CN111607112A - Color master batch generation process for improving coloring stability of synthetic fibers - Google Patents
Color master batch generation process for improving coloring stability of synthetic fibers Download PDFInfo
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Abstract
The invention discloses a color master batch production process for improving the coloring stability of synthetic fibers, which relates to the technical field of color master batches and comprises the following steps: 1) preparing three-dimensional porous particles by adopting calcium acetate monohydrate, chitosan solution and phosphoric acid; 2) preparing biomass cellulose by using bamboo chips; 3) treating the pretreated organic pigment to obtain a nano-coated organic pigment; 4) preparing the composite aerogel by using biomass cellulose, nano-coated organic pigment, three-dimensional porous particles and guanidine hydrochloride; 5) and grinding the composite aerogel, blending and extruding the ground composite aerogel with polyethylene, and then melting and blending the ground composite aerogel with a solubilizer and butylene terephthalate to obtain the required color master batch. According to the invention, the migration of the pigment particles under the external acting force is reduced, and the movement resistance of the pigment particles in the migration process is increased, so that the inhibition effect on the pigment particles during the migration is enhanced, and the coloring stability of the color master batch in the synthetic fiber is improved.
Description
Technical Field
The invention belongs to the technical field of color master batches, and particularly relates to a color master batch production process for improving the coloring stability of synthetic fibers.
Background
Synthetic fibers are chemical fibers made by spinning, forming and post-treating synthetic, linear polymers of suitable molecular weight and solubility (or meltability). Such polymers having fiber-forming properties are commonly referred to as fiber-forming polymers. Compared with natural fiber and artificial fiber, the raw material of the synthetic fiber is prepared by artificial synthesis method, and the production is not limited by natural conditions. Besides the general excellent properties of chemical fiber, such as high strength, light weight, easy washing and quick drying, good elasticity and resistance to mildew and moth, the synthetic fibers of different varieties have certain unique properties.
At present, there are two main ways of coloring synthetic fibers, one is dyeing after spinning, so-called "post-dyeing and finishing"; the other method is a dope dyeing method before spinning, namely adding pigment for dyeing before spinning. The former has complex process and higher cost; the latter process is relatively simple and low in cost. The color master batch coloring technology is a dope coloring technology before spinning. The colour master batch is composed of three basic elements of pigment or dye, carrier and additive, and is an aggregate made up by uniformly loading an excessive quantity of pigment in resin, its colouring power is higher than that of pigment itself, and when it is processed, a small quantity of colour master batch and uncoloured resin are mixed together so as to obtain the coloured resin or product with designed pigment concentration. The color master batch coloring method is simple and convenient to operate, accurate in metering, less in equipment pollution, easy to clean, convenient to use and easy to change colors. However, in practical application, the technical defects of large color difference and poor coloring stability exist, and the coloring effect is not ideal. For example, chinese patent CN2013101948933 discloses a colored polyester-polypropylene composite ultrafine fiber and a production method thereof, disclosing that the coloring strength of a color master batch on polyester is improved by adding an active substance cerium oxide nano powder material, thereby improving the coloring stability, but in practical production application, the coloring strength of the color master batch on polyester is improved by only adding an active substance, the effect is not ideal, especially in the process of spin-drying and washing the polyester fabric at a high rotation speed, the huge centrifugal force easily causes pigment particles to migrate to the surface layer of the fabric, so that the coloring stability is reduced, thereby causing the coloring effect to be unsatisfactory, and the requirements of consumers cannot be met.
Disclosure of Invention
The invention aims to provide a color master batch production process for improving the coloring stability of synthetic fibers aiming at the technical defect of poor coloring stability of the color master batch in the prior art, which reduces the migration of organic pigment particles under the action of external force, increases the motion resistance of the organic pigment particles in the migration process and further enhances the inhibition effect on the migration of the organic pigment particles by avoiding the direct contact of organic pigment with the outside, thereby realizing the improvement of the coloring stability of the color master batch in the synthetic fibers.
The invention is realized by the following technical scheme:
a color master batch production process for improving the coloring stability of synthetic fibers comprises the following specific process steps:
1) adding chitosan into glacial acetic acid solution with the mass percent of 2-4% according to the mass volume ratio of 1:25-30g/ml, stirring until the chitosan is completely dissolved to obtain chitosan solution, and then adding calcium acetate monohydrate, phosphoric acid and chitosan solution according to the mass volume ratio of 2-2.5 g: 0.5-0.6 ml: 50-55ml, dissolving weighed calcium acetate monohydrate in a chitosan solution, adding 80-85% by mass of phosphoric acid, stirring until the calcium acetate monohydrate is completely dissolved, freezing at-20 to-30 ℃ for 5-10h, transferring the frozen calcium acetate monohydrate into a freeze dryer, pre-freezing at-60 to-65 ℃ for 3-4h, then carrying out vacuum freeze drying at-80 to-90 ℃ for 70-75h, taking out a product, chopping the product, putting the product into a sodium hydroxide solution with the mass percent of 5-7%, soaking the product at 35-38 ℃ for 5-7h, washing the product to be neutral by deionized water after the soaking is finished, carrying out freeze drying for 15-25h again, and then grinding the product into powder to obtain three-dimensional porous particles with the particle size of 80-120 um; in the invention, chitosan is used as a template, and short rod-shaped hydroxyapatite is uniformly distributed in the wall of a chitosan pore by a freeze drying technology, so that porous particles with a three-dimensional interconnected pore structure are formed;
2) respectively putting bamboo chips into water and ethanol for ultrasonic cleaning, then soaking the bamboo chips in a sodium hydroxide solution with the concentration of 1-1.5mol/L, stirring for 2-3h at the temperature of 50-60 ℃, heating to 80-90 ℃, continuously stirring for 3-4h, cooling to room temperature, washing with water to be neutral, then dispersing the washed product in distilled water, then adding hydrogen peroxide with the concentration of 30-35% according to 1-2% of the volume of the distilled water, adjusting the pH to 9-10, reacting for 8-10h at the temperature of 50-55 ℃ for decoloration, washing with water and absolute ethyl alcohol, drying, and crushing with a crusher to obtain biomass cellulose; the invention uses bamboo chips as raw materials, and biomass cellulose is extracted from the bamboo chips;
3) weighing sodium polystyrene sulfonate powder according to the mass-to-volume ratio of 1:20-25g/ml, dissolving the sodium polystyrene sulfonate powder in deionized water, adding the organic pigment powder according to the mass ratio of 1:2-3 of the organic pigment to the sodium polystyrene sulfonate, putting a proper amount of zirconia beads in a grinding machine at the rotating speed of 3500-4500r/min for grinding for 1-1.5h, separating the zirconia beads out of the mixed slurry, centrifugally separating and washing the mixed slurry for 3-4 times, dispersing the mixed slurry into the deionized water according to the mass-to-volume ratio of 1:35-45g/ml, adding polydiallyl dimethyl sodium chloride solution accounting for 3-5% of the mass of the dispersion into the dispersion under the ultrasonic condition of 300-400W, ultrasonically treating for 15-25min, centrifugally washing for 3-4 times, repeating the operation for 2-3 times, and drying to obtain the pretreated organic pigment; in the invention, the polyelectrolyte PSS and PDADMAC are used for pretreating the surface of the organic pigment particles, so that the nano silicon dioxide particles can be better adsorbed to the surface of the organic pigment particles, which is beneficial to improving the coverage rate of the nano particles;
4) dispersing 0.7-1.2 parts of pretreated organic pigment particles into 180 parts of ethanol solution with the mass concentration of 70-80%, adding 50-55 parts of distilled water, adding 0.2-0.4 part of polyvinylpyrrolidone while stirring, uniformly mixing, adding 25-28% of ammonia water to adjust the pH to 8.5-10.5, then dropwise adding 23-30 parts of mixed solution of ethyl orthosilicate and ethanol with the volume ratio of 1:4-5, stirring for 20-25h at room temperature, washing with water, centrifuging for 3-4 times, and vacuum drying for 2-3d at room temperature to obtain the nano-coated organic pigment; according to the invention, the surface polarity of the organic pigment can be improved, the interface energy of the organic pigment and the biomass cellulose is reduced, the fixity of the pigment in the fiber and on the surface is improved, and the pigment particles can be prevented from migrating by coating the nano particles on the surface of the organic pigment;
5) pouring the biomass cellulose and the nano-coated organic pigment into a mixer according to the mass ratio of 10-15:1, adding water with the mass of 2-3 times of that of the biomass cellulose into the mixer, mixing for 2-3h at 30-40 ℃, drying for 30-40min by adopting steam with the temperature of 120-, standing at 60-70 deg.C for 10-15h to obtain composite hydrogel, rinsing the hydrogel with water to neutrality, freezing at-50 deg.C to-55 deg.C for 8-12h, and drying in vacuum freeze dryer for 90-110h to obtain composite aerogel; according to the invention, the dyed biomass cellulose is used as a support and is introduced into the aerogel structure to obtain the composite aerogel, the dyed biomass cellulose is inserted into the pores of the three-dimensional structure of the aerogel to be well protected, and the organic pigment can be prevented from being in direct contact with the outside, so that the migration of organic pigment particles under the action of the outside force can be reduced; the added guanidine hydrochloride can interact with active groups of the three-dimensional porous particles, so that a more obvious three-dimensional structure is formed by covalent bond crosslinking in the porous particles, the number of pores formed by the composite aerogel is increased, the movement resistance of the organic pigment particles in the migration process is increased, and the inhibition effect on the migration of the organic pigment particles is further enhanced;
6) grinding the composite aerogel into powder with the particle size of 20-30um, blending and extruding 30-50% of the composite aerogel powder and 50-70% of low-density polyethylene according to a certain mass percentage to obtain a polyethylene composite material, then melting and blending 20-25% of the polyethylene composite material, 3-4% of a solubilizer and 70-80% of butylene terephthalate according to the mass percentage, and extruding and granulating to obtain the required color master batch.
Compared with the prior art, the invention has the following advantages:
according to the color master batch production process provided by the invention, the organic pigment is fixed on the surface and inside of the biomass cellulose, then the dyed biomass cellulose is used as a support and is introduced into the aerogel structure to obtain the composite aerogel, so that the pigment can be prevented from being directly contacted with the outside, the migration of pigment particles can be inhibited, the coloring stability of the organic pigment is improved, meanwhile, the movement resistance of the organic pigment particles in the migration process is increased by the three-dimensional porous structure in the composite aerogel, the inhibiting effect on the migration of the organic pigment particles is further enhanced, and the coloring stability of the color master batch in synthetic fibers can be improved.
Detailed Description
The present invention will be further described with reference to specific embodiments.
Example 1
A color master batch production process for improving the coloring stability of synthetic fibers comprises the following specific process steps:
2) adding chitosan into a glacial acetic acid solution with the mass percent of 2% according to the mass-to-volume ratio of 1:25g/ml, stirring until the chitosan is completely dissolved to obtain a chitosan solution, and then adding calcium acetate monohydrate, phosphoric acid and the chitosan solution according to the mass-to-volume ratio of 2 g: 0.5 ml: 50ml, dissolving the weighed calcium acetate monohydrate in a chitosan solution, adding 80 mass percent of phosphoric acid, stirring until the calcium acetate monohydrate is completely dissolved, freezing at-20 ℃ for 5 hours, transferring the calcium acetate monohydrate into a freeze dryer after freezing, pre-freezing at-60 ℃ for 3 hours, then carrying out vacuum freeze drying at-80 ℃ for 70 hours, taking out a product, chopping the product, putting the product into a 5 mass percent sodium hydroxide solution, soaking the product at 35 ℃ for 5 hours, washing the product to be neutral by deionized water after soaking is finished, carrying out freeze drying again for 15 hours, and then grinding the product into powder to obtain three-dimensional porous particles with the particle size of 80 um;
2) respectively putting bamboo chips into water and ethanol for ultrasonic cleaning, then soaking the bamboo chips in a sodium hydroxide solution with the concentration of 1mol/L, stirring for 2 hours at 50 ℃, heating to 80 ℃, continuing to stir for 3 hours, cooling to room temperature, washing with water to be neutral, then dispersing the product after washing with water into distilled water, then adding hydrogen peroxide with the concentration of 30% according to 1% of the volume of the distilled water, adjusting the pH to 9, reacting for 8 hours at 50 ℃ for decolorization, washing with water and absolute ethyl alcohol, drying, and then crushing with a crusher to obtain biomass cellulose;
3) dissolving weighed sodium polystyrene sulfonate powder in deionized water according to the mass-to-volume ratio of 1:20g/ml, then adding organic pigment powder according to the mass ratio of 1:2 of the organic pigment to the sodium polystyrene sulfonate, putting a proper amount of zirconia beads into a grinding machine at the rotating speed of 3500r/min for grinding for 1h, then separating the zirconia beads out of the mixed slurry, centrifugally separating and washing the mixed slurry for 3 times, then dispersing the mixed slurry into the deionized water according to the mass-to-volume ratio of 1:35g/ml, adding a polydiallyl dimethyl sodium chloride solution accounting for 3% of the mass of the dispersion into the dispersion under the ultrasonic condition of 300W, ultrasonically treating for 15min, centrifugally washing for 3 times, repeating the operation for 2 times, and drying to obtain a pretreated organic pigment;
4) dispersing 0.7 part of pretreated organic pigment particles into 160 parts of ethanol solution with the mass concentration of 70%, adding 50 parts of distilled water, adding 0.2 part of polyvinylpyrrolidone while stirring, uniformly mixing, adding 25% ammonia water with the mass concentration to adjust the pH value to 8.5, then dropwise adding 23 parts of mixed solution of ethyl orthosilicate and ethanol with the volume ratio of 1:4, stirring for 20 hours at room temperature, washing with water, centrifuging for 3 times, and drying in vacuum for 2 days at room temperature to obtain the nano-coated organic pigment;
5) pouring biomass cellulose (with the length of 400-mesh and the diameter of 50-150 nm) and nano-coated organic pigment into a mixer according to the mass ratio of 10:1, adding water with the mass of 2 times of the biomass cellulose into the mixer, mixing for 2h at 30 ℃, drying for 30min by adopting steam at 120 ℃, obtaining dyed biomass cellulose after drying, then ultrasonically dispersing for 300W in deionized water to obtain dispersion liquid with the dyed biomass cellulose content of 5%, adding three-dimensional porous particles according to the mass ratio of 4:1 of the three-dimensional porous particles to the dyed biomass cellulose, continuing to ultrasonically disperse for 20min, then adding guanidine hydrochloride according to the mass ratio of 1:2 of the guanidine hydrochloride to the three-dimensional porous particles, stirring for 5min, transferring to a reaction kettle, standing for 10h at 60 ℃ to obtain composite hydrogel, rinsing the hydrogel to neutrality by using water, freezing for 8h at-50 ℃, then drying the aerogel in a vacuum freeze dryer for 90 hours to obtain composite aerogel;
6) grinding the composite aerogel into powder with the particle size of 20um, blending and extruding 30% of the composite aerogel powder and 70% of low-density polyethylene according to a certain mass percentage to obtain a polyethylene composite material, then melting and blending the polyethylene composite material according to the mass percentage of 20%, 3% of a solubilizer and 77% of butylene terephthalate, and extruding and granulating to obtain the required color master batch.
Control group 1: according to the mass fraction, adding 72% of PBT, 5.5% of micron-sized silicon dioxide, 18% of organic pigment, 1.4% of silane coupling agent, 1.6% of diethylene glycol adipate and 1.5% of amide amine acetate into a high-speed mixer, stirring and mixing at 700r/min and 50 ℃ for 20min to obtain a mixed material, adding the obtained mixed material into a double-screw extruder, and carrying out melt extrusion, air cooling and hot cutting granulation to obtain the color master batch.
The experimental method comprises the following steps: the preparation method of the synthetic fiber comprises the following steps: adding 0.01 part by weight of cerium oxide nano powder material and 5 parts by weight of color master batch into 100 parts by weight of polyester melt, fully dispersing and mixing, keeping the temperature at 235 ℃ for 0.5 hour to obtain functional polyester, carrying out conjugate drawing on the functional polyester melt and the polypropylene melt, coating the functional polyester on the outer surface of the polypropylene fiber to form a composite fiber, wherein in the drawing process, the core wire diameter of the polypropylene fiber is controlled to be 1.5 microns, the core wire spinning temperature of the polypropylene fiber is controlled to be 320 ℃, the spinning temperature of the functional polyester is controlled to be 290 ℃, and the diameter of the coated composite fiber is controlled to be 4 microns; by adopting the process method, the color master batches provided by the embodiment 1 and the comparison group 1 are respectively used for processing to prepare the synthetic fibers, the synthetic fibers are woven to obtain fabric samples, the obtained fabric samples are put into a drum washing machine for washing (the rotating speed is 1200r/min, the water temperature is 45 ℃, and the washing time is 30 min), the embodiment 1 and the comparison group 1 respectively provide 60 fabric samples, each fabric sample is washed for 50 times, after the washing is finished, the color change of each fabric sample before and after the washing is observed, and the results are as follows: the fabric samples provided in example 1 have unchanged color before and after washing, and the fabric samples provided in the control group 1 have unchanged color before and after washing of only 2 fabrics, and the remaining fabrics all have different color depth changes.
Example 2
A color master batch production process for improving the coloring stability of synthetic fibers comprises the following specific process steps:
3) adding chitosan into a glacial acetic acid solution with the mass percent of 3% according to the mass-to-volume ratio of 1:28g/ml, stirring until the chitosan is completely dissolved to obtain a chitosan solution, and then adding calcium acetate monohydrate, phosphoric acid and the chitosan solution according to the mass-to-volume ratio of 2.3 g: 0.55 ml: 52ml, dissolving the weighed calcium acetate monohydrate in a chitosan solution, adding 82% by mass of phosphoric acid, stirring until the calcium acetate monohydrate is completely dissolved, freezing at-25 ℃ for 7 hours, transferring the calcium acetate monohydrate into a freeze dryer after freezing, pre-freezing at-62 ℃ for 3.5 hours, then carrying out vacuum freeze drying at-85 ℃ for 72 hours, taking out the product, chopping the product, putting the product into a sodium hydroxide solution with the mass percentage of 6%, soaking the product at 37 ℃ for 6 hours, washing the product to be neutral by using deionized water after soaking, carrying out freeze drying again for 20 hours, and then grinding the product into powder to obtain three-dimensional porous particles with the particle size of 100 um;
2) respectively putting bamboo chips into water and ethanol for ultrasonic cleaning, then soaking the bamboo chips in a sodium hydroxide solution with the concentration of 1.2mol/L, stirring for 2.5h at 55 ℃, heating to 85 ℃, continuously stirring for 3.5h, cooling to room temperature, washing with water to be neutral, then dispersing the product after washing with water into distilled water, then adding hydrogen peroxide with the concentration of 32% according to 1.5% of the volume of the distilled water, adjusting the pH to 9.5, reacting for 9h at 52 ℃, decoloring, washing with water and absolute ethanol, drying, and crushing by a crusher to obtain biomass cellulose;
3) dissolving weighed sodium polystyrene sulfonate powder in deionized water according to the mass-to-volume ratio of 1:23g/ml, then adding organic pigment powder according to the mass ratio of 1:2.5 of the organic pigment to the sodium polystyrene sulfonate, putting a proper amount of zirconia beads into a grinding machine at the rotating speed of 4000r/min for grinding for 1.2h, then separating the zirconia beads out of the mixed slurry, centrifugally separating and washing the mixed slurry for 3 times, then dispersing the mixed slurry into the deionized water according to the mass-to-volume ratio of 1:40g/ml, adding a polydiallyldimethyl sodium chloride solution accounting for 4% of the mass of the dispersion into the dispersion under the ultrasonic condition of 350W, ultrasonically treating for 20min, centrifugally washing for 3 times, repeating the operation for 2 times, and drying to obtain a pretreated organic pigment;
4) dispersing 1.0 part of pretreated organic pigment particles into 170 parts of 75% ethanol solution by mass concentration, adding 52 parts of distilled water, adding 0.3 part of polyvinylpyrrolidone while stirring, uniformly mixing, adding 26% ammonia water by mass concentration to adjust the pH to 9.0, then dropwise adding 28 parts of mixed solution of ethyl orthosilicate and ethanol in a volume ratio of 1:4.5, stirring for 21 hours at room temperature, washing with water, centrifuging for 3 times, and vacuum-drying for 2 days at room temperature to obtain the nano-coated organic pigment;
5) pouring biomass cellulose and nano-coated organic pigment into a mixer according to the mass ratio of 12:1, adding water with the mass of 2.5 times of that of the biomass cellulose into the mixer, mixing for 2.5h at 35 ℃, drying for 35min by adopting steam with the temperature of 125 ℃, obtaining dyed biomass cellulose after drying, then ultrasonically dispersing in deionized water with 350W to obtain dispersion liquid with the dyed biomass cellulose content of 7%, adding three-dimensional porous particles according to the mass ratio of the three-dimensional porous particles to the dyed biomass cellulose of 4.5:1, continuing to ultrasonically disperse for 25min, then adding guanidine hydrochloride according to the mass ratio of the guanidine hydrochloride to the three-dimensional porous particles of 1:2.5, stirring for 7min, transferring into a reaction kettle, standing for 12h at the temperature of 65 ℃ to obtain composite hydrogel, leaching the hydrogel with water to be neutral, freezing for 10h at the temperature of-52 ℃, then drying for 100h in a vacuum freeze dryer, obtaining the composite aerogel;
6) grinding the composite aerogel into powder with the particle size of 30um, blending and extruding 40% of the composite aerogel powder and 60% of low-density polyethylene according to a certain mass percentage to obtain a polyethylene composite material, then melting and blending the polyethylene composite material according to the mass percentage of 23%, 4% of a solubilizer and 73% of butylene terephthalate, and extruding and granulating to obtain the required color master batch.
Control group 2: according to the mass fraction, adding 70% of PBT, 5.8% of micron-sized silicon dioxide, 20% of organic pigment, 1.4% of silane coupling agent, 1.5% of diethylene glycol adipate and 1.3% of amide amine acetate into a high-speed mixer, stirring and mixing at 700r/min and 50 ℃ for 20min to obtain a mixed material, adding the obtained mixed material into a double-screw extruder, and carrying out melt extrusion, air cooling and hot cutting granulation to obtain the color master batch.
The experimental method comprises the following steps: the preparation method of the synthetic fiber comprises the following steps: adding 0.01 part by weight of cerium oxide nano powder material and 5 parts by weight of color master batch into 100 parts by weight of polyester melt, fully dispersing and mixing, keeping the temperature at 235 ℃ for 0.5 hour to obtain functional polyester, carrying out conjugate drawing on the functional polyester melt and the polypropylene melt, coating the functional polyester on the outer surface of the polypropylene fiber to form a composite fiber, wherein in the drawing process, the core wire diameter of the polypropylene fiber is controlled to be 1.5 microns, the core wire spinning temperature of the polypropylene fiber is controlled to be 320 ℃, the spinning temperature of the functional polyester is controlled to be 290 ℃, and the diameter of the coated composite fiber is controlled to be 4 microns; by adopting the process method, the color master batches provided by the embodiment 2 and the comparison group 2 are respectively used for processing to prepare the synthetic fibers, the synthetic fibers are woven to obtain fabric samples, the obtained fabric samples are put into a drum washing machine for washing (the rotating speed is 1200r/min, the water temperature is 45 ℃, and the washing time is 30 min), the embodiment 2 and the comparison group 2 respectively provide 60 fabric samples, each fabric sample is washed for 50 times, after the washing is finished, the color change of each fabric sample before and after the washing is observed, and the results are as follows: the fabric samples provided in example 2 have no color change before and after washing, and the color of only 1 fabric sample provided in the control group 2 has no color change before and after washing, and the remaining fabrics all have color depth difference changes.
Example 3
A color master batch production process for improving the coloring stability of synthetic fibers comprises the following specific process steps:
4) adding chitosan into a glacial acetic acid solution with the mass percent of 4% according to the mass-to-volume ratio of 1:30g/ml, stirring until the chitosan is completely dissolved to obtain a chitosan solution, and then adding calcium acetate monohydrate, phosphoric acid and the chitosan solution according to the mass-to-volume ratio of 2.5 g: 0.6 ml: 55ml, dissolving the weighed calcium acetate monohydrate in a chitosan solution, adding phosphoric acid with the mass fraction of 85% into the solution, stirring the solution until the calcium acetate monohydrate is completely dissolved, freezing the solution at minus 30 ℃ for 10 hours, transferring the frozen solution into a freeze dryer, pre-freezing the solution at minus 65 ℃ for 4 hours, then carrying out vacuum freeze drying at minus 90 ℃ for 75 hours, taking out the product, chopping the product, putting the product into a sodium hydroxide solution with the mass fraction of 7%, soaking the product at 38 ℃ for 7 hours, washing the product to be neutral by deionized water after the soaking is finished, carrying out freeze drying again for 25 hours, and then grinding the product into powder to obtain three-dimensional porous particles with the particle size of 120 um;
2) respectively putting bamboo chips into water and ethanol for ultrasonic cleaning, then soaking the bamboo chips into a sodium hydroxide solution with the concentration of 1.5mol/L, stirring for 3 hours at the temperature of 60 ℃, heating to 90 ℃, continuously stirring for 4 hours, cooling to room temperature, washing with water to be neutral, then dispersing the product after washing with water into distilled water, then adding hydrogen peroxide with the concentration of 35% according to 2% of the volume of the distilled water, adjusting the pH to 10, reacting for 10 hours at the temperature of 55 ℃, decoloring, washing with water and absolute ethyl alcohol, drying, and crushing by a crusher to obtain biomass cellulose;
3) dissolving weighed sodium polystyrene sulfonate powder in deionized water according to the mass-to-volume ratio of 1:25g/ml, then adding organic pigment powder according to the mass ratio of 1:3 of the organic pigment to the sodium polystyrene sulfonate, putting a proper amount of zirconia beads into a grinding machine at the rotating speed of 4500r/min for grinding for 1.5h, then separating the zirconia beads out of the mixed slurry, centrifugally separating and washing the mixed slurry for 4 times, then dispersing the mixed slurry into the deionized water according to the mass-to-volume ratio of 1:45g/ml, adding a polydiallyldimethyl sodium chloride solution accounting for 5% of the mass of the dispersion into the dispersion under the ultrasonic condition of 400W, ultrasonically treating for 25min, centrifugally washing for 4 times, repeating the operation for 3 times, and drying to obtain a pretreated organic pigment;
4) dispersing 1.2 parts of pretreated organic pigment particles into 180 parts of ethanol solution with the mass concentration of 80%, adding 55 parts of distilled water, adding 0.4 part of polyvinylpyrrolidone while stirring, uniformly mixing, adding ammonia water with the mass concentration of 28% to adjust the pH value to 10.5, then dropwise adding 30 parts of mixed solution of ethyl orthosilicate and ethanol with the volume ratio of 1:5, stirring for 25 hours at room temperature, washing with water, centrifuging for 4 times, and drying in vacuum for 3 days at room temperature to obtain the nano-coated organic pigment;
5) pouring biomass cellulose and nano-coated organic pigment into a mixer according to the mass ratio of 15:1, adding water with the mass of 3 times of that of the biomass cellulose into the mixer, mixing for 3h at 40 ℃, drying for 40min by adopting steam at 130 ℃, obtaining dyed biomass cellulose after drying, then ultrasonically dispersing 400W in deionized water to obtain dispersion liquid with the dyed biomass cellulose content of 10%, adding three-dimensional porous particles according to the mass ratio of 5:1 of the three-dimensional porous particles to the dyed biomass cellulose, continuing to ultrasonically disperse for 30min, then adding guanidine hydrochloride according to the mass ratio of 1:3 of the guanidine hydrochloride to the three-dimensional porous particles, stirring for 8min, transferring to a reaction kettle, standing for 15h at 70 ℃ to obtain composite hydrogel, rinsing the hydrogel with water to neutrality, freezing for 12h at-55 ℃, then drying for 110h in a vacuum freeze dryer, obtaining the composite aerogel;
6) grinding the composite aerogel into powder with the particle size of 30um, blending and extruding 50% of the composite aerogel powder and 50% of low-density polyethylene according to a certain mass percentage to obtain a polyethylene composite material, then melting and blending the polyethylene composite material according to the mass percentage of 25%, 4% of solubilizer and 71% of butylene terephthalate, and extruding and granulating to obtain the required color master batch.
Control group 3: according to the mass fraction, adding 70% of PBT, 6% of micron-sized silicon dioxide, 20% of organic pigment, 1.25% of silane coupling agent, 1.35% of diethylene glycol adipate and 1.4% of amine acetate into a high-speed mixer, stirring and mixing for 20min at 700r/min and 50 ℃ to obtain a mixed material, adding the obtained mixed material into a double-screw extruder, and carrying out melt extrusion, air-cooling and hot-cutting granulation to obtain the color master batch.
The experimental method comprises the following steps: the preparation method of the synthetic fiber comprises the following steps: adding 0.01 part by weight of cerium oxide nano powder material and 5 parts by weight of color master batch into 100 parts by weight of polyester melt, fully dispersing and mixing, keeping the temperature at 235 ℃ for 0.5 hour to obtain functional polyester, carrying out conjugate drawing on the functional polyester melt and the polypropylene melt, coating the functional polyester on the outer surface of the polypropylene fiber to form a composite fiber, wherein in the drawing process, the core wire diameter of the polypropylene fiber is controlled to be 1.5 microns, the core wire spinning temperature of the polypropylene fiber is controlled to be 320 ℃, the spinning temperature of the functional polyester is controlled to be 290 ℃, and the diameter of the coated composite fiber is controlled to be 4 microns; by adopting the process method, the color master batches provided by the embodiment 3 and the comparison group 3 are respectively used for processing to prepare the synthetic fibers, the synthetic fibers are woven to obtain fabric samples, the obtained fabric samples are put into a drum washing machine for washing (the rotating speed is 1200r/min, the water temperature is 45 ℃, and the washing time is 30 min), the embodiment 3 and the comparison group 3 respectively provide 60 fabric samples, each fabric sample is washed for 50 times, after the washing is finished, the color change of each fabric sample before and after the washing is observed, and the results are as follows: the fabric samples provided in example 3 did not change in color before and after washing, and only 3 fabric samples provided in control group 3 did not change in color before and after washing, and the remaining fabric samples all showed a difference in color depth.
The experiments show that the coloring stability of the color master batch in the synthetic fiber can be improved by enhancing the inhibiting effect on the migration of the organic pigment particles, so that the coloring effect of the synthetic fiber is improved, and the colored synthetic fiber cannot fade in the long-term use and washing process.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention.
Claims (10)
1. A color master batch production process for improving the coloring stability of synthetic fibers is characterized by comprising the following specific process steps:
weighing a proper amount of calcium acetate monohydrate, dissolving the calcium acetate monohydrate in a chitosan solution, adding a proper amount of phosphoric acid with the mass fraction of 80-85%, stirring until the calcium acetate monohydrate is completely dissolved, freezing the calcium acetate monohydrate at the temperature of-20 to-30 ℃ for 5-10h, transferring the calcium acetate monohydrate into a freeze dryer for pre-freezing after freezing, then carrying out vacuum freeze drying at the temperature of-80 to-90 ℃ for 70-75h, taking out the product, chopping the product, soaking the product in a sodium hydroxide solution, washing the product to be neutral by deionized water after soaking, carrying out freeze drying for 15-25h again, and then grinding the product into powder to obtain three-dimensional porous particles;
2) respectively putting bamboo chips into water and ethanol for ultrasonic cleaning, then soaking the bamboo chips in a sodium hydroxide solution with the concentration of 1-1.5mol/L, stirring for 2-3h at the temperature of 50-60 ℃, heating to 80-90 ℃, continuously stirring for 3-4h, cooling to room temperature, washing with water to be neutral, then soaking and decoloring in hydrogen peroxide, washing with water and absolute ethyl alcohol, drying, and crushing by a crusher to obtain biomass cellulose;
3) dispersing pretreated organic pigment particles into an ethanol solution, adding a proper amount of distilled water, adding polyvinylpyrrolidone while stirring, uniformly mixing, adding ammonia water to adjust the pH value to 8.5-10.5, then dropwise adding a mixed solution of ethyl orthosilicate and ethanol, stirring at room temperature for 20-25h, washing with water, centrifuging for 3-4 times, and drying at room temperature in vacuum for 2-3d to obtain a nano-coated organic pigment;
4) pouring biomass cellulose and nano-coated organic pigment into a mixer, adding a proper amount of water into the mixer, mixing for 2-3h at 30-40 ℃, drying to obtain dyed biomass cellulose, then performing 300-400W ultrasonic dispersion in deionized water to obtain dispersion liquid, adding a proper amount of three-dimensional porous particles, continuing performing ultrasonic dispersion for 20-30min, then adding a proper amount of guanidine hydrochloride, stirring for 5-8min, transferring to a reaction kettle, standing for 10-15h at 60-70 ℃ to obtain composite hydrogel, leaching the hydrogel with water to neutrality, freezing, and drying in a vacuum freeze dryer to obtain composite aerogel;
5) grinding the composite aerogel into powder, blending and extruding the powder with low-density polyethylene according to a certain mass percentage to obtain a polyethylene composite material, then melting and blending the polyethylene composite material by 20-25% by mass, 3-4% by mass of a solubilizer and 70-80% by mass of butylene terephthalate, and extruding and granulating to obtain the required color master batch.
2. The process for producing color masterbatch for improving the coloring stability of synthetic fiber according to claim 1, wherein in the step 1), the chitosan solution is prepared by the following steps: adding chitosan into 2-4% glacial acetic acid solution according to the mass volume ratio of 1:25-30g/ml, and stirring until the chitosan is completely dissolved.
3. The process for producing color masterbatch for improving the coloring stability of synthetic fiber according to claim 1, wherein in the step 1), the mass-to-volume ratio of the calcium acetate monohydrate, the phosphoric acid and the chitosan solution is 2-2.5 g: 0.5-0.6 ml: 50-55 ml; the pre-freezing temperature is-60 to-65 ℃, and the pre-freezing time is 3 to 4 hours; the mass percent of the sodium hydroxide solution is 5-7%; the soaking temperature is 35-38 ℃, and the soaking time is 5-7 h; the particle size of the three-dimensional porous particles is 80-120 um.
4. The color master batch production process for improving the coloring stability of the synthetic fiber according to claim 1, wherein in the process step 2), the hydrogen peroxide solution soaking and decoloring treatment comprises the following steps: dispersing the product after water washing in distilled water, adding 30-35% hydrogen peroxide according to 1-2% of the volume of the distilled water, adjusting the pH to 9-10, and reacting at 50-55 ℃ for 8-10 h.
5. The process for producing color concentrates for improving the color stability of synthetic fibers according to claim 1, wherein in step 3), the pretreated organic pigment is prepared by the following steps: weighing sodium polystyrene sulfonate powder according to the mass-to-volume ratio of 1:20-25g/ml, dissolving the sodium polystyrene sulfonate powder in deionized water, adding the organic pigment powder according to the mass ratio of 1:2-3 of the organic pigment to the sodium polystyrene sulfonate, putting a proper amount of zirconia beads in a grinding machine at the rotating speed of 3500-4500r/min for grinding for 1-1.5h, separating the zirconia beads out of the mixed slurry, centrifugally separating and washing the mixed slurry for 3-4 times, dispersing the mixed slurry into the deionized water according to the mass-to-volume ratio of 1:35-45g/ml, adding polydiallyl dimethyl sodium chloride solution accounting for 3-5% of the mass of the dispersion into the dispersion under the ultrasonic condition of 300-400W, ultrasonically treating for 15-25min, centrifugally washing for 3-4 times, repeating the operation for 2-3 times, and drying to obtain the pretreated organic pigment.
6. The process for producing color masterbatch for improving the coloring stability of synthetic fiber according to claim 1, wherein in the step 3), the raw materials comprise the following components in parts by weight: 0.7-1.2 parts of pretreated organic pigment, 180 parts of ethanol 160-containing materials, 50-55 parts of water, 0.2-0.4 part of polyvinylpyrrolidone and 23-30 parts of mixed solution of tetraethoxysilane and ethanol.
7. The process for producing color masterbatch for improving the coloring stability of synthetic fiber according to claim 1, wherein in the step 3), the concentration of ammonia water is 25-28%; the concentration of the ethanol is 70-80%; in the mixed solution of the ethyl orthosilicate and the ethanol, the volume ratio of the ethyl orthosilicate to the ethanol is 1: 4-5.
8. The color master batch production process for improving the coloring stability of the synthetic fiber according to claim 1, wherein in the process step 4), the mass ratio of the biomass cellulose to the nano-coated organic pigment is 10-15: 1; the addition amount of the water is 2-3 times of the mass of the biological cellulose; the drying is carried out by adopting steam at the temperature of 120-130 ℃ for 30-40 min.
9. The process for producing color masterbatch for improving the coloring stability of synthetic fiber according to claim 1, wherein in the step 4), the content of dyed biomass cellulose in the dispersion is 5-10%; the mass ratio of the three-dimensional porous particles to the dyed biomass cellulose is 4-5: 1; the mass ratio of the guanidine hydrochloride to the three-dimensional porous particles is 1: 2-3; the temperature of the frozen hydrogel is-50 ℃ to-55 ℃, and the freezing time is 8-12 h; the vacuum freeze drying time is 90-110 h.
10. The color master batch production process for improving the coloring stability of the synthetic fiber according to claim 1, wherein in the process step 5), the ground composite aerogel has a particle size of 20-30um and the mass percentages of the ground composite aerogel and the low-density polyethylene are 30-50% and 50-70%, respectively; the solubilizer is at least one of styrene-maleic anhydride copolymer, PE graft and methyl methacrylate-butadiene-styrene copolymer.
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