CN109371718B - Method for dyeing cellulose acetate fibers by berberine - Google Patents
Method for dyeing cellulose acetate fibers by berberine Download PDFInfo
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- CN109371718B CN109371718B CN201811264298.1A CN201811264298A CN109371718B CN 109371718 B CN109371718 B CN 109371718B CN 201811264298 A CN201811264298 A CN 201811264298A CN 109371718 B CN109371718 B CN 109371718B
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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
- D06P1/655—Compounds containing ammonium groups
- D06P1/66—Compounds containing ammonium groups containing quaternary ammonium groups
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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
- D06P1/64—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 without sulfate or sulfonate groups
- D06P1/642—Compounds containing nitrogen
- D06P1/6426—Heterocyclic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- 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
- D06P3/82—Textiles which contain different kinds of fibres
- D06P3/8204—Textiles which contain different kinds of fibres fibres of different chemical nature
- D06P3/8266—Textiles which contain different kinds of fibres fibres of different chemical nature mixtures of fibres containing hydroxyl and nitrile groups
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Abstract
The invention discloses a method for dyeing cellulose acetate fibers by berberine, which is characterized by comprising the following steps: pretreating the cellulose acetate fiber by using ionic liquid to swell the cellulose acetate fiber so as to facilitate the adsorption and diffusion of nitrilase and berberine; and nitrilase is used for treating the cellulose acetate to hydrolyze part of cyano groups into carboxylic acid, so that the treated cellulose acetate has electrostatic attraction to cation berberine, and the dyeing base for dyeing the cellulose acetate on the berberine is increased, thereby improving the color yield and the color fastness. The invention provides a process for dyeing berberine on vinegar green fibers, which is ecological and health-care and has better color yield.
Description
The technical field is as follows:
the invention relates to a method for dyeing cellulose acetate fibers, in particular to a method for dyeing cellulose acetate fibers by berberine.
Background art:
the berberine is a common isoquinoline alkaloid, has a quaternary ammonium structure, belongs to quaternary ammonium alkaloids, has good water solubility, is non-toxic and harmless, is ecological and environment-friendly, and has antibacterial and health-care effects. At present, the action of berberine is mainly used in the aspects of biological pharmacy and the like.
The cellulose acetate fiber is a novel fiber prepared by organically combining natural plant macromolecules and synthetic elements, not only keeps the characteristics of bulkiness, softness, smoothness, high strength and the like of acrylic fiber, but also has good dimensional stability, heat retention property and antistatic property, and is mainly applied to the fields of underwear, sweaters, exterior decoration, home textiles and the like.
At present, a dyeing process for applying berberine to the cellulose acetate fibers is not developed, how to fully utilize excellent berberine dye, and the research on a dyeing processing process and a method for the cellulose acetate fibers is urgent.
The invention content is as follows:
the invention aims to solve the technical problem of providing a method for dyeing cellulose acetate fibers by berberine.
The technical scheme adopted by the invention is as follows:
a method for dyeing cellulose acetate fibers by berberine is characterized by comprising the following steps:
(1) pretreating vinegar green fibers: firstly, treating the cellulose acetate fibers by using ionic liquid, and then treating the cellulose acetate fibers by using nitrilase;
(2) dyeing the acetate blue fiber: and (3) dyeing the pretreated vinegar green fiber by using berberine.
Better dye uptake and dye fastness can be obtained by adopting the following preferred scheme:
the pretreatment process of the step (1) comprises the following steps: (1) the ionic liquid pretreatment process comprises the following steps: the cellulose acetate fiber is prepared by mixing cellulose acetate fiber in 80-95% of ionic liquid by mass percent in a bath ratio of 1: treating at 45, 50-70 deg.C for 20-50min, taking out sample, washing with anhydrous ethanol, and washing with water. (2) And (3) nitrilase treatment process: nitrilase was used at 4% owf-10% owf, pH 7.0, bath ratio 1: treating at 40, 40-60 deg.C for 20-50min, washing with water, and oven drying.
The ionic liquid is preferably i-allyl-3-methylimidazolium chloride (tradename, kokataca, inc. in lanzhou).
The dyeing process in the step (2) comprises the following steps: (1) the process prescription is as follows: the berberine is used in 1-6% owf, the pH value is 3-9, the bath ratio is 1: 30, of a nitrogen-containing gas; (2) the process conditions are as follows: dyeing at room temperature, heating to 70-100 ℃ at 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
The best scheme is as follows:
(1) pretreatment, (1) ionic liquid pretreatment process: the cellulose acetate fiber is prepared by mixing 90 mass percent of I-allyl-3-methylimidazolium chloride ionic liquid in a bath ratio of 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. (2) And (3) nitrilase treatment process: nitrilase was used at 6% owf, pH 7.0, bath ratio 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
(2) The dyeing process comprises the following steps: berberine is used in an amount of 1-7% owf (according to the required color depth), the pH value is 4, the bath ratio is 1: and (3) dyeing at room temperature, heating to 90 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
The beneficial effects and principles of the invention are as follows:
(1) the invention uses the antibacterial and environment-friendly berberine for the dyeing processing of the vinegar green fiber, realizes the ecological dyeing of the vinegar green fiber, simultaneously expands the application field of the berberine, and has very obvious effects on the aspects of dyeing quality and environmental protection because the berberine has the characteristics of safety, environmental protection, antibiosis and health care.
(2) The method comprises the steps of firstly adopting ionic liquid and nitrilase to pretreat the cellulose acetate, and then adopting berberine to dye the pretreated cellulose acetate. The cellulose acetate fiber has compact molecular crystalline structure and the nitrilase is difficult to enter the fiber due to the hydrogen bond action between the cyano groups on the adjacent macromolecules, the hydrogen bond between the macromolecular chains of the cellulose acetate fiber is firstly opened by adopting the treatment of the ionic liquid, the cellulose acetate fiber swells, the nitrilase is easy to permeate into the cellulose acetate fiber, the cyano groups on the cellulose acetate fiber molecules are hydrolyzed into carboxyl groups, the adsorption capacity and the electrostatic attraction to the cation berberine are enhanced, the dyeing percentage and the dyeing fastness of the berberine are improved, and the K/S value and the dye fastness of the berberine meet the requirements of the serviceability.
The present invention is described in further detail below with reference to examples:
the specific implementation mode is as follows:
example 1: influence of different pretreatment processes on dyeing effect of cellulose acetate fibers
The method comprises the following steps of (1) treating by using an independent ionic liquid, (2) treating by using an independent nitrilase, and (3) pretreating the cellulose acetate by using an ionic liquid and nitrilase combined process, and dyeing the three kinds of pretreated cellulose acetate by using berberine, wherein the method comprises the following steps:
step a, pretreatment process:
(1) the single ionic liquid treatment process comprises the following steps: the mass fraction of the allyl-3-methylimidazole chloride ionic liquid is 90 percent, and the bath ratio is 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water.
(2) The single nitrilase treatment process comprises the following steps: nitrilase was used at 6% owf, pH 7.0, bath ratio 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
(3) The combined pretreatment process of the ionic liquid and the nitrilase comprises the following steps: the mass fraction of the allyl-3-methylimidazole chloride ionic liquid is 90 percent, and the bath ratio is 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. ② the nitrilase dosage is 6% owf, pH is 7.0, bath ratio is 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
Step b, dyeing process:
berberine is used in 3% owf, pH is 4, bath ratio is 1: and (3) dyeing at room temperature, heating to 90 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
The three different pretreated vinegar cyan fibers and the non-pretreated vinegar cyan fibers are dyed by berberine according to the dyeing process, and K/S value tests are respectively carried out, and the results are shown in Table 1.
Table 1, comparison of the dyeing properties of non-pretreated acetocyan fibers with different pretreated fibers.
Sample (I) | K/S |
Without pretreatment | 6.4165 |
Individual ionic liquid treatment | 6.8543 |
Nitrilase treatment alone | 7.0157 |
Combined pretreatment of ionic liquid and nitrilase | 8.6242 |
As can be seen from table 1: 1. after pretreatment, the K/S value of the cellulose acetate blue fiber dyeing is increased, and the color yield is increased; 2. the combined pretreatment process of the ionic liquid and the nitrilase has better effect compared with the ionic liquid treatment/nitrilase treatment alone, because: firstly, hydrogen bonds among macromolecular chains of the cellulose acetate fibers are opened by adopting ionic liquid treatment, the cellulose acetate fibers swell, nitrilase easily permeates into the cellulose acetate fibers, cyano groups on molecules of the cellulose acetate fibers are hydrolyzed into carboxyl groups, the adsorption capacity and the electrostatic attraction to cationic berberine are enhanced, and the dye-uptake percentage and the dye fastness of the berberine are improved.
Example 2: influence of the dosage of the ionic liquid on the dyeing performance of the acetocyan fiber.
A method for dyeing cellulose acetate fibers by berberine comprises the following steps:
step a, pretreatment process: the mass fraction of the allyl-3-methylimidazolium chloride ionic liquid is 80-95%, and the bath ratio is 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. ②, the nitrilase dosage is 6% owf, the pH is 7.0, the bath ratio is 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
Step b, dyeing process: berberine is used in 3% owf, pH is 4, bath ratio is 1: and (3) dyeing at room temperature, heating to 90 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
By adopting the process, the dosage of the I-allyl-3-methylimidazolium chloride ionic liquid is adjusted, and the influence on the dyeing property of the acetocyan fiber is tested, and the result is shown in table 2.
Table 2 effect of ionic liquid dosage on dyeing performance.
Amount of Ionic liquid (%) | K/S |
80 | 8.3881 |
85 | 8.5414 |
90 | 8.6242 |
95 | 8.6611 |
As can be seen from table 2: within a certain range, the K/S value is increased along with the increase of the dosage of the ionic liquid, and the color yield is increased. When the dosage of the ionic liquid is more than 90%, the dosage is continuously increased, the change of the K/S value is not large, economic factors are comprehensively considered, and when the dosage of the ionic liquid is 90%, the effect is optimal.
Example 3: the influence of the amount of nitrilase on the dyeing properties of acetocyan fibers.
A method for dyeing cellulose acetate fibers by berberine comprises the following steps:
step a, pretreatment process: the mass fraction of the allyl-3-methylimidazole chloride ionic liquid is 90 percent, and the bath ratio is 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. ② the nitrilase dosage is 4-10% owf, pH is 7.0, bath ratio is 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
Step b, dyeing process: berberine is used in 3% owf, pH is 4, bath ratio is 1: and (3) dyeing at room temperature, heating to 90 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
The above process was used to adjust the amount of nitrilase used and to test its effect on staining performance as shown in table 3.
TABLE 3 influence of nitrilase dosage on the dyeing properties.
Nitrilase amount (% owf) | K/S |
4 | 7.9154 |
6 | 8.6242 |
8 | 8.7645 |
10 | 8.8713 |
As can be seen from table 3: the K/S value increases with increasing nitrilase dosage, and the color yield does not change much when the nitrilase dosage exceeds 6% owf.
Example 4: the influence of the berberine amount on the dyeing performance.
A method for dyeing cellulose acetate fibers by berberine comprises the following steps:
step a, pretreatment process: the mass fraction of the allyl-3-methylimidazole chloride ionic liquid is 90 percent, and the bath ratio is 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. ② the nitrilase dosage is 6% owf, pH is 7.0, bath ratio is 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
Step b, dyeing process: the berberine is used in 1-7% owf, the pH value is 4, the bath ratio is 1: and (3) dyeing at room temperature, heating to 90 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
The above process was used to adjust the berberine dose and test its effect on staining performance as shown in table 4.
Table 4, effect of berberine dosage on staining performance.
As can be seen from table 4: with the increase of the using amount of the berberine, the K/S value is increased, and the color yield is increased. The specific dosage is determined according to the required color depth during dyeing, and the required berberine dosage is small during dyeing of light color; when the color is dyed in dark color, the consumption of the berberine is large.
Example 5: influence of dyeing pH on dyeing properties.
A method for dyeing cellulose acetate fibers by berberine comprises the following steps:
step a, pretreatment process: the mass fraction of the allyl-3-methylimidazole chloride ionic liquid is 90 percent, and the bath ratio is 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. ② the nitrilase dosage is 6% owf, pH is 7.0, bath ratio is 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
Step b, dyeing process: the berberine dosage is 3% owf, the pH value is 3-11, the bath ratio is 1: and (3) dyeing at room temperature, heating to 90 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
The above process was used to adjust different pH and test its effect on staining performance as shown in table 5.
Table 5 effect of dyeing pH on dyeing performance.
pH | K/S |
3 | 8.6723 |
4 | 8.6242 |
5 | 8.6049 |
7 | 8.6352 |
9 | 8.0116 |
11 | 6.4384 |
As can be seen from table 5: the dyeing pH values are different, the change of the K/S value is large, and the color yield is large under the acidic condition; under alkaline conditions, the color yield is reduced, and the color light is changed, which is caused by the change of the molecular structure of the berberine under alkaline conditions.
Example 6: the effect of different dyeing temperatures on dyeing performance.
A method for dyeing cellulose acetate fibers by berberine comprises the following steps:
step a, pretreatment process: the mass fraction of the allyl-3-methylimidazole chloride ionic liquid is 90 percent, and the bath ratio is 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. ② the nitrilase dosage is 6% owf, pH is 7.0, bath ratio is 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
Step b, dyeing process: berberine is used in 3% owf, pH is 4, bath ratio is 1: dyeing at room temperature, heating at 1 deg.C/min, maintaining at 70-100 deg.C for 60 min, washing with water, and oven drying.
The above process was used to adjust different temperatures and test their effect on dyeing performance as shown in table 6.
Table 6, effect of dyeing temperature on dyeing performance.
Dyeing temperature (. degree.C.) | K/S |
70 | 6.7051 |
80 | 8.1873 |
90 | 8.6242 |
100 | 8.4319 |
As can be seen from table 6: and (3) further increasing the K/S value with the increase of the dyeing temperature, and continuing to increase the temperature until the K/S value is maximum under the dyeing condition of 90 ℃, so that the color yield is slightly reduced.
Example 7: and (5) comparing the color fastness.
The process comprises the following steps:
step a, pretreatment process: the mass fraction of the allyl-3-methylimidazole chloride ionic liquid is 90 percent, and the bath ratio is 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. ② the nitrilase dosage is 6% owf, pH is 7.0, bath ratio is 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
Step b, dyeing process: berberine is used in 3% owf, pH is 4, bath ratio is 1: and (3) dyeing at room temperature, heating at 1 ℃/min, keeping the temperature at 90 ℃ for 60 minutes, washing with water, and drying.
The results of comparing the colorfastness of the above examples with that of the samples not pretreated are shown in Table 7.
TABLE 7 soaping fastness
As can be seen from Table 7, the fastness to soaping of the dyed sample is slightly improved by carrying out combined pretreatment on the acetocyan fiber by the ionic liquid and the nitrilase and then carrying out the berberine dyeing.
And (3) analysis and summary:
1. according to the method, firstly, the cellulose acetate is pretreated by the ionic liquid and nitrilase, and then the pretreated cellulose acetate is dyed by the berberine, so that the color yield and the color fastness of the berberine on the cellulose acetate are effectively improved.
2. Through the process control of the ionic liquid, nitrilase, the consumption of the berberine, the dyeing pH value, the dyeing temperature and the like, the dyeing rate of the berberine can be effectively improved, and the ecological dyeing of the berberine on the cellulose acetate is finally realized.
3. The comprehensive optimal embodiment is as follows:
the pretreatment process comprises (1) ionic liquid treatment: the cellulose acetate fiber is prepared by mixing 90 mass percent of I-allyl-3-methylimidazolium chloride ionic liquid in a bath ratio of 1: treating at 45 deg.C and 60 deg.C for 30min, taking out sample, washing with anhydrous ethanol for 3 times, and washing with water. (2) Nitrilase treatment: nitrilase was used at 6% owf, pH 7.0, bath ratio 1: treating at 40 and 45 deg.C for 30min, washing with water, and oven drying.
The dyeing process comprises the following steps: berberine is used in an amount of 1-7% owf (according to the required color depth), the pH value is 4, the bath ratio is 1: and (3) dyeing at room temperature, heating to 90 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
Claims (4)
1. A method for dyeing cellulose acetate fibers by berberine is characterized by comprising the following steps: the method comprises the following steps:
(1) pretreatment: firstly, treating the cellulose acetate fibers by using ionic liquid to swell the cellulose acetate fibers so as to facilitate the adsorption and diffusion of nitrilase and berberine; then nitrilase is utilized to treat the cellulose acetate fiber, so that part of cyano groups are hydrolyzed into carboxylic acid;
(2) dyeing: and then the pretreated vinegar green fiber is dyed by berberine.
2. The method for dyeing acetocyanine fibers by berberine according to claim 1, which is characterized in that: the pretreatment process of the step (1) comprises the following steps: (a) ionic liquid pretreatment: the cellulose acetate fiber is prepared by mixing cellulose acetate fiber in 80-95% of ionic liquid by mass percent in a bath ratio of 1: treating at 45, 50-70 deg.C for 20-50min, taking out sample, washing with anhydrous ethanol, and washing with water; (b) nitrilase treatment: nitrilase was used at 4% owf-10% owf, pH =7.0, bath ratio 1: treating at 40, 40-60 deg.C for 20-50min, washing with water, and oven drying.
3. The method for dyeing acetocyanine fibers by berberine according to claim 1, which is characterized in that: the dyeing process in the step (2) comprises the following steps: berberine is used at 1-7% owf, pH =3-9, bath ratio is 1: and (3) dyeing at room temperature, heating to 70-100 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
4. The method for dyeing acetocyanine fibers by berberine according to claim 1, which is characterized in that:
(1) the pretreatment process comprises (a) ionic liquid pretreatment: the cellulose acetate fiber is prepared by mixing cellulose acetate fiber in 80-95% of ionic liquid by mass percent in a bath ratio of 1: treating at 45, 50-70 deg.C for 20-50min, taking out sample, washing with anhydrous ethanol, and washing with water; (b) nitrilase treatment: nitrilase was used at 4% owf-10% owf, pH =7.0, bath ratio 1: treating at 40, 40-60 deg.C for 20-50min, washing with water, and oven drying;
(2) the dyeing process comprises the following steps: berberine is used at 1-7% owf, pH =3-9, bath ratio is 1: and (3) dyeing at room temperature, heating to 70-100 ℃ at the temperature of 1 ℃/min, keeping the temperature for 60 minutes, washing with water, and drying.
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CN105002592A (en) * | 2015-02-13 | 2015-10-28 | 吉林奇峰化纤股份有限公司 | Acetate fiber and preparation method thereof |
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CN105002592A (en) * | 2015-02-13 | 2015-10-28 | 吉林奇峰化纤股份有限公司 | Acetate fiber and preparation method thereof |
CN107541966A (en) * | 2017-10-17 | 2018-01-05 | 昆山凯洲环保科技有限公司 | A kind of textile dye and preparation method thereof and non-aqueous dyeing method |
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