fiber anion modifier (I-1)
Cyanuric chloride (99%) 186 portions
182 portions of sulfanilic acid (95 percent)
2. Laboratory preparation process of low-temperature cotton fiber anion modifier A
S01, adding water, crushed ice and cyanuric chloride into a beaker, stirring for 1 hour, adding water and sulfanilic acid into a second beaker, and adjusting the pH value to be between 5 and 6 by hydrochloric acid to ensure that the solution is transparent;
s02, slowly dripping sulfanilic acid hydrochloride in the second beaker into the beaker, finishing dripping for 1 hour, controlling the temperature to be below 5 ℃, carrying out condensation reaction, and determining the reaction end point to determine the end of the reaction (taking a sample on filter paper, dripping an amino reagent, and obtaining the reaction end point when the sample does not show yellow);
s03, adjusting the pH value of the system to 7-8 by baking soda (sodium bicarbonate), adding 25-40% neutral salt by volume, salting out, stirring for 1 hour, performing filter pressing, and drying the filter cake at 85 ℃ to obtain low-temperature cotton fiber anion modifiers (I-1).
3. The cotton cloth low-temperature modification process formula comprises the following steps:
low-temperature type cotton fiber anion modifier (I-1) 2% (o.w.f)
Neutral salt 20g/L
10g/L of soda ash (namely sodium carbonate)
Bath ratio: 10: 1
4. The cotton cloth low-temperature modification process flow comprises the following steps:
preparing a modified working solution from the cotton fiber anion modifier and neutral salt, wetting and squeezing cotton cloth, putting the cotton cloth into the modified working solution, treating for 15 minutes, heating to 25 ℃, adding soda ash, carrying out modification treatment for 30-60 minutes, taking out the cotton cloth, and washing with cold water until the pH value of the cloth surface is neutral.
5. The dyeing process formula of the cotton cloth cationic dye comprises the following steps:
cationic brilliant red X-GRL 2% (o.w.f)
Glacial acetic acid 2% (o.w.f)
Sodium acetate 1% (o.w.f)
Levelling agent 12270.5% (o.w.f)
Bath ratio: 10: 1
6. The dyeing process formula of the cotton cloth cationic dye comprises the following steps:
and (3) after the cationic dye, glacial acetic acid, sodium acetate and a leveling agent 1227 are prepared into a dyeing working solution, putting the modified cotton cloth into the dyeing working solution, slowly heating to 95 ℃, dyeing for 30-60 minutes, taking out the cotton cloth, washing with cold water, soaping, washing with cold water, and drying.
7. Color fastness to washing
And (3) carrying out a color fastness to washing test on the dyed cotton cloth according to the test method (2) in GB/T392 l-2008 'color fastness to washing test for textile color fastness to soaping'. The color fastness to washing was judged according to the level of sample discoloration and the level of lining fabric staining, and the test results are shown in Table 1.
TABLE 1 cationic brilliant red X-GRL dyed cotton cloth color fastness to washing test results
| Cationic brilliant red X-GRL | |
| Fastness to fading | Grade 5 |
| Color fastness to staining | Grade 5 |
8. Color fastness to sunlight test
The color fastness to sunlight of the dyed cotton cloth is tested according to a test method in AATCC TM16-2003 (Artificial light color fastness to xenon arc) of textiles, and the color fastness to sunlight is judged according to the color change grade of the fabric to be subjected to sunlight, and the test result is shown in Table 2.
TABLE 2 cationic Brilliant Red X-GRL dyed cotton cloth color fastness to sunlight test results
| Cationic brilliant red X-GRL | |
| Color fastness to light for 20h | Grade 6 |
| Color fastness to light for 40h | 5-6 stages |
Example 2
1. Laboratory preparation formula of high-temperature cotton fiber anion modifier (I-2)
Cyanuric chloride (99%) 186 portions
364 portions of sulfanilic acid (95 percent)
2. Laboratory preparation process of high-temperature cotton fiber anion modifier B
S01, adding water, crushed ice and cyanuric chloride into a beaker, stirring for 1 hour, adding water and 1/2 sulfanilic acid into a second beaker, and adjusting the pH value to 5-6 with hydrochloric acid to ensure that the solution is transparent;
s02: slowly dripping sulfanilic acid hydrochloride in the beaker B into the beaker A, and finishing dripping within 1 hour; controlling the temperature below 5 ℃, carrying out condensation reaction, and determining the reaction end point by measuring the reaction end point (taking a sample on filter paper, dropwise adding an amino reagent, and determining that no yellow color is displayed as the reaction end point);
s04: adding 1/2 sulfanilic acid into the beaker A, adjusting the pH value to 6-6.5 with baking soda, standing overnight, heating to 20-25 ℃ the next day, adjusting the pH value to 5-6 with baking soda, and reacting for 6 hours;
s03, finally adjusting the pH value of the system to 7-8 by baking soda, adding 25-40% neutral salt by volume, salting out, stirring for 1 hour, performing filter pressing, and drying the filter cake at 85 ℃ to obtain high-temperature cotton fiber anion modifiers B.
3. The cotton cloth high-temperature modification process formula comprises the following steps:
high-temperature type cotton fiber anion modifier (I-2) 2% (o.w.f)
Neutral salt 30g/L
15g/L of soda ash
Bath ratio: 10: 1
4. The cotton cloth high-temperature modification process flow comprises the following steps:
preparing a modified working solution from the cotton fiber anion modifier and neutral salt, wetting and squeezing cotton cloth, putting the cotton cloth into the modified working solution, treating for 15 minutes, heating to 90 ℃, adding soda ash, carrying out modification treatment for 30-60 minutes, taking out the cotton cloth, and washing with cold water until the pH value of the cloth surface is neutral.
5. The dyeing process formula of the cotton cloth cationic dye comprises the following steps:
cationic brilliant blue X-GRL 1% (o.w.f)
Glacial acetic acid 2% (o.w.f)
Sodium acetate 1% (o.w.f)
Levelling agent 12270.5% (o.w.f)
Bath ratio: 10: 1
6. The dyeing process formula of the cotton cloth cationic dye comprises the following steps:
and (3) after the cationic dye, glacial acetic acid, sodium acetate and a leveling agent 1227 are prepared into a dyeing working solution, putting the modified cotton cloth into the dyeing working solution, slowly heating to 95 ℃, dyeing for 30-60 minutes, taking out the cotton cloth, washing with cold water, soaping, washing with cold water, and drying.
7. Color fastness to washing
And (3) carrying out a color fastness to washing test on the dyed cotton cloth according to the test method (2) in GB/T392 l-2008 'color fastness to washing test for textile color fastness to soaping'. The color fastness to washing was judged according to the level of sample discoloration and the level of lining fabric staining, and the test results are shown in Table 3.
TABLE 3 cationic brilliant blue X-GRL dyed cotton cloth color fastness to washing test results
| Cationic brilliant blue X-GRL | |
| Fastness to fading | Grade 5 |
| Color fastness to staining | Grade 5 |
8. Color fastness to sunlight test
The color fastness to sunlight of the dyed cotton cloth is tested according to a test method in AATCC TM16-2003 (Artificial light color fastness to xenon arc) of textiles, and the color fastness to sunlight is judged according to the color change grade of the fabric to be subjected to sunlight, and the test result is shown in Table 4.
TABLE 4 cationic brilliant blue X-GRL dyed cotton cloth color fastness to sunlight test results
| Cationic red X-GRL | |
| Color fastness to light for 20h | Grade 5 |
| Color fastness to light for 40h | 4-5 stages |
Example 3 color fastness to washing test
And (3) carrying out a washing fastness test on the cotton cloth dyed by the dye with the concentration of 5% according to the test method (2) in GB/T392 l-2008 'textile color fastness test soaping fastness'. The color fastness to washing was judged according to the level of sample discoloration and the level of lining fabric staining, and the test results are shown in Table 5.
TABLE 5 color fastness to washing test results
| Sun-fast active blue 1# | Sun-fast active blue 2# | Sun-fast active blue 3# | Sun-fast active blue 4# | |
| Fastness to fading | 4.5 stage | 4.5 stage | 4.5 stage | 4.5 stage |
| Color fastness to staining | 4.5 stage | 4.5 stage | 4.5 stage | 4.5 stage |
Example 4 crock fastness test
The rubbing color fastness test is carried out on the cotton cloth dyed by the dye with the concentration of 5 percent according to the test method in GB/T3920-. The crocking fastness was judged according to the degree of staining of the rubbed fabric and the test results are shown in Table 6.
TABLE 6 rubbing fastness test results
| Sun-fast active blue 1# | Sun-fast active blue 2# | Sun-fast active blue 3# | Sun-fast active blue 4# | |
| Colour fastness to dry rubbing | 4.5 stage | 4.5 stage | 4.5 stage | 4.5 stage |
| Color fastness to wet rubbing | Grade 3.5 | Grade 3.5 | Grade 3.0 | Grade 3.5 |
Example 5 color fastness to sunlight test
The cotton cloth dyed with 5% dye concentration is subjected to a color fastness to sunlight test according to a test method in AATCC TM16-2003 (Artificial light color fastness to xenon arc) and the color fastness to sunlight is judged according to the color change grade of the fabric to be subjected to sunlight test, and the test result is shown in Table 7.
TABLE 7 test results of color fastness to sunlight
| Sun-fast active blue 1# | Sun-fast active blue 2# | Sun-fast active blue 3# | Sun-fast active blue 4# | |
| Color fastness to light for 20h | Grade 6 | Grade 6 | 5-6 stages | 5-6 stages |
| Color fastness to light for 40h | 5-6 stages | 5-6 stages | 5-6 stages | 5-6 stages |
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (9)
- The preparation method of the cotton fiber anionic modifier is characterized by comprising the following steps:s01, adding water, crushed ice and cyanuric chloride into a beaker, stirring for 1-2 hours, adding water and sulfanilic acid into a second beaker, and adjusting the pH value to 5-6 by hydrochloric acid;s02, dripping sulfanilic acid hydrochloride in the second beaker into the beaker, finishing dripping within 1-2 hours, keeping the temperature below 5 ℃, and carrying out condensation reaction until the reaction is finished;s03: adjusting the pH value of the system to 7-8 by using sodium bicarbonate; adding 25-40% neutral salt by volume for salting out; stirring for 1-2 hours, carrying out filter pressing, and drying a filter cake to obtain the filter cake.
- 2. The method of kinds of anionic modifiers for cotton fiber according to claim 1, wherein the molar ratio of cyanuric chloride to sulfanilic acid is 0.8-1.2: 0.8-1.2, and in step S01, cyanuric chloride and sulfanilic acid are added in a molar ratio of 0.8-1.2: 0.8-1.2.
- 3. The method for preparing anionic modifiers for cotton fibers according to claim 1, wherein the molar ratio of cyanuric chloride to sulfanilic acid is 0.5-1.1: 0.9-2.4, cyanuric chloride and sulfanilic acid are added in the step S01 in the molar ratio of 0.5-1.1: 0.45-1.2, and the steps S02 and S03 further include the steps S04, S04, adding the rest sulfanilic acid into the beaker, adjusting the pH value to 6-6.5 with sodium bicarbonate, standing overnight, heating to 20-25 ℃ the next day, adjusting the pH value to 5-6 with sodium bicarbonate, and reacting for 6 hours.
- 4. The method for preparing anionic modifiers for cotton fibers according to claim 1, wherein the stirring is performed for 1 hour in step S01, the dropwise addition is performed for 1 hour in step S02, and the stirring is performed for 1 hour in step S03.
- 5. The method for preparing kinds of anionic modifiers of cotton fiber according to claim 1, wherein in step S03, the filter cake is dried at 85 ℃.
- 6, cotton fiber anionic modifier prepared by the method for preparing cotton fiber anionic modifier according to any of claims 1-5, wherein the structural formula of the cotton fiber anionic modifier is shown in formula (I):r ═ Cl or R ═
- 7, cotton cloth modified dyeing process using cotton fiber anionic modifying agents as claimed in claim 6, characterized by comprising the following steps:(1) preparing a modified working solution from a cotton fiber anion modifier and neutral salt; wetting and squeezing cotton cloth, putting into a modified working solution, treating for 10-20 minutes, heating to 20-30 ℃, adding sodium carbonate, performing modification treatment for 30-60 minutes, taking out the cotton cloth, washing with cold water until the pH value of the cloth surface is neutral, and obtaining the modified cotton cloth;(2) preparing a dyeing working solution from a cationic dye, glacial acetic acid, sodium acetate and a leveling agent, putting the modified cotton cloth obtained in the step S02 into the dyeing working solution, heating to 90-100 ℃, dyeing for 30-60 minutes, taking out the cotton cloth, washing with cold water, soaping, washing with cold water, and drying.
- 8. The kinds of cotton cloth modified dyeing process of claim 7, wherein in step S01, the cotton fiber anionic modifier 1-3%, the neutral salt 20-40g/L, the sodium carbonate 10-15g/L, the bath ratio is 10: 1.
- 9. The kinds of cotton cloth modified dyeing process of claim 7, wherein in step S02, the cationic dye is 1-3%, the glacial acetic acid is 1-3%, the sodium acetate is 1-3%, the leveling agent is 0.5-1%, and the bath ratio is 10: 1.
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| CN114045599A (en) * | 2021-11-02 | 2022-02-15 | 晋江七匹狼服装制造有限公司 | Environment-friendly yarn-dyed check fabric and processing technology thereof |
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| CN101864676A (en) * | 2010-06-08 | 2010-10-20 | 上海工程技术大学 | Cation modified dyeing method of ceiba fiber textiles |
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