CN116988325B - A method for improving the ozone fastness of indigo-dyed denim fabrics - Google Patents

Abstract

The invention discloses a method for improving ozone fastness of indigo-dyed jean fabric, which belongs to the technical field of textile printing and dyeing processing and comprises the following steps of adding the indigo-dyed jean fabric into a treatment bath containing reactive amino condensate and secondary amino organosilicon emulsion, controlling the bath ratio to be 1:30, heating to 60 ℃ for 45min, taking out the fabric, dehydrating and drying at 100-120 ℃. The reactive amino condensate prepared by the invention has the advantages of high amino content, large reducing effect and strong ozone resistance, simultaneously has reactivity, can react with fibers during fixation, has durability, and can provide softness of fabrics on one hand and reduce secondary amino groups in molecules on the other hand by adding the secondary amino organosilicon emulsion into the treatment bath, thereby improving ozone color fastness.

Description

Method for improving ozone fastness of indigo dyed jean fabric

Technical Field

The invention belongs to the technical field of textile printing and dyeing processing, and particularly relates to a method for improving ozone fastness of indigo-dyed jean fabric.

Background

Indigo is one of the most well-known and widely used dyes in the world. The use of indigo on textile dyes can be traced back to 2500 years before the male element. Especially, jean fabric and clothing are popular with consumers, and the yield is continuously improved. The industrial process is quickened, the quantity of the urban automobiles is greatly increased, the ozone is high in oxidizing property, indigo can attack carbon-carbon double bonds on indigo dye under the action of the ozone, indigo red, tannic acid and the like are generated, so that indigo fabrics fade and turn yellow, and a large number of indigo jeans fabric test results show that the ozone fastness is disqualified, and the quality of indigo jeans products is greatly influenced.

The research shows that the polyamine with stronger reducibility can react with ozone before the vat dye, and plays a role in protecting the vat dye. Wei Jiang from the oxidation resistance mechanism, compared with four amine compounds of dodecylaniline, diethanolamine, diethylenetriamine and triethylenetetramine, the amine compound is found to have a certain effect on the improvement of ozone fastness of vat dyes, and the higher the mass fraction of amino nitrogen atoms in the reducing organic matters is, the more remarkable effect on the improvement of ozone resistance is achieved, and along with the increase of the concentration of finishing liquid, the ozone resistance also shows a certain rising trend (research of ozone fastness of vat dyes and a lifter thereof [ D ]. Donghua university, 2008). However, polyamines themselves have volatility, irritation and sensitization and cannot be directly applied to vat dye dyed fabrics. Amine compounds are introduced into polyurethane by kingdom building and the like to develop a water-based polyurethane polymer for improving ozone fastness of pure cotton fabrics, and the optimized application process conditions are that 20g/L of polyurethane lifting agent dispersion liquid is padded, 80 ℃ is dried, 100 ℃ is baked for 3min, or the fabric is finished by adopting an impregnation method, the polyurethane lifting agent dispersion liquid is 10% (owf), the bath ratio is 1:20, and the ozone fastness is improved (synthesis and application of indigo ozone fastness lifting agent [ J ]. Printing and dyeing, 2009,35 (08): 1-4.). Polyurethane preparation is complex and affects other properties of the fabric. The invention patent with the application number 201611109173.2 discloses an ozone fastness improver for vat dyes, a preparation method and application thereof, and provides an epoxy end group hyperbranched polyamide-amine which is used as the ozone fastness improver for vat dyes, but the product uses amide as a reducing substance, so that the problem of insufficient reducing capability exists.

Based on the above analysis, development of agents and processing methods for improving ozone fastness of indigo-dyed denim fabrics is urgent.

Disclosure of Invention

The invention aims to overcome the defects and limitations in the prior art and provides a method for effectively improving the ozone fastness of indigo dyed jean fabric.

The technical solution of the invention is as follows:

A method for improving ozone fastness of indigo-dyed denim fabric comprising the steps of:

Adding the indigo dyed jean fabric into a treatment bath containing reactive amino condensate and secondary amino organosilicon emulsion, controlling the bath ratio to be 1:30, heating to 60 ℃ for treatment for 45min, taking out the fabric, dehydrating, and drying at 100-120 ℃.

The mass concentration of the reactive amino condensate is 1-10 g/L, and the mass concentration of the secondary amino organosilicon emulsion is 1-5 g/L.

The reactive amino condensate is prepared by condensing polyethylene polyamine serving as a raw material and epoxy chloropropane serving as a cross-linking agent, and the specific condensation method comprises the steps of dissolving triethylene tetramine and tetraethylene pentamine with a certain volume ratio in an ethanol solution in a four-neck flask under magnetic stirring, enabling the whole reaction system to be in a closed state, placing the reaction flask in an ice-water bath, controlling the temperature in the flask to be not higher than 10 ℃, slowly dropwise adding epoxy chloropropane by using a constant-pressure funnel after the triethylene tetramine and the tetraethylene pentamine are completely dissolved, continuously reacting for 30-90 minutes in a cold water bath after the dropwise adding of the ethanol solution of para-aminodiphenylamine, continuously reacting for 20-60 minutes after the dropwise adding of the ethanol solution, heating to 60 ℃, preserving heat for 2 hours, cooling to room temperature, adding acetic acid to adjust the pH value to 3-6, and performing reduced pressure distillation at 50 ℃ to obtain the reactive amino condensate.

The volume ratio of triethylene tetramine to tetraethylene pentamine is 1:1-1:3.

When the triethylene tetramine and the tetraethylene pentamine are dissolved in an ethanol solution, the ratio of the volume of the ethanol solution to the total volume of the triethylene tetramine and the tetraethylene pentamine is 1:1-2:1.

The volume of the epoxy chloropropane is 2 times of the total volume of triethylene tetramine and tetraethylene pentamine.

The mass fraction of the para-aminodiphenylamine in the ethanol solution of the para-aminodiphenylamine is 10% -50%.

The secondary amino organosilicon emulsion is a conventional industrial product, and the amine value is 0.4-0.8.

Compared with the prior art, the invention has the advantages that:

(1) The reactive amino condensate prepared by the invention has the advantages of high amino content, large reducing effect and strong ozone resistance, and simultaneously has reactivity, can react with fibers during fixation, and has durability.

(2) The treatment bath of the invention adds the secondary amino organosilicon emulsion, on one hand, provides the softness of the fabric, and on the other hand, the secondary amino carried in the molecule also has a reducing effect, thus improving the ozone color fastness.

Detailed description of the preferred embodiments

The invention is further described below with reference to examples.

Example 1

(1) Under magnetic stirring, 36mL of triethylene tetramine and tetraethylene pentamine with the volume ratio of 1:1 are dissolved in 50mL of ethanol solution in a four-neck flask, the whole reaction system is in a closed state, the reaction flask is placed in an ice-water bath, the temperature in the flask is controlled to be not higher than 10 ℃, 72mL of epoxy chloropropane is slowly dripped by a constant pressure funnel after the triethylene tetramine and the tetraethylene pentamine are completely dissolved, the reaction is continued in a cold water bath for 40 minutes after the dripping is finished, 20mL of 30% ethanol solution of para-aminodiphenylamine is continuously dripped, the reaction is carried out for 30 minutes after the dripping is finished, the temperature is raised to 60 ℃, the reaction is kept for 2 hours, the pH is regulated to 4 by adding acetic acid after cooling to room temperature, and the reactive amino condensate is obtained by reduced pressure distillation;

(2) Adding the indigo dyed jean fabric into a treatment bath containing 2g/L of reactive amino condensate and 2g/L of secondary amino organosilicon emulsion, controlling the bath ratio to be 1:30, adjusting the pH value to be 8, heating to 60 ℃ for 45min, taking out the fabric, dehydrating, and drying at 100-120 ℃.

Example 2

(1) Under magnetic stirring, 36mL of triethylene tetramine and tetraethylene pentamine with the volume ratio of 1:1.5 are dissolved in 50mL of ethanol solution in a four-neck flask, the whole reaction system is in a closed state, the reaction flask is placed in an ice-water bath, the temperature in the flask is controlled to be not higher than 10 ℃, 72mL of epoxy chloropropane is slowly dripped by a constant pressure funnel after the triethylene tetramine and the tetraethylene pentamine are completely dissolved, the reaction is continued in a cold water bath for 70 minutes after the dripping is finished, 40mL of 30% ethanol solution of para-aminodiphenylamine is continuously dripped, the reaction is carried out for 50 minutes after the dripping is finished, the temperature is raised to 60 ℃, the reaction is kept for 2 hours, acetic acid is added to adjust the pH to 4.5,50 ℃ after the reaction is cooled to the room temperature, and the reaction is distilled under reduced pressure to obtain the reactive amino condensate;

(2) Adding the indigo dyed jean fabric into a treatment bath containing 5g/L of reactive amino condensate and 3g/L of secondary amino organosilicon emulsion, controlling the bath ratio to be 1:30, adjusting the pH value to be 8, heating to 60 ℃ for 45min, taking out the fabric, dehydrating, and drying at 100-120 ℃.

Example 3

(1) Under magnetic stirring, 36mL of triethylene tetramine and tetraethylene pentamine with the volume ratio of 1:2 are dissolved in 50mL of ethanol solution in a four-neck flask, the whole reaction system is in a closed state, the reaction flask is placed in an ice-water bath, the temperature in the flask is controlled to be not higher than 10 ℃, 72mL of epoxy chloropropane is slowly dripped by a constant pressure funnel after the triethylene tetramine and the tetraethylene pentamine are completely dissolved, 30mL of 30% ethanol solution of para-aminodiphenylamine is continuously dripped in a cold water bath for reaction for 60 minutes after the dripping is finished, the temperature is raised to 60 ℃, the reaction is kept for 2 hours, acetic acid is added to adjust the pH to 3.5,50 ℃ after cooling to room temperature, and the reaction is carried out under reduced pressure and distilled to obtain the reactive amino condensate;

(2) Adding the indigo dyed jean fabric into a treatment bath containing 7g/L of reactive amino condensate and 4g/L of secondary amino organosilicon emulsion, controlling the bath ratio to be 1:30, adjusting the pH value to be 8, heating to 60 ℃ for 45min, taking out the fabric, dehydrating, and drying at 100-120 ℃.

The light fastness was tested according to GB/T8427-2019 "textile color fastness to artificial light fastness: xenon arc", the soaping fastness was tested according to GB/T3921-2008 "textile color fastness to soaping fastness", and the ozone fastness was tested according to AATCC 109-2016 "Colorfastness to Ozone in the Atmosphere under Low Humidities". The color fastness indexes of the untreated jean fabric and the jean fabrics of examples 1 to 3 are measured and shown in Table 1.

Table 1 results of color fastness testing of the untreated denim fabric, example 1 to 3 denim fabrics

As shown in Table 1, the method of the invention can effectively improve the ozone fastness of the indigo-dyed jean fabric without affecting other color fastness of the fabric, and compared with untreated jean fabric, the ozone fastness of the jean fabric treated by the method of the invention is greatly improved.

The above examples merely illustrate specific embodiments of the disclosure, but the embodiments of the disclosure are not limited by the foregoing. Any changes, modifications, substitutions, combinations, and simplifications that may be made without materially departing from the spirit and principles of the inventive concepts of the present disclosure are intended to be equivalent substitutes and are intended to be included within the scope of protection as defined by the claims.

Claims (6)

1. A method for improving the ozone fastness of indigo-dyed denim fabric, characterized by comprising the following steps: Indigo-dyed denim fabric was added to a treatment bath containing a reactive amino condensate and a secondary amino silicone emulsion, with a bath ratio of 1:30. The mixture was heated to 60°C and treated for 45 minutes. The fabric was then removed, dehydrated, and dried at 100°C–120°C. The reactive amino condensate had a mass concentration of 1–10 g/L, and the secondary amino silicone emulsion had a mass concentration of 1–5 g/L. The reactive amino condensate was formed by condensation of polyethylenepolyamine as a raw material and epichlorohydrin as a crosslinking agent. The specific condensation method was as follows: Under magnetic stirring, a certain volume ratio of triethylenetetramine and tetraethylenepentamine was dissolved in an ethanol solution in a four-necked flask, keeping the entire reaction system in a sealed state. The reaction flask was placed in an ice-water bath, and the temperature inside the flask was controlled not to exceed 10°C. After triethylenetetramine and tetraethylenepentamine were completely dissolved at ℃, epichlorohydrin was slowly added dropwise using a constant pressure funnel. After the addition was complete, the reaction was continued in a cold water bath for 30-90 minutes. Then, an ethanol solution of p-aminodiphenylamine was added dropwise. After the addition was complete, the reaction was continued for 20-60 minutes. The temperature was raised to 60℃ and the reaction was maintained at this temperature for 2 hours. After cooling to room temperature, acetic acid was added to adjust the pH to 3-6. The reactive amino condensate was obtained by vacuum distillation at 50℃. 2. The method for improving the ozone fastness of indigo-dyed denim fabric as described in claim 1, characterized in that: the volume ratio of triethylenetetramine and tetraethylenepentamine is 1:1 to 1:3. 3. The method for improving the ozone fastness of indigo-dyed denim fabric as described in claim 1, characterized in that: when the triethylenetetramine and tetraethylenepentamine are dissolved in an ethanol solution, the ratio of the volume of the ethanol solution to the total volume of the triethylenetetramine and tetraethylenepentamine is 1:1 to 2:1. 4. The method for improving the ozone fastness of indigo-dyed denim fabric as described in claim 1, characterized in that: the volume of epichlorohydrin is twice the total volume of triethylenetetramine and tetraethylenepentamine. 5. The method for improving the ozone fastness of indigo-dyed denim fabric as described in claim 1, characterized in that: the mass fraction of p-aminodiphenylamine in the ethanol solution of p-aminodiphenylamine is 10%~50%. 6. The method for improving the ozone fastness of indigo-dyed denim fabric as described in claim 1, characterized in that: the amine value of the secondary amino silicone emulsion is 0.4~0.8.