CN112210094A - Antibacterial agent-containing slow-release porous aerogel PET color master batch and preparation method thereof - Google Patents
Antibacterial agent-containing slow-release porous aerogel PET color master batch and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a sustained-release porous aerogel PET color master batch containing an antibacterial agent, which comprises the following steps: s1, preparing an antibacterial agent solution; s2, preparing porous aerogel; s3, preparing porous aerogel containing an antibacterial agent; s4, preparing the PET color master batch containing the antibacterial agent and the slow-release porous aerogel. The prepared antibacterial agent-containing slow-release porous aerogel PET color master batch is mainly used for coloring fibers before spinning, can not only color PET fibers, but also endow colored PET fibers with excellent antibacterial property and excellent mechanical property.
Description
Technical Field
The invention relates to the technical field of PET materials, and particularly relates to a PET color master batch containing an antibacterial agent and slow-release porous aerogel and a preparation method thereof.
Background
At present, the yield of polyester fibers in China exceeds thousands of tons, one third of the polyester fibers needs to be colored, 4000 thousands of tons of colored sewage are discharged every year by using a dye dyeing method, and the color fastness of the dyeing, such as light fastness, washing fastness, perspiration fastness, sublimation fastness and the like, is far lower than that of the dyeing before spinning, so that the method is not suitable for the needs of social development and improvement of living standard of people. The dyeing before spinning of the terylene is a new process for directly preparing colored terylene fiber by melting or dispersing the color master batch in the polyester spinning solution for melt spinning, and is the most effective way for omitting the dyeing of the terylene.
Along with the improvement of the living standard of people, people increasingly pay attention to the antibacterial property of clothes and textile ornaments. At present, the production method of the colored polyester yarn is to add single color master batch for coloring during spinning, and add single antibacterial master batch to endow antibacterial performance when the antibacterial performance is needed, so that the defects of multiple processing components, complex process and the like are caused.
The aerogel is a light nano solid material which is formed by mutually gathering nano-scale ultrafine particles to form a nano porous network structure and is filled with gaseous dispersion media in network pores. The porosity is as high as 99.8%, the typical size of the holes is 1-40 nm, and the specific surface area is 400-1200 m2In terms of/g, and a density as low as 3kg/m3The heat conductivity coefficient at room temperature can be as low as below 0.010W/(m.K), and the light-weight, light-transmitting, heat-insulating, heat-preserving, sound-insulating, fireproof and impact-resistant light-weight material has excellent chemical stability and non-inflammability. Due to the characteristics, the silica aerogel material has wide application potential in the aspects of materials, thermal, acoustic, optical, microelectronic, particle detection and the like.
Disclosure of Invention
The invention aims to provide an antibacterial agent-containing slow-release porous aerogel PET color master batch and a preparation method thereof, and the prepared antibacterial agent-containing slow-release porous aerogel PET color master batch is mainly used for coloring fibers before spinning, can not only color PET fibers, but also endow colored PET filaments with excellent antibacterial property and excellent mechanical property.
The technical scheme of the invention is realized as follows:
the invention provides a preparation method of a sustained-release porous aerogel PET color master batch containing an antibacterial agent, which comprises the following steps:
s1, preparing an antibacterial agent solution;
s2, preparing porous aerogel;
s3, preparing porous aerogel containing an antibacterial agent;
s4, preparing the PET color master batch containing the antibacterial agent and the slow-release porous aerogel.
As a further improvement of the invention, the antibacterial agent is a mixture of nisin and natamycin, the mass ratio is 3: 1-3, the content of the antibacterial agent in the antibacterial agent solution is 5-10 wt%, and the balance is water.
As a further improvement of the present invention, step S2 includes:
s201, cooling a mixed aqueous solution containing NaOH and urea to below 5 ℃, adding graphene oxide into the mixed solution, mechanically stirring to obtain a graphene oxide solution, adding sodium carboxymethylcellulose into another mixed aqueous solution containing NaOH and urea, mechanically stirring to obtain a sodium carboxymethylcellulose solution, and mixing the graphene oxide solution and the sodium carboxymethylcellulose solution according to the volume ratio of 1: 1-3 to obtain a mixed solution;
s202, pouring liquid paraffin into a reactor, mechanically stirring, dropwise adding the mixed solution into the liquid paraffin, and mechanically stirring after dropwise adding; and then adding epoxy chloropropane into the liquid paraffin, reacting at room temperature, neutralizing with hydrochloric acid after the reaction is finished, removing the upper layer of the liquid paraffin, repeatedly washing the lower layer of the standard product with distilled water and absolute ethyl alcohol to obtain hydrogel beads, and freeze-drying the hydrogel to obtain the porous aerogel.
As a further improvement of the invention, in the mixed aqueous solution containing NaOH and 5-10 wt% of urea, the mass fraction of the NaOH is 3-5 wt%, and the mass fraction of the urea is 5-10 wt%; the volume-mass ratio of the mixed aqueous solution containing NaOH and urea to the graphene oxide is (10-30) to 1; the volume-mass ratio of the mixed aqueous solution containing NaOH and urea to the sodium carboxymethyl cellulose is (30-50) to 1; the mass ratio of the liquid paraffin to the mixed solution to the epichlorohydrin is 100: 10-30: 5-12.
As a further improvement of the present invention, step S3 includes the following steps: sequentially adding the antibacterial agent solution, the porous aerogel, the coupling agent and the surfactant into a shearing disperser, heating to 50 ℃, preserving heat, performing first shearing dispersion, then adding a stabilizer accounting for 0.1-5 wt% of the total mass of the materials, performing second shearing to obtain a porous aerogel suspension dispersion liquid containing the antibacterial agent, and volatilizing the solvent to obtain the dry porous aerogel containing the antibacterial agent.
As a further improvement of the invention, the shearing force of the first shearing and dispersing is 5250-6000ips, the shearing time is 4-9min, the temperature rising rate is 3 ℃/min, the shearing force of the second shearing and dispersing is 2500-3000ips, and the shearing time is 5-10 min; the coupling agent is a mixture of a silane coupling agent KH550 and a silane coupling agent KH570, the mass ratio is 5: 1-3, the surfactant is a mixture of Tween-80 and span-80, the mass ratio is 10: 1-3, and the stabilizer is a mixture of magnesium stearate and aluminum stearate, and the mass ratio is 1: 2-4.
As a further improvement of the present invention, step S4 includes the following steps: adding the dried porous aerogel containing the antibacterial agent into a grinding machine, adding the pigment, the dispersing agent and the antioxidant, mixing and grinding to obtain a composite modifier containing the antibacterial agent; and adding the composite modifier containing the antibacterial agent into the PET slices, melting at high temperature, keeping the melting for 10-15min, and extruding and granulating to obtain the PET color master batch containing the antibacterial agent slow-release porous aerogel.
As a further improvement of the invention, the high-temperature melting temperature is 300-500 ℃, and the dispersant is selected from one of sodium polyacrylate, potassium polyacrylate and ammonium polyacrylate; the antioxidant is selected from one of 2, 4-di- (n-octylthiomethylene) -6-methylphenol, 2, 4-di (dodecylthiomethyl) -6-methylphenol, dilauryl thiodipropionate or distearyl thiodipropionate; the pigment is one or a mixture of phthalocyanine pigment, titanium dioxide, carbon black, ultramarine pigment and titanium yellow pigment.
As a further improvement of the invention, the method comprises the following steps:
s1, preparing an antibacterial agent solution: mixing nisin and natamycin in a mass ratio of 3 to (1-3) to obtain an antibacterial agent, and preparing the antibacterial agent and water into an antibacterial agent solution, wherein the content of the antibacterial agent is 5-10 wt%;
s2, preparing the porous aerogel:
s201, putting 10-30 parts by weight of mixed aqueous solution containing 3-5 wt% of NaOH and 5-10 wt% of urea into a refrigerator, freezing to-10 ℃, adding 1 part by weight of graphene oxide into the mixed solution, mechanically stirring for 5min to obtain graphene oxide solution, adding 1 part by weight of sodium carboxymethylcellulose into another 30-50 parts by weight of mixed aqueous solution containing 3-5 wt% of NaOH and 5-10 wt% of urea, mechanically stirring for 1-2h to obtain sodium carboxymethylcellulose solution, and mixing the graphene oxide solution and the sodium carboxymethylcellulose solution according to the volume ratio of 1: 1-3 to obtain mixed solution;
s202, pouring 100 parts by weight of liquid paraffin into a reactor, mechanically stirring for 10-20min, dripping 10-30 parts by weight of mixed solution into the liquid paraffin, and mechanically stirring for 10-30min after dripping is finished; adding 5-12 parts by weight of epichlorohydrin into liquid paraffin, reacting at room temperature for 1-3h, neutralizing with 5-12% hydrochloric acid after the reaction is finished, removing the upper layer of liquid paraffin, repeatedly washing the lower layer of standard product with distilled water and absolute ethyl alcohol to obtain hydrogel beads, and freeze-drying the hydrogel to obtain porous aerogel;
s3, preparing the porous aerogel containing the antibacterial agent: sequentially adding 2-5 parts by weight of an antibacterial agent solution, 10-20 parts by weight of porous aerogel, 1-2 parts by weight of a coupling agent and 0.5-1.5 parts by weight of a surfactant into a shearing disperser, heating to 50 ℃ at a speed of 3 ℃/min, preserving heat, performing primary shearing dispersion, wherein the shearing force is 5250-6000ips, the shearing time is 4-9min, then adding a stabilizer accounting for 0.1-5 wt% of the total mass of the materials, performing secondary shearing, wherein the shearing force is 2500-3000ips, and the shearing time is 5-10min to obtain a porous aerogel suspension dispersion liquid containing the antibacterial agent, and volatilizing the solvent to obtain the dry porous aerogel containing the antibacterial agent;
s4, preparing the antibacterial agent-containing slow-release porous aerogel PET color master batch: adding 5-10 parts by weight of dried porous aerogel containing the antibacterial agent into a grinding machine, adding 2-5 parts by weight of pigment, 1-3 parts by weight of dispersing agent and 0.5-1 part by weight of antioxidant, mixing and grinding to obtain a composite modifier containing the antibacterial agent; adding 5-10 parts by weight of composite modifier containing the antibacterial agent into 100 parts by weight of PET slices, melting at the high temperature of 300-500 ℃, keeping the melting for 10-15min, and extruding and granulating to obtain the PET color master batch containing the antibacterial agent slow-release porous aerogel.
The invention further protects the antibacterial agent-containing slow-release porous aerogel PET color master batch prepared by the preparation method.
The invention has the following beneficial effects: according to the invention, the antibacterial agent-containing slow-release porous aerogel is prepared by using the porous aerogel ingeniously, so that the master batch has good antibacterial and bacteriostatic properties, aromaticity, anti-sensitivity or anti-inflammatory properties and other functions, the antibacterial agent-containing porous aerogel is uniformly dispersed in the slices, and the prepared master batch is further prepared into fibers and has good functions;
the nisin is a polypeptide substance produced by streptococcus lactis, can inhibit the growth and reproduction of most gram-positive bacteria, has strong inhibiting effect on spores of bacillus, has special effect on the gram-positive bacteria producing the spores, has an antibacterial mechanism by interfering the normal function of cell membranes to cause the permeation, nutrient loss and membrane potential reduction of the cell membranes so as to cause the death of pathogenic bacteria and putrefying bacteria cells, and has an action mechanism of combining with ergosterol and other sterol groups of fungi to inhibit the biosynthesis of the ergosterol so as to distort the cell membranes and finally cause leakage and cause the cell death; after the nisin and the natamycin are compounded, most of bacteria, fungi and the like can be killed or inhibited from increasing in value, so that the efficient antibacterial effect is achieved, and the composite antibacterial agent has good anti-aging performance.
The prepared antibacterial agent-containing slow-release porous aerogel PET color master batch is mainly used for coloring fibers before spinning, can not only color PET fibers, but also endow colored PET fibers with excellent antibacterial property and excellent mechanical property.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is an SEM image of a porous aerogel prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1 controlled release porous aerogel PET color masterbatch containing antimicrobial agent
The method comprises the following steps:
s1, preparing an antibacterial agent solution: mixing nisin and natamycin in a mass ratio of 3: 1 to obtain an antibacterial agent, and preparing the antibacterial agent and water into an antibacterial agent solution, wherein the content of the antibacterial agent is 5 wt%;
s2, preparing the porous aerogel:
s201, putting 10g of mixed aqueous solution containing 3 wt% of NaOH and 5 wt% of urea into a refrigerator, freezing to-10 ℃, adding 1g of graphene oxide into the mixed solution, mechanically stirring for 5min to obtain a graphene oxide solution, adding 1g of sodium carboxymethylcellulose into another 30g of mixed aqueous solution containing 3 wt% of NaOH and 5 wt% of urea, mechanically stirring for 1h to obtain a sodium carboxymethylcellulose solution, and mixing the graphene oxide solution and the sodium carboxymethylcellulose solution according to the volume ratio of 1: 1 to obtain a mixed solution;
s202, pouring 100g of liquid paraffin into a reactor, mechanically stirring for 10min, dropwise adding 10g of mixed solution into the liquid paraffin, and mechanically stirring for 10min after dropwise adding; adding 5g of epichlorohydrin into liquid paraffin, reacting at room temperature for 1h, neutralizing with 5% hydrochloric acid after the reaction is finished, removing the upper layer of liquid paraffin, repeatedly washing the lower layer of standard product with distilled water and absolute ethyl alcohol to obtain hydrogel beads, and freeze-drying the hydrogel to obtain the porous aerogel, wherein an SEM picture of the porous aerogel is shown in figure 1, and the particle size of the porous aerogel is 200-300 nm;
s3, preparing the porous aerogel containing the antibacterial agent: sequentially adding 2g of an antibacterial agent solution, 10g of porous aerogel, 1g of a coupling agent and 0.5g of a surfactant into a shearing disperser, heating to 50 ℃ at a speed of 3 ℃/min, preserving heat, carrying out first shearing dispersion, wherein the shearing force is 5250ips, the shearing time is 4min, then adding a stabilizer accounting for 0.1 wt% of the total mass of the materials, carrying out second shearing, the shearing force is 2500ips, the shearing time is 5min, obtaining a porous aerogel suspension dispersion liquid containing the antibacterial agent, and volatilizing the solvent to obtain the dried porous aerogel containing the antibacterial agent;
the coupling agent is a mixture of a silane coupling agent KH550 and a silane coupling agent KH570 in a mass ratio of 5: 1, the surfactant is a mixture of Tween-80 and span-80 in a mass ratio of 10: 1, and the stabilizer is a mixture of magnesium stearate and aluminum stearate in a mass ratio of 1: 2.
S4, preparing the antibacterial agent-containing slow-release porous aerogel PET color master batch: adding 5g of dried porous aerogel containing the antibacterial agent into a grinding machine, adding 2g of titanium yellow pigment, 1g of sodium polyacrylate and 0.5g of 2, 4-bis (dodecyl-sulfur methyl) -6-methylphenol, mixing and grinding to obtain a composite modifier containing the antibacterial agent; and adding 5g of composite modifier containing the antibacterial agent into 100 parts by weight of PET slices, melting at the high temperature of 300 ℃, keeping the melting for 10min, and extruding and granulating to obtain the PET color master batch containing the antibacterial agent slow-release porous aerogel.
Example 2 controlled release porous aerogel PET color masterbatch containing antimicrobial agent
The method comprises the following steps:
s1, preparing an antibacterial agent solution: mixing nisin and natamycin in a mass ratio of 1: 1 to obtain an antibacterial agent, and preparing the antibacterial agent and water into an antibacterial agent solution, wherein the content of the antibacterial agent is 10 wt%;
s2, preparing the porous aerogel:
s201, placing 30g of mixed aqueous solution containing 5 wt% of NaOH and 10 wt% of urea in a refrigerator, freezing to-10 ℃, adding 1g of graphene oxide into the mixed solution, mechanically stirring for 5min to obtain a graphene oxide solution, adding 1g of sodium carboxymethylcellulose into another 50g of mixed aqueous solution containing 5 wt% of NaOH and 10 wt% of urea, mechanically stirring for 2h to obtain a sodium carboxymethylcellulose solution, and mixing the graphene oxide solution and the sodium carboxymethylcellulose solution according to the volume ratio of 1: 3 to obtain a mixed solution;
s202, pouring 100g of liquid paraffin into a reactor, mechanically stirring for 20min, dripping 30g of mixed solution into the liquid paraffin, and mechanically stirring for 30min after dripping is finished; adding 12g of epichlorohydrin into liquid paraffin, reacting at room temperature for 3 hours, neutralizing with 12% hydrochloric acid after the reaction is finished, removing the upper layer of liquid paraffin, repeatedly washing the lower layer of standard product with distilled water and absolute ethyl alcohol to obtain hydrogel beads, and freeze-drying the hydrogel to obtain porous aerogel;
s3, preparing the porous aerogel containing the antibacterial agent: sequentially adding 5g of an antibacterial agent solution, 20g of porous aerogel, 2g of a coupling agent and 1.5g of a surfactant into a shearing disperser, heating to 50 ℃ at a speed of 3 ℃/min, preserving heat, carrying out first shearing dispersion, wherein the shearing force is 6000ips, the shearing time is 9min, then adding a stabilizer accounting for 5 wt% of the total mass of the materials, carrying out second shearing, the shearing force is 3000ips, the shearing time is 10min, obtaining a porous aerogel suspension dispersion liquid containing the antibacterial agent, and volatilizing the solvent to obtain the dried porous aerogel containing the antibacterial agent;
the coupling agent is a mixture of a silane coupling agent KH550 and a silane coupling agent KH570 in a mass ratio of 5: 3, the surfactant is a mixture of Tween-80 and span-80 in a mass ratio of 10: 3, and the stabilizer is a mixture of magnesium stearate and aluminum stearate in a mass ratio of 1: 4.
S4, preparing the antibacterial agent-containing slow-release porous aerogel PET color master batch: adding 10g of dried porous aerogel containing the antibacterial agent into a grinding machine, adding 5g of carbon black, 3g of potassium polyacrylate and 1g of dilauryl thiodipropionate, mixing and grinding to obtain a composite modifier containing the antibacterial agent; and adding 10g of composite modifier containing the antibacterial agent into 100g of PET slices, melting at the high temperature of 500 ℃, keeping the melting for 15min, and extruding and granulating to obtain the PET color master batch containing the antibacterial agent slow-release porous aerogel.
Example 3 controlled release porous aerogel PET color masterbatch containing antimicrobial agent
The method comprises the following steps:
s1, preparing an antibacterial agent solution: mixing nisin and natamycin in a mass ratio of 3: 2 to obtain an antibacterial agent, and preparing the antibacterial agent and water into an antibacterial agent solution, wherein the content of the antibacterial agent is 7 wt%;
s2, preparing the porous aerogel:
s201, 20g of mixed aqueous solution containing 4 wt% of NaOH and 7 wt% of urea is placed into a refrigerator to be frozen to-10 ℃, 1g of graphene oxide is added into the mixed solution, mechanical stirring is carried out for 5min to obtain graphene oxide solution, 1g of sodium carboxymethyl cellulose is added into another 40g of mixed aqueous solution containing 4 wt% of NaOH and 7 wt% of urea, mechanical stirring is carried out for 1.5h to obtain sodium carboxymethyl cellulose solution, and the graphene oxide solution and the sodium carboxymethyl cellulose solution are mixed according to the volume ratio of 1: 2 to obtain mixed solution;
s202, pouring 100g of liquid paraffin into a reactor, mechanically stirring for 15min, dropwise adding 20g of mixed solution into the liquid paraffin, and mechanically stirring for 20min after dropwise adding; adding 10g of epichlorohydrin into liquid paraffin, reacting at room temperature for 2 hours, neutralizing with 10% hydrochloric acid after the reaction is finished, removing the upper layer of liquid paraffin, repeatedly washing the lower layer of standard product with distilled water and absolute ethyl alcohol to obtain hydrogel beads, and freeze-drying the hydrogel to obtain the porous aerogel;
s3, preparing the porous aerogel containing the antibacterial agent: sequentially adding 3g of an antibacterial agent solution, 15g of porous aerogel, 1.5g of a coupling agent and 1g of a surfactant into a shearing disperser, heating to 50 ℃ at a speed of 3 ℃/min, preserving heat, carrying out first shearing dispersion with a shearing force of 5700ips for 7min, adding a stabilizer accounting for 2.5 wt% of the total mass of the materials, carrying out second shearing with a shearing force of 2700ips for 7min to obtain a porous aerogel suspension dispersion liquid containing the antibacterial agent, and volatilizing the solvent to obtain the dried porous aerogel containing the antibacterial agent;
the coupling agent is a mixture of a silane coupling agent KH550 and a silane coupling agent KH570 in a mass ratio of 5: 2, the surfactant is a mixture of Tween-80 and span-80 in a mass ratio of 10: 2, and the stabilizer is a mixture of magnesium stearate and aluminum stearate in a mass ratio of 1: 3.
S4, preparing the antibacterial agent-containing slow-release porous aerogel PET color master batch: adding 7g of dried porous aerogel containing the antibacterial agent into a grinding machine, adding 3g of titanium dioxide, 2g of ammonium polyacrylate and 0.7g of distearyl thiodipropionate, mixing and grinding to obtain a composite modifier containing the antibacterial agent; and adding 7g of composite modifier containing the antibacterial agent into 100g of PET slices, melting at the high temperature of 400 ℃, keeping the melting for 12min, and extruding and granulating to obtain the PET color master batch containing the antibacterial agent slow-release porous aerogel.
Comparative example 1
Compared with example 3, the antibacterial agent is nisin, and other conditions are not changed.
Comparative example 2
Compared with example 3, the antibacterial agent is natamycin, and other conditions are not changed.
Test example 1
The obtained porous aerogels prepared in examples 1 to 3 were tested and characterized by a laser particle size analyzer and an ultraviolet spectrophotometer, and the particle size distribution of the porous aerogel of this example were found, and the drug loading was as shown in table 1:
TABLE 1
| Particle size (nm) | Index of particle size distribution | Drug loading (%) | |
| Example 1 | 246.1±0.11 | 0.434 | 90 |
| Example 2 | 242.5±0.12 | 0.475 | 94 |
| Example 3 | 247.2±0.05 | 0.425 | 95 |
As can be seen from the above table, the porous aerogel prepared by the method of the present invention has the characteristics of uniform particle size distribution, high drug loading, etc.
Test example 2
The master batches prepared in examples 1-3 of the present invention and comparative examples 1-2 were subjected to performance tests, and the results are shown in Table 2.
The melt flow rate is detected according to the GB/T3682 method;
the density is detected according to a GB/T1033 method;
the tensile strength is detected according to the GB/T1040 method;
TABLE 2
| Group of | Melt flow Rate (g/10min) | Density (g/cm)3) | Tensile Strength (MPa) |
| Example 1 | 24.3 | 0.912 | 31.4 |
| Example 2 | 24.1 | 0.910 | 32.7 |
| Example 3 | 24.5 | 0.913 | 33.0 |
| Comparative example 1 | 22.1 | 0.892 | 27.3 |
| Comparative example 2 | 23.2 | 0.874 | 29.4 |
Test example 3 antibacterial property test
The master batches prepared in the examples 1-3 and the comparative examples 1-2 are tested for antibacterial performance, and the test method refers to GB/T21510-2008 detection, and adopts a film pasting method, namely escherichia coli ATYCC 25922 and staphylococcus aureus ATCC 6538. Refer to GB21551.2-2010 "Special requirements for antibacterial materials with antibacterial, degerming and purifying functions for household and similar appliances". Detection bacteria: candida albicans ATCC 10231(Candida albicans).
The results are shown in Table 3.
TABLE 3
As shown in the table, the master batch prepared by the invention has good antibacterial performance.
Compared with the example 3, the antibacterial agent in the comparative examples 1 and 2 is respectively nisin or natamycin, the antibacterial property is obviously reduced, and the mechanical property is also reduced, the nisin is a polypeptide substance produced by streptococcus lactis, can inhibit the growth and the reproduction of most gram-positive bacteria, has strong inhibiting effect on spores of bacillus, and particularly has special effect on the gram-positive bacteria producing the spores, the antibacterial mechanism is that the nisin is combined with ergosterol and other sterol groups of fungi to inhibit the biosynthesis of the ergosterol, so that the cell membrane is distorted, and finally the cell is leaked to cause the cell death; after the nisin and the natamycin are compounded, the composite antibacterial agent can kill or inhibit the appreciation of most bacteria, fungi and the like, so that the high-efficiency antibacterial effect is achieved, and the composite antibacterial agent has good anti-aging performance.
Compared with the prior art, the antibacterial agent-containing slow-release porous aerogel is prepared by skillfully utilizing the porous aerogel, so that the master batch has good antibacterial and bacteriostatic properties, aromaticity, anti-sensitivity or anti-inflammatory functions and the like, and the porous aerogel containing the antibacterial agent is uniformly dispersed in the slices, so that the prepared master batch is further prepared into fibers and has good functions;
the nisin is a polypeptide substance produced by streptococcus lactis, can inhibit the growth and reproduction of most gram-positive bacteria, has strong inhibiting effect on spores of bacillus, has special effect on the gram-positive bacteria producing the spores, has an antibacterial mechanism by interfering the normal function of cell membranes to cause the permeation, nutrient loss and membrane potential reduction of the cell membranes so as to cause the death of pathogenic bacteria and putrefying bacteria cells, and has an action mechanism of combining with ergosterol and other sterol groups of fungi to inhibit the biosynthesis of the ergosterol so as to distort the cell membranes and finally cause leakage and cause the cell death; after the nisin and the natamycin are compounded, most of bacteria, fungi and the like can be killed or inhibited from increasing in value, so that the efficient antibacterial effect is achieved, and the composite antibacterial agent has good anti-aging performance.
The prepared antibacterial agent-containing slow-release porous aerogel PET color master batch is mainly used for coloring fibers before spinning, can not only color PET fibers, but also endow colored PET fibers with excellent antibacterial property and excellent mechanical property.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch is characterized by comprising the following steps of:
s1, preparing an antibacterial agent solution;
s2, preparing porous aerogel;
s3, preparing porous aerogel containing an antibacterial agent;
s4, preparing the PET color master batch containing the antibacterial agent and the slow-release porous aerogel.
2. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch as claimed in claim 1, wherein the antibacterial agent is a mixture of nisin and natamycin in a mass ratio of 3 (1-3), the antibacterial agent content in the antibacterial agent solution is 5-10 wt%, and the balance is water.
3. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch according to claim 1, wherein the step S2 comprises the following steps:
s201, cooling a mixed aqueous solution containing NaOH and urea to below 5 ℃, adding graphene oxide into the mixed solution, mechanically stirring to obtain a graphene oxide solution, adding sodium carboxymethylcellulose into another mixed aqueous solution containing NaOH and urea, mechanically stirring to obtain a sodium carboxymethylcellulose solution, and mixing the graphene oxide solution and the sodium carboxymethylcellulose solution according to a volume ratio of 1: (1-3) mixing to obtain a mixed solution;
s202, pouring liquid paraffin into a reactor, mechanically stirring, dropwise adding the mixed solution into the liquid paraffin, and mechanically stirring after dropwise adding; and then adding epoxy chloropropane into the liquid paraffin, reacting at room temperature, neutralizing with hydrochloric acid after the reaction is finished, removing the upper layer of the liquid paraffin, repeatedly washing the lower layer of the standard product with distilled water and absolute ethyl alcohol to obtain hydrogel beads, and freeze-drying the hydrogel to obtain the porous aerogel.
4. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch according to claim 3, wherein in the mixed aqueous solution containing NaOH and 5-10 wt% of urea, the mass fraction of NaOH is 3-5 wt%, and the mass fraction of urea is 5-10 wt%; the volume-mass ratio of the mixed aqueous solution containing NaOH and urea to the graphene oxide is (10-30): 1; the volume-mass ratio of the mixed aqueous solution containing NaOH and urea to the sodium carboxymethyl cellulose is (30-50): 1; the mass ratio of the liquid paraffin to the mixed solution to the epichlorohydrin is 100: (10-30): (5-12).
5. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch according to claim 1, wherein the step S3 comprises the following steps: sequentially adding the antibacterial agent solution, the porous aerogel, the coupling agent and the surfactant into a shearing disperser, heating to 50 ℃, preserving heat, performing first shearing dispersion, then adding a stabilizer accounting for 0.1-5 wt% of the total mass of the materials, performing second shearing to obtain a porous aerogel suspension dispersion liquid containing the antibacterial agent, and volatilizing the solvent to obtain the dry porous aerogel containing the antibacterial agent.
6. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch according to claim 5, wherein the shearing force of the first shearing dispersion is 5250-6000ips, the shearing time is 4-9min, the temperature rising rate is 3 ℃/min, the shearing force of the second shearing dispersion is 2500-3000ips, and the shearing time is 5-10 min; the coupling agent is a mixture of a silane coupling agent KH550 and a silane coupling agent KH570, the mass ratio is 5 (1-3), the surfactant is a mixture of Tween-80 and span-80, the mass ratio is 10 (1-3), and the stabilizer is a mixture of magnesium stearate and aluminum stearate, and the mass ratio is 1 (2-4).
7. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch according to claim 1, wherein the step S4 comprises the following steps: adding the dried porous aerogel containing the antibacterial agent into a grinding machine, adding the pigment, the dispersing agent and the antioxidant, mixing and grinding to obtain a composite modifier containing the antibacterial agent; and adding the composite modifier containing the antibacterial agent into the PET slices, melting at high temperature, keeping the melting for 10-15min, and extruding and granulating to obtain the PET color master batch containing the antibacterial agent slow-release porous aerogel.
8. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch according to claim 7, wherein the high-temperature melting temperature is 300-500 ℃, and the dispersing agent is selected from one of sodium polyacrylate, potassium polyacrylate and ammonium polyacrylate; the antioxidant is selected from one of 2, 4-di- (n-octylthiomethylene) -6-methylphenol, 2, 4-di (dodecylthiomethyl) -6-methylphenol, dilauryl thiodipropionate or distearyl thiodipropionate; the pigment is one or a mixture of phthalocyanine pigment, titanium dioxide, carbon black, ultramarine pigment and titanium yellow pigment.
9. The preparation method of the antibacterial agent-containing slow-release porous aerogel PET color master batch according to claim 1, characterized by comprising the following steps:
s1, preparing an antibacterial agent solution: mixing nisin and natamycin in a mass ratio of 3 (1-3) to obtain an antibacterial agent, and preparing the antibacterial agent and water into an antibacterial agent solution, wherein the content of the antibacterial agent is 5-10 wt%;
s2, preparing the porous aerogel:
s201, putting 10-30 parts by weight of mixed aqueous solution containing 3-5 wt% of NaOH and 5-10 wt% of urea into a refrigerator, freezing to-10 ℃, adding 1 part by weight of graphene oxide into the mixed solution, mechanically stirring for 5min to obtain graphene oxide solution, adding 1 part by weight of sodium carboxymethylcellulose into another 30-50 parts by weight of mixed aqueous solution containing 3-5 wt% of NaOH and 5-10 wt% of urea, mechanically stirring for 1-2h to obtain sodium carboxymethylcellulose solution, mixing the graphene oxide solution and the sodium carboxymethylcellulose solution according to a volume ratio of 1: (1-3) mixing to obtain a mixed solution;
s202, pouring 100 parts by weight of liquid paraffin into a reactor, mechanically stirring for 10-20min, dripping 10-30 parts by weight of mixed solution into the liquid paraffin, and mechanically stirring for 10-30min after dripping is finished; adding 5-12 parts by weight of epichlorohydrin into liquid paraffin, reacting at room temperature for 1-3h, neutralizing with 5-12% hydrochloric acid after the reaction is finished, removing the upper layer of liquid paraffin, repeatedly washing the lower layer of standard product with distilled water and absolute ethyl alcohol to obtain hydrogel beads, and freeze-drying the hydrogel to obtain porous aerogel;
s3, preparing the porous aerogel containing the antibacterial agent: sequentially adding 2-5 parts by weight of an antibacterial agent solution, 10-20 parts by weight of porous aerogel, 1-2 parts by weight of a coupling agent and 0.5-1.5 parts by weight of a surfactant into a shearing disperser, heating to 50 ℃ at a speed of 3 ℃/min, preserving heat, performing primary shearing dispersion, wherein the shearing force is 5250-6000ips, the shearing time is 4-9min, then adding a stabilizer accounting for 0.1-5 wt% of the total mass of the materials, performing secondary shearing, wherein the shearing force is 2500-3000ips, and the shearing time is 5-10min to obtain a porous aerogel suspension dispersion liquid containing the antibacterial agent, and volatilizing the solvent to obtain the dry porous aerogel containing the antibacterial agent;
s4, preparing the antibacterial agent-containing slow-release porous aerogel PET color master batch: adding 5-10 parts by weight of dried porous aerogel containing the antibacterial agent into a grinding machine, adding 2-5 parts by weight of pigment, 1-3 parts by weight of dispersing agent and 0.5-1 part by weight of antioxidant, mixing and grinding to obtain a composite modifier containing the antibacterial agent; adding 5-10 parts by weight of composite modifier containing the antibacterial agent into 100 parts by weight of PET slices, melting at the high temperature of 300-500 ℃, keeping the melting for 10-15min, and extruding and granulating to obtain the PET color master batch containing the antibacterial agent slow-release porous aerogel.
10. The antibacterial agent-containing slow-release porous aerogel PET color master batch prepared by the preparation method according to any one of claims 1 to 9.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112852207A (en) * | 2021-02-23 | 2021-05-28 | 广东施彩新材料科技有限公司 | Polylactic acid PDLLA slow-release antibacterial agent and preparation method and application thereof |
| CN114134591A (en) * | 2021-12-13 | 2022-03-04 | 中国科学技术大学先进技术研究院 | Preparation method of polyester composite fiber |
| CN114182531A (en) * | 2021-02-20 | 2022-03-15 | 青岛尼希米生物科技有限公司 | Protein modified antibacterial flame-retardant cotton fiber and preparation method and application thereof |
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2020
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114182531A (en) * | 2021-02-20 | 2022-03-15 | 青岛尼希米生物科技有限公司 | Protein modified antibacterial flame-retardant cotton fiber and preparation method and application thereof |
| CN114182531B (en) * | 2021-02-20 | 2024-03-19 | 云起(青岛)材料科技有限公司 | Protein modified antibacterial flame-retardant cotton fiber, and preparation method and application thereof |
| CN112852207A (en) * | 2021-02-23 | 2021-05-28 | 广东施彩新材料科技有限公司 | Polylactic acid PDLLA slow-release antibacterial agent and preparation method and application thereof |
| CN114134591A (en) * | 2021-12-13 | 2022-03-04 | 中国科学技术大学先进技术研究院 | Preparation method of polyester composite fiber |
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Application publication date: 20210112 |