CN113550019B - Preparation method of colored regenerated cellulose conductive filaments based on waste textiles - Google Patents
Preparation method of colored regenerated cellulose conductive filaments based on waste textiles Download PDFInfo
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- CN113550019B CN113550019B CN202110908027.0A CN202110908027A CN113550019B CN 113550019 B CN113550019 B CN 113550019B CN 202110908027 A CN202110908027 A CN 202110908027A CN 113550019 B CN113550019 B CN 113550019B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B15/00—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/04—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of yarns, threads or filaments
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Abstract
The application discloses a preparation method of colored regenerated cellulose conductive filaments based on waste textiles, which comprises the following steps: classifying and recycling the waste textiles, and then opening the waste textiles into waste fibers; treating waste fibers by dilute inorganic acid, and dissolving the waste fibers in ionic liquid to obtain regenerated cellulose solution; dispersing indium tin oxide in dimethyl sulfoxide to obtain indium tin oxide dispersion liquid; mixing the regenerated cellulose solution with the indium tin oxide dispersion liquid, performing ultrasonic treatment, and stirring to obtain regenerated cellulose spinning liquid; and wet spinning, and leaching the residual ionic liquid to obtain regenerated cellulose conductive filaments with corresponding colors. The method is simple to operate, the parameters are easy to control, and the colored regenerated cellulose conductive filament prepared by recycling, preprocessing, dissolving, preparing the conductive spinning solution and wet spinning the colored waste textiles has good microscopic morphology, excellent mechanical property, color fastness and conductivity.
Description
Technical Field
The application belongs to the field of reutilization of waste textiles, and particularly relates to a preparation method of colored regenerated cellulose conductive filaments based on waste textiles.
Background
The total fiber processing amount of China is about 5000 ten thousand tons, and waste textiles with more than 2000 ten thousand tons are produced in one year. Wherein, 300 ten thousand tons of waste cotton textiles account for 50 percent of the waste natural fiber textiles. In recent years, with the improvement of living standard, the consumption demand of people for pure cotton textiles is continuously increased, and the number of waste cotton textiles is continuously increased. However, 75 to 80% of the waste cotton is mainly treated by incineration and landfill, which generates malodorous gas, polluted air, surface water and groundwater. In addition, the textile contains heavy metal ions, dyes and penetrants, and if the textile is improperly treated, the textile can cause environmental and public health problems, so that the textile is not only wasteful of precious resources, but also causes serious environmental pollution. Therefore, the recycling of waste textiles is particularly important. The existing method for recycling waste textiles mainly comprises mechanical recycling, chemical recycling and heat energy recycling. And the performance and economic value of the product obtained by mechanical recovery are low, and the potential recoverable value of cotton is lost by heat energy recovery. Therefore, the recycling of waste textiles becomes a current urgent problem to be solved.
Currently, functional fibers composed of a polymer and an electrical conductor are of great interest. Cellulose is the most abundant natural polymer in nature, has biocompatibility, biodegradability and better thermal stability and chemical stability, and can be skillfully combined with metal powder, conductive polymer and the like to prepare the conductive fiber. The imidazole ionic liquid is a good solvent of cellulose, and is a green solvent which is mainly used for effectively breaking intermolecular hydrogen bonds of cellulose by anions in the solvent to dissolve the cellulose without degradation, is difficult to volatilize and easy to recycle, and is used for dissolving the cellulose. However, the cellulose solution dissolved by the ionic liquid has high viscosity, is not easy to spin, and influences the application of waste textiles in preparing fibers. Meanwhile, the document 'influence of dyeing and water washing on the structure and performance of the conductive fiber' discloses that the surface structure of the conductive fiber is damaged by dyeing, so that the conductivity of the fiber is reduced, and the application of waste textiles in preparing the conductive fiber is influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the application aims to provide a preparation method of colored regenerated cellulose conductive filaments based on waste textiles.
The technical scheme for solving the technical problems is that the application provides a preparation method of colored regenerated cellulose conductive filaments based on waste textiles, which is characterized by comprising the following steps:
1) Classifying and recycling the waste textiles, and then opening the waste textiles into waste fibers;
2) Treating the waste fibers obtained in the step 1) with dilute inorganic acid to reduce the polymerization degree of the waste fibers, washing the waste fibers with deionized water to be neutral, and drying the waste fibers;
3) Dissolving the fiber obtained in the step 2) by using an ionic liquid to obtain a regenerated cellulose solution;
4) Dispersing indium tin oxide in dimethyl sulfoxide to obtain indium tin oxide dispersion liquid;
5) Mixing the regenerated cellulose solution obtained in the step 3) with the indium tin oxide dispersion liquid obtained in the step 4), performing ultrasonic treatment, and stirring to obtain regenerated cellulose spinning solution;
6) Carrying out wet spinning on the regenerated cellulose spinning solution obtained in the step 5) to obtain a primary regenerated cellulose conductive filament;
7) Immersing the nascent regenerated cellulose conductive filaments obtained in the step 6) in deionized water to remove residual ionic liquid, thereby obtaining regenerated cellulose conductive filaments with corresponding colors.
Compared with the prior art, the application has the beneficial effects that:
(1) The method is simple to operate, the parameters are easy to control, and the colored regenerated cellulose conductive filament prepared by recycling, preprocessing, dissolving, preparing the conductive spinning solution and wet spinning the colored waste textiles has good microscopic morphology, excellent mechanical property, color fastness and conductivity.
(2) The method maintains the primary colors of waste textiles, the weak acid environment pretreatment is used for reducing the polymerization degree of cellulose, the cellulose molecule is mainly acted in the process of dissolving cellulose by the ionic liquid, and the dye is not damaged or destroyed in both process steps, so that the dye is stably present on the fiber, the bleaching of the waste textiles and the secondary dyeing of regenerated cellulose conductive filaments are avoided, the pollution is reduced, the cost and the production time are saved, the green recovery cycle is realized, and meanwhile, the damage of the surface structure of the conductive fiber caused by the dyeing process is avoided, and the conductive performance of the conductive fiber is further influenced.
(3) The method has no requirement on the strength of the waste textiles, and the waste textiles with extremely low strength after long-term use can still be used. The method is characterized in that the waste textiles are subjected to acid treatment and crushing pretreatment, the textiles with long service time and low strength are easy to pretreat instead, the defect that the application of regenerated yarns is limited due to short fiber strength is avoided in mechanical recovery, and 100% recycling of the waste cotton textiles can be realized.
(4) According to the method, transparent conductive indium tin oxide and regenerated cellulose are mixed for wet spinning, and a conductive material is embedded into fibers, so that the conductive performance is stable and cannot fall off, the prepared regenerated cellulose conductive filament has the functions of static resistance, radiation resistance and the like, the primary color of waste textiles cannot be influenced by the indium tin oxide, and the recovery and high-quality utilization of the waste textiles are realized.
(5) The present method explores the possibility of mixing together different colored fiber powders to create a new color. The mixture of yellow and blue fiber powders produced green fibers with a uniform color distribution. Similarly, the ability to generate new colors using colored cotton waste mixtures, which produce purple fibers from a mixture of blue and red fiber powders, can increase process flexibility, further reducing the need for traditional coloring processes.
(6) The color regenerated cellulose conductive filament prepared by the method has the breaking strength of 100-400 Mpa, the breaking elongation of 5-17% and the color fastness of 4-5 grade; the conductivity is 0.1-200S/m, the textile woven by the conductive filament has excellent mechanical property, antistatic property, radiation protection and other properties, the X-ray protection efficiency of 120kV (100 keV) of the tube voltage is 20-80%, and the conductive filament can be used in the fields of intelligent wearable and radiation protection clothing preparation and the like.
Drawings
FIG. 1 is an SEM image of the surface of regenerated cellulose conductive filaments prepared in example 1 of the present application;
FIG. 2 is a close-up SEM of FIG. 1 of the present application;
FIG. 3 is an SEM image of a cross-section of a regenerated cellulose conductive filament prepared according to example 1 of the present application;
FIG. 4 is a close-up SEM image of FIG. 3 of the present application;
FIG. 5 is an XRD pattern of the raw materials and regenerated cellulose conductive filaments prepared in example 3 and comparative example 3 of the present application;
fig. 6 is a schematic view of a wet spinning apparatus according to the present application.
Detailed Description
Specific examples of the present application are given below. The specific examples are provided only for further details of the present application and do not limit the scope of the claims.
The application provides a preparation method (short method) of colored regenerated cellulose conductive filaments based on waste textiles, which is characterized by comprising the following steps:
1) Waste textiles are classified and recycled according to colors, original colors of the waste textiles are reserved, and the waste textiles are opened into waste fibers through a cloth opener;
preferably, in the step 1), the waste textiles are textiles with different colors and different worn degrees, which are made of fibers taking cellulose as a main constituent substance, and comprise pure cotton textiles, pure hemp textiles, viscose textiles and the like.
2) Treating the waste fibers obtained in the step 1) with dilute inorganic acid to reduce the polymerization degree of the waste fibers, facilitate dissolution, washing with deionized water to neutrality, and drying;
preferably, in step 2), the mineral acid is sulfuric acid, nitric acid or hydrochloric acid;
preferably, in step 2), the treatment conditions are: the treatment is carried out in a water bath environment at 50-90 deg.C (preferably 75 deg.C) in a mineral acid at a concentration of 0.1-1 wt% (preferably 0.5 wt%) for 0.5-3 h.
3) Dissolving the fiber obtained in the step 2) by using an ionic liquid to obtain a regenerated cellulose solution;
preferably, in step 3), the dissolution conditions are: dissolving in an oil bath environment of 70-100 ℃ (preferably 90 ℃) for 1-6 hours to obtain regenerated cellulose solution with the concentration of 3-20 wt% (preferably 3-12 wt%).
Preferably, in step 3), the ionic liquid is 1-butyl-3-methylimidazole chloride.
4) Dispersing indium tin oxide in dimethyl sulfoxide to obtain indium tin oxide dispersion liquid;
preferably, in step 4), the concentration of the indium tin oxide dispersion is 0.5 to 3wt% (preferably 0.5 to 2 wt%); during dispersion, the mode of alternating ultrasonic and stirring intervals is adopted, stirring is carried out for 10-40 min after each ultrasonic for 10-40 min (preferably stirring is carried out for 0.5h after each ultrasonic for 0.5 h), the total ultrasonic time is 1-3 h (preferably 2 h), and an ultrasonic cleaner is adopted for ultrasonic.
5) Mixing the regenerated cellulose solution obtained in the step 3) and the indium tin oxide dispersion liquid obtained in the step 4), then ultrasonically oscillating for 0.2-2 hours (preferably 1-2 hours) under ultrasonic waves with the power of 30-8000W (preferably 180W) and the frequency of 20-120 kHz (preferably 40 kHz), and stirring for 1-2 hours at normal temperature at the speed of 0-1000 r/min (preferably 300 r/min) by using a magnetic stirrer to obtain regenerated cellulose spinning solution;
preferably, in step 5), the mass ratio of the indium tin oxide dispersion to the regenerated cellulose solution is 1-5:1 (preferably 1-3:1).
6) Carrying out wet spinning on the regenerated cellulose spinning solution obtained in the step 5) to obtain a primary regenerated cellulose conductive filament;
preferably, in the step 6), the coagulating bath for wet spinning is deionized water at 25-70 ℃, and the spinning conditions are as follows: the specification of the injector is 20-100 ml, the pump flow rate, namely the propelling speed of the spinning solution, is 40-100 ml/h, the diameter of the spinning needle is 0.45-1.2 mm, the speed of the roller I is 20-50 mm/s, and the speed ratio of the roller II to the roller I is 1-3:1; the speed of the winding roller is the same as that of the second roller.
7) Soaking the nascent regenerated cellulose conductive filaments obtained in the step 6) in deionized water for at least 2 hours for completely leaching residual ionic liquid, and then drying to obtain regenerated cellulose conductive filaments with corresponding colors.
Preferably, the steps are added between the step 2) and the step 3): and (3) immediately feeding the fiber obtained in the step (2) into a Raymond mill to grind the fiber into powder after freezing the fiber by liquid nitrogen.
In the examples below, the resistance of the filaments was measured with a multimeter and the conductivity was calculated. The strength and elongation at break test method is a single fiber strength machine tensile test, and the YG001D electronic single fiber strength machine has a gauge of 20mm and a tensile speed of 10mm/min.
Example 1
1) Recovering red waste pure cotton textiles, and opening the waste cotton cloth by adopting a multifunctional fine shuttle opener to obtain waste cotton fibers;
2) Adding 2g of waste cotton fibers into 200ml of 0.5wt% dilute sulfuric acid, heating to 75 ℃ in a water bath kettle, keeping for 2 hours, washing to be neutral by deionized water, and drying in an oven at 50 ℃ for later use;
3) Freezing the fiber obtained in the step 2) by liquid nitrogen, immediately putting the fiber into a Raymond mill, and grinding the fiber into powder;
4) Weighing 3g of 1-butyl-3-methylimidazole chloride, putting into a sealed bottle, and putting into an oil bath pot at 90 ℃ until the solution is transparent; weighing 0.2g of the powder obtained in the step 3), placing the powder into a sealed bottle, and completely dissolving the fiber in an oil bath at 90 ℃ to obtain regenerated cellulose solution;
5) 0.1g of indium tin oxide was dispersed in 6g of dimethyl sulfoxide to obtain an indium tin oxide dispersion; during dispersion, stirring for 0.5h after each ultrasonic treatment for 0.5h;
6) Mixing the regenerated cellulose solution obtained in the step 4) with the indium tin oxide dispersion liquid obtained in the step 5), performing ultrasonic treatment for 1h under ultrasonic waves with the power of 180W and the frequency of 40kHz, and stirring for 1h at the normal temperature at the speed of 300r/min by using a magnetic stirrer to obtain regenerated cellulose spinning solution;
7) The regenerated cellulose spinning solution obtained in the step 6) is defoamed, placed in a 20ml medical injector, then connected with a spinning needle, subjected to wet spinning in a wet spinning device, the advancing speed of the spinning solution is 70ml/h, the speed of a roller I is 20mm/s, the speed ratio of a roller II to a roller I is 1.5:1, and the receiving mode is roller receiving, so that the primary regenerated cellulose conductive filaments are obtained;
8) And (3) soaking the nascent regenerated cellulose conductive filaments obtained in the step (7) in deionized water for 2 hours, and drying at 50 ℃ to obtain red regenerated cellulose conductive filaments.
As can be seen from fig. 1 and 2, the red regenerated cellulose conductive filament prepared in example 1 is uniform, and the surface is grooved in the longitudinal direction, which is a typical structural feature of the fiber prepared by wet spinning, which indicates that the regenerated cellulose conductive filament prepared in the application is better in molding.
As can be seen from fig. 3 and fig. 4, the regenerated cellulose conductive filament has a circular cross section, a compact structure and no obvious defect and cavity inside, which indicates that the preparation process of the application is better, and the prepared regenerated cellulose conductive filament has a better structure.
Comparative example 1
Comparative example 1 differs from example 1 in that: the conductive material indium tin oxide is not added into the regenerated cellulose spinning solution, and specifically comprises the following steps:
1) Recovering red waste pure cotton textiles, and opening the waste cotton cloth by adopting a multifunctional fine shuttle opener to obtain waste cotton fibers;
2) Weighing 2g of waste cotton fibers, adding the waste cotton fibers into 200ml of dilute sulfuric acid with the concentration of 0.5wt%, heating to 75 ℃ in a water bath kettle, keeping for 2 hours, washing with deionized water to be neutral, and drying in an oven at 50 ℃ for later use;
3) Freezing the fiber obtained in the step 2) by liquid nitrogen, immediately putting the fiber into a Raymond mill, and grinding the fiber into powder;
4) Weighing 3g of 1-butyl-3-methylimidazole chloride, putting into a sealed bottle, and putting into an oil bath pot at 90 ℃ until the solution is transparent; weighing 0.2g of the powder obtained in the step 3), placing the powder into a sealed bottle, and completely dissolving the fiber in an oil bath at 90 ℃ to obtain regenerated cellulose solution;
5) Placing the regenerated cellulose solution obtained in the step 4) into a 20ml medical injector, connecting a spinning needle, and carrying out wet spinning in a wet spinning device, wherein the advancing speed of the spinning solution is 70ml/h, the speed of a roller I is 20mm/s, the speed ratio of a roller II to a roller I is 1.5:1, and the receiving mode is roller receiving, so as to obtain a primary regenerated cellulose filament;
6) Soaking the regenerated cellulose filaments obtained in the step 5) in deionized water for 2 hours, and drying at 50 ℃ to obtain red regenerated cellulose filaments.
TABLE 1
Examples | strength/MPa | Elongation at break/% | Conductivity S/m |
Example 1 | 323.58 | 11.95 | 0.13 |
Comparative example 1 | 330.86 | 11.58 | —— |
As can be seen from table 1, the addition of indium tin oxide does not reduce the mechanical properties of the cellulose filaments, as compared with comparative example 1, so that it imparts good electrical conductivity while maintaining good mechanical properties.
Example 2
1) Recovering blue waste pure cotton textiles, and loosening the waste cotton cloth by adopting a multifunctional fine shuttle opener to obtain waste cotton fibers;
2) Weighing 2g of waste cotton fibers, adding the waste cotton fibers into 200ml of dilute sulfuric acid with the concentration of 0.5wt%, heating to 75 ℃ in a water bath kettle, keeping for 2 hours, washing with deionized water to be neutral, and drying in an oven at 50 ℃ for later use;
3) Freezing the fiber obtained in the step 2) by liquid nitrogen, immediately putting the fiber into a Raymond mill, and grinding the fiber into powder;
4) Weighing 3g of 1-butyl-3-methylimidazole chloride, putting into a sealed bottle, and putting into an oil bath pot at 90 ℃ until the solution is transparent; weighing 0.2g of the powder obtained in the step 3), placing the powder into a sealed bottle, and completely dissolving the fiber in an oil bath at 90 ℃ to obtain regenerated cellulose solution;
5) 0.2g of indium tin oxide was dispersed in 6g of dimethyl sulfoxide to obtain an indium tin oxide dispersion; during dispersion, stirring for 0.5h after each ultrasonic treatment for 0.5h;
6) Mixing the regenerated cellulose solution obtained in the step 4) with the indium tin oxide dispersion liquid obtained in the step 5), performing ultrasonic treatment for 1h under ultrasonic waves with the power of 180W and the frequency of 40kHz, and stirring for 1h at the normal temperature at the speed of 300r/min by using a magnetic stirrer to obtain regenerated cellulose spinning solution;
7) The regenerated cellulose spinning solution obtained in the step 6) is defoamed, placed in a 20ml medical injector, then connected with a spinning needle, subjected to wet spinning in a wet spinning device, the advancing speed of the spinning solution is 70ml/h, the speed of a roller I is 20mm/s, the speed ratio of a roller II to a roller I is 1.5:1, and the receiving mode is roller receiving, so that the primary regenerated cellulose conductive filaments are obtained;
8) And (3) soaking the nascent regenerated cellulose conductive filaments obtained in the step (7) in deionized water for 2 hours, and drying at 50 ℃ to obtain the blue regenerated cellulose conductive filaments.
Comparative example 2
Comparative example 2 differs from example 2 in that: the raw materials adopt pure white waste pure cotton textiles, and the final cellulose filaments need to be dyed, specifically:
1) Recovering pure white waste pure cotton textiles, and opening the waste cotton cloth by adopting a multifunctional fine shuttle opener to obtain waste cotton fibers;
2) Weighing 2g of waste cotton fibers, adding the waste cotton fibers into 200ml of dilute sulfuric acid with the concentration of 0.5wt%, heating to 75 ℃ in a water bath kettle, keeping for 2 hours, washing with deionized water to be neutral, and drying in an oven at 50 ℃ for later use;
3) Freezing the fiber obtained in the step 2) by liquid nitrogen, immediately putting the fiber into a Raymond mill, and grinding the fiber into powder;
4) Weighing 3g of 1-butyl-3-methylimidazole chloride, putting into a sealed bottle, and putting into an oil bath pot at 90 ℃ until the solution is transparent; weighing 0.2g of the powder obtained in the step 3), placing the powder into a sealed bottle, and completely dissolving the fiber in an oil bath at 90 ℃ to obtain regenerated cellulose solution;
5) 0.2g of indium tin oxide was dispersed in 6g of dimethyl sulfoxide to obtain an indium tin oxide dispersion; during dispersion, stirring for 0.5h after each ultrasonic treatment for 0.5h;
6) Mixing the regenerated cellulose solution obtained in the step 4) with the indium tin oxide dispersion liquid obtained in the step 5), performing ultrasonic treatment for 1h under ultrasonic waves with the power of 180W and the frequency of 40kHz, and stirring for 1h at the normal temperature at the speed of 300r/min by using a magnetic stirrer to obtain regenerated cellulose spinning solution;
7) The regenerated cellulose spinning solution obtained in the step 6) is defoamed, placed in a 20ml medical injector, then connected with a spinning needle, subjected to wet spinning in a wet spinning device, the advancing speed of the spinning solution is 70ml/h, the speed of a roller I is 20mm/s, the speed ratio of a roller II to a roller I is 1.5:1, and the receiving mode is roller receiving, so that the primary regenerated cellulose conductive filaments are obtained;
8) Soaking the nascent regenerated cellulose conductive filaments obtained in the step 7) in deionized water for 2 hours, and drying at 50 ℃ to obtain the pure white regenerated cellulose conductive filaments.
9) And (3) conventionally dyeing the pure white regenerated cellulose conductive filaments obtained in the step (8) by using indigo to obtain blue regenerated cellulose conductive filaments.
TABLE 2
Table 2 shows the fabric fastnesses measured according to the standards GB T5718-1997 and GB T3920-2008. As can be seen from Table 2, the colored regenerated cellulose conductive filaments prepared by the method have excellent color fastness, successfully solve the problems that the dyes float on the surface of the fabric and are easy to stain and fade after the fabric is dyed, and avoid the problems of uneven dyeing and the like caused by surface grooves of wet spinning.
TABLE 3 Table 3
Examples | strength/MPa | Elongation at break/% | Conductivity S/m |
Example 2 | 320.49 | 10.26 | 8.84 |
Comparative example 2 | 296.85 | 8.32 | 5.62 |
As can be seen from Table 3, the pure white regenerated cellulose conductive filaments of example 2 were significantly reduced in mechanical properties and conductivity after dyeing, and the strength was reduced by 7% and the conductivity was reduced by 36% as compared with comparative example 2. Because the dye needs to be subjected to padding dyeing for a plurality of times during coloring, the surface structure of the regenerated cellulose conductive filament is damaged, so that the mechanical property and the conductivity of the regenerated cellulose conductive filament are reduced, in addition, the surface of the regenerated cellulose filament is grooved, and the uneven adsorption of dye molecules can increase the resistance of the regenerated cellulose conductive filament, so that the conductivity of the regenerated cellulose conductive filament is reduced.
Example 3
1) Recovering red waste pure cotton textiles, and opening the waste cotton cloth by adopting a multifunctional fine shuttle opener to obtain waste cotton fibers;
2) Weighing 2g of waste cotton fibers, adding the waste cotton fibers into 200ml of dilute sulfuric acid with the concentration of 0.5wt%, heating to 75 ℃ in a water bath kettle, keeping for 2 hours, washing with deionized water to be neutral, and drying in an oven at 50 ℃ for later use;
3) Freezing the fiber obtained in the step 2) by liquid nitrogen, immediately putting the fiber into a Raymond mill, and grinding the fiber into powder;
4) Weighing 3g of 1-butyl-3-methylimidazole chloride, putting into a sealed bottle, and putting into an oil bath pot at 90 ℃ until the solution is transparent; weighing 0.2g of the powder obtained in the step 3), placing the powder into a sealed bottle, and completely dissolving the fiber in an oil bath at 90 ℃ to obtain regenerated cellulose solution;
5) 0.2g of indium tin oxide was dispersed in 4g of dimethyl sulfoxide to obtain an indium tin oxide dispersion; during dispersion, stirring for 0.5h after each ultrasonic treatment for 0.5h;
6) Mixing the regenerated cellulose solution obtained in the step 4) with the indium tin oxide dispersion liquid obtained in the step 5), performing ultrasonic treatment for 1h under ultrasonic waves with the power of 180W and the frequency of 40kHz, and stirring for 1h at the normal temperature at the speed of 300r/min by using a magnetic stirrer to obtain regenerated cellulose spinning solution;
7) The regenerated cellulose spinning solution obtained in the step 6) is defoamed, placed in a 20ml medical injector, then connected with a spinning needle, subjected to wet spinning in a wet spinning device, the advancing speed of the spinning solution is 70ml/h, the speed of a roller I is 20mm/s, the speed ratio of a roller II to a roller I is 1.5:1, and the receiving mode is roller receiving, so that the primary regenerated cellulose conductive filaments are obtained;
8) And (3) soaking the nascent regenerated cellulose conductive filaments obtained in the step (7) in deionized water for 2 hours, and drying at 50 ℃ to obtain red regenerated cellulose conductive filaments.
Comparative example 3
Comparative example 3 differs from example 3 in that: the raw materials adopt brand new undyed white pure cotton fibers, and concretely comprise:
1) Weighing 2g of brand new undyed white pure cotton fibers, adding the brand new white pure cotton fibers into 200ml of dilute sulfuric acid with the concentration of 0.5wt%, heating to 75 ℃ in a water bath kettle, keeping the temperature for 2 hours, washing the white pure cotton fibers to be neutral by deionized water, and drying the white pure cotton fibers in an oven at 50 ℃ for later use;
2) Freezing the fiber obtained in the step 1) by liquid nitrogen, immediately putting the fiber into a Raymond mill, and grinding the fiber into powder;
3) Weighing 3g of 1-butyl-3-methylimidazole chloride, putting into a sealed bottle, and putting into an oil bath pot at 90 ℃ until the solution is transparent; weighing 0.2g of the powder obtained in the step 2), placing the powder into a sealed bottle, and completely dissolving the fiber in an oil bath at 90 ℃ to obtain regenerated cellulose solution;
4) 0.2g of indium tin oxide was dispersed in 6g of dimethyl sulfoxide to obtain an indium tin oxide dispersion; during dispersion, stirring for 0.5h after each ultrasonic treatment for 0.5h;
5) Mixing the regenerated cellulose solution obtained in the step 3) with the indium tin oxide dispersion liquid obtained in the step 4), performing ultrasonic treatment for 1h under ultrasonic waves with the power of 180W and the frequency of 40kHz, and stirring for 1h at the normal temperature at the speed of 300r/min by using a magnetic stirrer to obtain regenerated cellulose spinning solution;
6) The regenerated cellulose spinning solution obtained in the step 5) is defoamed, placed in a 20ml medical injector, then connected with a spinning needle, subjected to wet spinning in a wet spinning device, the advancing speed of the spinning solution is 70ml/h, the speed of a roller I is 20mm/s, the speed ratio of a roller II to a roller I is 1.5:1, and the receiving mode is roller receiving, so that the nascent regenerated cellulose conductive filaments are obtained;
7) Soaking the nascent regenerated cellulose conductive filaments obtained in the step 6) in deionized water for 2 hours, and drying at 50 ℃ to obtain the pure white regenerated cellulose conductive filaments.
As can be seen from fig. 5, the regenerated cellulose filaments prepared from the waste fabric containing the dye have the same crystalline structure as the regenerated cellulose filaments prepared from the completely new pure cotton, and are all the transition from cellulose I to cellulose II. The presence of the dye does not affect the properties of the regenerated cellulose fibers.
TABLE 4 Table 4
Examples | strength/MPa | Elongation at break/% | Conductivity S/m |
Example 3 | 319.55 | 10.89 | 8.52 |
Comparative example 3 | 328.93 | 10.11 | 8.52 |
As can be seen from table 4, the mechanical properties of the colored regenerated cellulose conductive filaments recovered based on the waste textiles are comparable to those of regenerated cellulose filaments based on entirely new pure cotton fibers in example 3 compared with comparative example 3.
Claims (10)
1. The preparation method of the colored regenerated cellulose conductive filament based on the waste textile is characterized by comprising the following steps of:
1) Classifying and recycling the waste textiles according to the colors, retaining the original colors of the waste textiles, and then opening the waste textiles into waste fibers;
2) Treating the waste fibers obtained in the step 1) with dilute inorganic acid to reduce the polymerization degree of the waste fibers, washing the waste fibers with deionized water to be neutral, and drying the waste fibers;
3) Dissolving the fiber obtained in the step 2) by using an ionic liquid to obtain a regenerated cellulose solution;
4) Dispersing indium tin oxide in dimethyl sulfoxide to obtain indium tin oxide dispersion liquid;
5) Mixing the regenerated cellulose solution obtained in the step 3) with the indium tin oxide dispersion liquid obtained in the step 4), performing ultrasonic treatment, and stirring to obtain regenerated cellulose spinning solution;
6) Carrying out wet spinning on the regenerated cellulose spinning solution obtained in the step 5) to obtain a primary regenerated cellulose conductive filament;
7) Immersing the nascent regenerated cellulose conductive filaments obtained in the step 6) in deionized water to remove residual ionic liquid, thereby obtaining regenerated cellulose conductive filaments with corresponding colors.
2. The method for producing colored regenerated cellulose conductive filaments based on waste textiles according to claim 1, wherein in step 1), the waste textiles are textiles with different colors and different degrees of wear and tear made of fibers mainly composed of cellulose.
3. The method for producing colored regenerated cellulose conductive filaments based on waste textiles according to claim 1, wherein in step 2), the inorganic acid is sulfuric acid, nitric acid or hydrochloric acid.
4. The method for preparing colored regenerated cellulose conductive filaments based on waste textiles according to claim 1, wherein in step 2), the treatment conditions are: treating in a water bath environment at 50-90 ℃ for 0.5-3 h in an inorganic acid with the concentration of 0.1-1 wt%.
5. The method for preparing colored regenerated cellulose conductive filaments based on waste textiles according to claim 1, wherein in step 3), the dissolution conditions are: and dissolving in an oil bath environment at 70-100 ℃ for 1-6 hours to obtain a regenerated cellulose solution with the concentration of 3-20wt%.
6. The method for preparing colored regenerated cellulose conductive filaments based on waste textiles according to claim 1, wherein in the step 4), the concentration of the indium tin oxide dispersion liquid is 0.5-3wt%; during dispersion, the mode of alternating ultrasonic and stirring intervals is adopted, stirring is carried out for 10-40 min after each ultrasonic for 10-40 min, and the total ultrasonic time is 1-3 h.
7. The method for producing colored regenerated cellulose conductive filaments based on waste textiles according to claim 1, wherein in step 5), the ultrasound is: ultrasonic oscillation is carried out for 0.2-2 hours under the condition that the ultrasonic power is 30-8000W and the frequency is 20-120 kHz; stirring is as follows: stirring for 1-2 hours at normal temperature at the speed of 300-1000 r/min in a magnetic stirrer.
8. The method for preparing colored regenerated cellulose conductive filaments based on waste textiles according to claim 1, wherein in the step 5), the mass ratio of the indium tin oxide dispersion liquid to the regenerated cellulose solution is 1-5:1.
9. The method for preparing the colored regenerated cellulose conductive filaments based on the waste textiles according to claim 1, wherein in the step 6), the coagulation bath of wet spinning is deionized water at 25-70 ℃, and the spinning conditions are as follows: the advancing speed of the spinning solution is 40-100 ml/h, the diameter of a spinning needle is 0.45-1.2 mm, the speed of a roller I is 20-50 mm/s, and the speed ratio of a roller II to a roller I is 1-3:1; the speed of the winding roller is the same as that of the second roller.
10. The preparation method of the colored regenerated cellulose conductive filament based on the waste textile is characterized by comprising the following steps of:
1) Classifying and recycling the waste textiles according to the colors, retaining the original colors of the waste textiles, and then opening the waste textiles into waste fibers;
2) Treating the waste fibers obtained in the step 1) with dilute inorganic acid to reduce the polymerization degree of the waste fibers, washing the waste fibers with deionized water to be neutral, and drying the waste fibers;
3) Freezing the fiber obtained in the step 2) by liquid nitrogen, and immediately putting the fiber into a pulverizer to be pulverized;
4) Dissolving the powder obtained in the step 3) by using an ionic liquid to obtain a regenerated cellulose solution;
5) Dispersing indium tin oxide in dimethyl sulfoxide to obtain indium tin oxide dispersion liquid;
6) Mixing the regenerated cellulose solution obtained in the step 4) with the indium tin oxide dispersion liquid obtained in the step 5), performing ultrasonic treatment, and stirring to obtain regenerated cellulose spinning solution;
7) Carrying out wet spinning on the regenerated cellulose spinning solution obtained in the step 6) to obtain a primary regenerated cellulose conductive filament;
8) Immersing the nascent regenerated cellulose conductive filaments obtained in the step 7) in deionized water to remove residual ionic liquid, thereby obtaining regenerated cellulose conductive filaments with corresponding colors.
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CN105420928A (en) * | 2015-11-04 | 2016-03-23 | 北京国科华仪科技有限公司 | Flexible nacre-like structure electromagnetic shielding fiber material and preparing method thereof |
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