CN118185079A - Black antibacterial nylon 6 master batch for enhancing blackness and blue phase and preparation method thereof - Google Patents

Black antibacterial nylon 6 master batch for enhancing blackness and blue phase and preparation method thereof Download PDF

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Publication number
CN118185079A
CN118185079A CN202410409483.4A CN202410409483A CN118185079A CN 118185079 A CN118185079 A CN 118185079A CN 202410409483 A CN202410409483 A CN 202410409483A CN 118185079 A CN118185079 A CN 118185079A
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temperature
master batch
nylon
black
temperature zone
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CN202410409483.4A
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张子明
陈梦婷
邓梦颖
丁洁
林志鹏
彭玉林
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Fujian Yongrong Jinjiang Co Ltd
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Fujian Yongrong Jinjiang Co Ltd
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Abstract

The invention discloses a black antibacterial nylon 6 master batch for enhancing blackness and blue phase and a preparation method thereof, belonging to the technical field of chemical fibers; in the preparation process of the nylon 6 master batch, the colored carbon black powder and the nano zinc oxide are added, and uniformly dispersed black master batch is obtained by premixing and melt extrusion of the zinc oxide and the carbon black in the preparation process; the black antibacterial nylon 6 master batch prepared by the invention activates carrier resin, enhances the surface energy of polyamide, improves the compatibility of carbon black and polyamide, enhances the dispersibility of the black antibacterial nylon 6 master batch in polyamide, reduces the aggregation of colored carbon black powder, endows the black master batch with good blackness and glossiness, and has a bluish or blue phase, thereby improving the coloring effect of the black master batch, and free Zn 2+ can still keep certain activity after the zinc oxide is mixed with carbon black powder, so that the prepared black antibacterial nylon 6 master batch is easy to interact with electronegative bacteria to realize antibacterial effect.

Description

Black antibacterial nylon 6 master batch for enhancing blackness and blue phase and preparation method thereof
Technical Field
The invention belongs to the technical field of chemical fibers, and particularly relates to a black antibacterial nylon 6 master batch for enhancing blackness and blue phase and a preparation method thereof.
Background
Nylon 6 fiber is used as the second largest chemical fiber worldwide, and has the main characteristics of high breaking strength, excellent wear resistance, low weight, good elasticity and the like. In recent years, the awareness of people on health and environmental protection is increasingly enhanced, the technology of coloring nylon 6 fibers by using stock solution is also greatly developed, various colors are endowed to the fibers in the melt spinning process by adding color master batches, the printing and dyeing links in the production process of downstream enterprises are omitted, and the nylon 6 fiber has outstanding environmental protection characteristics. The black nylon 6 filament accounts for about 30% of the stock solution coloring nylon 6 in the current market, and is mainly applied to close-fitting articles such as swimwear, silk stockings and the like, thereby having wide market prospect.
In the preparation process of the black nylon 6 master batch, the carbon black has small particle size and high specific surface area, so that the unmodified carbon black and the master batch polyamide have poor compatibility, and agglomeration phenomenon is easy to occur, so that the uniform dispersion effect of the carbon black in the carrier resin is reduced, and the blackness and the coloring degree effect of the final spinning coloring are affected. On the other hand, in addition to the requirements of textiles for diversification, color beauty, environmental protection, etc., the functional requirements of garments are increasing, and the antibacterial function is attracting more and more attention from the industry. At present, silver antibacterial agents are commonly adopted in antibacterial fibers, but the safety of products is always in full of disputes because nano silver is easy to accumulate in a human body after being absorbed by the human body. Therefore, the preparation method for effectively enhancing the blackness and blue phase of the black nylon 6 master batch, overcoming the defects of silver antibacterial agents and endowing the black nylon 6 master batch with antibacterial efficacy is researched, and the preparation method has wide practical value and wide application prospect.
In the invention, the high-concentration antibacterial black nylon 6 master batch is prepared, the addition amount of the master batch is reduced, and the spinnability of the fiber is effectively improved, wherein the adopted mode is to replace part of silver by TiO 2 with lower cost, so that the potential hazard that nano silver is absorbed by a human body can not be completely solved, and the problem that the black degree and the coloring degree effect of spinning are finally influenced due to poor compatibility of carbon black and polyamide is not solved; the invention discloses a method for preparing antistatic black master batch by using graphene coated carbon black with publication number CN111363346A and a product thereof, wherein the method comprises the following steps: (1) Modifying the carbon black by using a dispersing agent to obtain modified carbon black; uniformly mixing graphene oxide and modified carbon black in a solvent, and performing aftertreatment to obtain graphene oxide coated modified carbon black; the dispersant is sodium dodecyl benzene sulfonate, APS, DL602. One or more of sodium dodecyl sulfate; (2) Reducing the obtained graphene oxide coated modified carbon black by using a reducing agent, and performing aftertreatment to obtain graphene coated carbon black; (3) The obtained graphene coated carbon black and the matrix master batch are subjected to melt mixing and granulating to obtain antistatic black master batch, but the black master batch mainly solves the technical problem how to greatly improve the dispersibility, the color uniformity and the antistatic property of the carbon black in the matrix material, and does not relate to the improvement of the antibacterial performance.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a black antibacterial nylon 6 master batch for enhancing blackness and blue phase and a preparation method thereof, wherein colored carbon black powder and nano zinc oxide are added in the process of preparing the nylon 6 master batch, and uniformly dispersed black master batch is obtained by premixing and melt extrusion of zinc oxide and carbon black in the preparation process.
The technical scheme of the invention is as follows:
The invention aims at providing a preparation method of black antibacterial nylon 6 master batch for enhancing blackness and blue phase, which comprises the steps of adding spinning grade nylon 6 chips into a main feeding position of a double-screw extruder, introducing carbon black powder, auxiliary agent powder and zinc oxide which are premixed in proper proportion into a side feeding position, melting and plasticizing the main feeding and the side feeding by controlling the temperature of each section of the double-screw extruder, and obtaining the composite black antibacterial nylon 6 master batch through bracing, water tank cooling, granulating vibration screening and vacuum constant temperature drying.
Further, the spinning grade nylon 6 slice accounts for 56% -58% of the total mass of the spinning grade nylon 6 slice, zinc oxide, auxiliary agent powder and carbon black powder.
Further, the zinc oxide accounts for 9-11% of the total mass of the spinning grade nylon 6 chips, zinc oxide, the auxiliary agent powder and the carbon black powder.
Further, the carbon black powder accounts for 30-32% of the total mass of the spinning grade nylon 6 chips, zinc oxide, the auxiliary agent powder and the carbon black powder.
Further, the auxiliary agent powder is dispersant JHX-100/HD65/330.
Further, the auxiliary agent powder accounts for 1-3% of the total mass of the spinning grade nylon 6 chips, zinc oxide, the auxiliary agent powder and the carbon black powder.
Further, the temperatures of the temperature zones of each section are respectively as follows: the temperature of the first-stage temperature zone is 225 ℃; the temperature of the second section temperature zone is 225 ℃, the temperature of the third section temperature zone is 230 ℃, the temperature of the fourth section temperature zone is 230 ℃, the temperature of the fifth section temperature zone is 230 ℃, the temperature of the sixth section temperature zone is 225-230 ℃, the temperature of the seventh section temperature zone is 210-215 ℃, the temperature of the eighth section temperature zone is 200-205 ℃, the temperature of the ninth section temperature zone is 195-205 ℃, the temperature of the tenth section temperature zone is 185-195 ℃, the temperature of the eleventh section temperature zone is 180-190 ℃ and the temperature of the head temperature zone is 230-240 ℃.
Further, the melting temperature is 225 ℃ to 230 ℃.
Further, the granulating vibration screening is to screen out a finished product with proper particle size by a vibrating screen with a screen mesh with 1-3mm aperture after granulating by a granulator with the rotating speed of 890 rpm.
The second purpose of the invention is to provide a black antibacterial nylon 6 master batch for enhancing blackness and blue phase.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the invention, zinc oxide is introduced in a proper proportion in the process of preparing the nylon 6 master batch, so that the carrier resin is effectively activated, the surface energy of polyamide is enhanced, the compatibility of carbon black and polyamide is improved, the agglomeration phenomenon caused by poor compatibility of unmodified carbon black and master batch polyamide is effectively reduced, good blackness and glossiness are given to the black master batch, the hue is represented as bluish phase or blue phase, the coloring effect of the carbon black master batch is improved, and finally the black master batch with enhanced blackness and blue phase and uniform dispersion is prepared.
2. In the preparation method, zinc oxide can still keep certain activity of free Zn 2+ after being mixed with carbon black powder, so that the black nylon 6 master batch prepared by the method has good antibacterial performance when the blackness and the blue are enhanced, can interact with electronegative bacteria to destroy the cell activity of the electronegative bacteria so as to generate an antibacterial effect, and has excellent performance in inhibiting the antibacterial rate of candida albicans, escherichia coli and staphylococcus aureus.
Reference numerals
FIG. 1 is a graph showing the color measurement results of corresponding sock belts of fibers produced by the black antibacterial nylon 6 master batches prepared in examples 1 to 4 of the present invention.
Detailed Description
The invention is further described in connection with the accompanying drawings and the preferred embodiments, which are given solely for the purpose of illustration and are not intended to limit the scope of the invention.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified;
The quantitative tests in the following examples were all set up three repeated experiments, and the results were averaged;
The experimental methods in the following examples are all conventional methods unless otherwise specified;
Example 1
The embodiment provides a preparation method of black antibacterial nylon 6 master batch for enhancing blackness and blue phase, which specifically comprises the following steps:
s1, adding spinning nylon 6 slices into a main feeding position of a double-screw extruder, wherein the proportion is 63%, and adding 30% of carbon black powder, 3% of dispersant JHX-100/HD65/330 and 4% of zinc oxide powder into a side feeding position;
S2, melting and plasticizing raw materials by controlling the temperature of each section of temperature zone of the double-screw extruder, wherein the temperature of each section of temperature zone of the extruder is respectively as follows: the temperature of the first-stage temperature zone is 225 ℃; the temperature of the second section temperature zone is 225 ℃, the temperature of the third section temperature zone is 230 ℃, the temperature of the fourth section temperature zone is 230 ℃, the temperature of the fifth section temperature zone is 230 ℃, the temperature of the sixth section temperature zone is 225 ℃, the temperature of the seventh section temperature zone is 215 ℃, the temperature of the eighth section temperature zone is 200 ℃, the temperature of the ninth section temperature zone is 205 ℃, the temperature of the tenth section temperature zone is 185 ℃, the temperature of the eleventh section temperature zone is 190 ℃, and the temperature of the machine head temperature zone is 230 ℃;
S3, cooling by a brace, cooling by a water tank, granulating, vibrating, screening, and drying at a constant temperature in vacuum to obtain the composite black antibacterial nylon 6 master batch.
Example 2
The embodiment provides a preparation method of black antibacterial nylon 6 master batch for enhancing blackness and blue phase, which specifically comprises the following steps:
S1, adding a spinning grade nylon 6 slice into a main feeding position of a double-screw extruder, wherein the proportion is 61%, and adding 31% of carbon black powder, 2% of dispersant JHX-100/HD65/330 and 6% of zinc oxide powder into a side feeding position;
s2, melting and plasticizing raw materials by controlling the temperature of each section of temperature zone of the double-screw extruder, wherein the temperature of the first section of temperature zone is 225 ℃; the temperature of the second section temperature zone is 225 ℃, the temperature of the third section temperature zone is 230 ℃, the temperature of the fourth section temperature zone is 230 ℃, the temperature of the fifth section temperature zone is 230 ℃, the temperature of the sixth section temperature zone is 230 ℃, the temperature of the seventh section temperature zone is 210 ℃, the temperature of the eighth section temperature zone is 205 ℃, the temperature of the ninth section temperature zone is 195 ℃, the temperature of the tenth section temperature zone is 195 ℃, the temperature of the eleventh section temperature zone is 180 ℃ and the temperature of the machine head temperature zone is 240 ℃;
S3, cooling by a brace, cooling by a water tank, granulating, vibrating, screening, and drying at a constant temperature in vacuum to obtain the composite black antibacterial nylon 6 master batch.
Example 3
The embodiment provides a preparation method of black antibacterial nylon 6 master batch for enhancing blackness and blue phase, which specifically comprises the following steps:
S1, adding spinning nylon 6 slices into a main feeding position of a double-screw extruder, wherein the proportion is 59%, and adding 32% of carbon black powder, 1% of dispersant JHX-100/HD65/330 and 8% of zinc oxide powder into a side feeding position;
S2, melting and plasticizing raw materials by controlling the temperature of each section of temperature zone of the double-screw extruder, wherein the temperature of the first section of temperature zone is 225 ℃; the temperature of the second section temperature zone is 225 ℃, the temperature of the third section temperature zone is 230 ℃, the temperature of the fourth section temperature zone is 230 ℃, the temperature of the fifth section temperature zone is 230 ℃, the temperature of the sixth section temperature zone is 230 ℃, the temperature of the seventh section temperature zone is 215 ℃, the temperature of the eighth section temperature zone is 200 ℃, the temperature of the ninth section temperature zone is 195 ℃, the temperature of the tenth section temperature zone is 190 ℃, the temperature of the eleventh section temperature zone is 180 ℃, and the temperature of the machine head temperature zone is 235 ℃;
S3, cooling by a brace, cooling by a water tank, granulating, vibrating, screening, and drying at a constant temperature in vacuum to obtain the composite black antibacterial nylon 6 master batch.
Example 4
The embodiment provides a preparation method of black antibacterial nylon 6 master batch for enhancing blackness and blue phase, which specifically comprises the following steps:
s1, adding spinning nylon 6 slices into a main feeding position of a double-screw extruder, wherein the proportion is 57%, and adding 30% of carbon black powder, 3% of dispersant JHX-100/HD65/330 and 10% of zinc oxide powder into a side feeding position;
S2, melting and plasticizing raw materials by controlling the temperature of each section of temperature zone of the double-screw extruder, wherein the temperature of the first section of temperature zone is 225 ℃; the temperature of the second section temperature zone is 225 ℃, the temperature of the third section temperature zone is 230 ℃, the temperature of the fourth section temperature zone is 230 ℃, the temperature of the fifth section temperature zone is 230 ℃, the temperature of the sixth section temperature zone is 225 ℃, the temperature of the seventh section temperature zone is 210 ℃, the temperature of the eighth section temperature zone is 205 ℃, the temperature of the ninth section temperature zone is 200 ℃, the temperature of the tenth section temperature zone is 195 ℃, the temperature of the eleventh section temperature zone is 185 ℃, and the temperature of the machine head temperature zone is 230 ℃;
S3, cooling by a brace, cooling by a water tank, granulating, vibrating, screening, and drying at a constant temperature in vacuum to obtain the composite black antibacterial nylon 6 master batch.
Comparative example 1
The comparative example provides a preparation method of nylon 6 master batch, which comprises the following steps:
S1, adding spinning grade nylon 6 slices into a main feeding position of a double-screw extruder, wherein the proportion is 67%, and adding 30% of carbon black powder and 3% of dispersing agent JHX-100/HD65/330 into a side feeding position;
s2, melting and plasticizing raw materials by controlling the temperature of each section of temperature zone of the double-screw extruder, wherein the temperature of the first section of temperature zone is 225 ℃; the temperature of the second section temperature zone is 225 ℃, the temperature of the third section temperature zone is 230 ℃, the temperature of the fourth section temperature zone is 230 ℃, the temperature of the fifth section temperature zone is 230 ℃, the temperature of the sixth section temperature zone is 225 ℃, the temperature of the seventh section temperature zone is 215 ℃, the temperature of the eighth section temperature zone is 200 ℃, the temperature of the ninth section temperature zone is 205 ℃, the temperature of the tenth section temperature zone is 185 ℃, the temperature of the eleventh section temperature zone is 190 ℃, and the temperature of the machine head temperature zone is 230 ℃;
S3, cooling by a brace, cooling by a water tank, granulating, vibrating, screening, and drying at a constant temperature in vacuum to obtain the composite black antibacterial nylon 6 master batch.
Performance testing
1. The indexes such as breaking strength, breaking elongation and antibacterial property of the fibers produced by the nylon 6 master batches prepared in examples 1 to 4 and comparative example 1 were measured, and blackness comparison was performed, and the results are shown in table 1.
TABLE 1 color measurement results for corresponding hosiery belts of the fibers produced in examples 1-4 and comparative example 1
As can be seen from the hue in comparison of the measured data of the hose Lab, the hues of examples 1-3 were bluish for comparative example 1, whereas the hue of example 4 with the highest ZnO yarn formation was reddish for comparative example 1. From the aspect of blackness, under the condition that the carbon black content in the finished yarn is the same, the blackness of the examples 1-4 added with ZnO is deeper than that of the comparative example 1 without ZnO, and the blackness of the sock belts is deeper along with the continuous increase of the zinc oxide addition amount, but the deepening degree is gradually reduced, so that the zinc oxide addition can be proved to effectively deepen the spinning blackness of nylon 6.
2. The fibers produced by the nylon 6 master batches prepared in examples 1 to 4 and comparative example 1 were tested for antimicrobial properties by the "evaluation of textile-antimicrobial properties-vibration method (GB/T20944.3-2008)", and the results are shown in Table 2.
TABLE 2 antibacterial Property test results of the fibers produced in examples 1 to 4 and comparative example 1
The results show that the antibacterial rate of the candida albicans of the fiber produced in the comparative example 1 only reaches the national standard basic value (70%), and the more excellent the antibacterial performance of the candida albicans of the fiber produced in the experimental examples 1-4 is along with the increase of the ZnO content in the finished yarn, the more excellent the antibacterial effect of the candida albicans is, and the antibacterial effect of the candida albicans is effectively improved; in addition, the coliform bacteria inhibition rate of the produced fibers in experimental examples 1-4 is improved by 6% compared with comparative example 1, and experimental examples 1-4 are basically equivalent to comparative example 1 in terms of staphylococcus aureus bacteria inhibition rate.
Comprehensively comparing blackness, hue and antibacterial performance: in terms of blackness, examples 3, 4 were comparable in blackness; in terms of antibiosis, the antibacterial rates of the candida albicans, the escherichia coli and the staphylococcus aureus in the examples 3 and 4 are basically consistent; in terms of hue, the hue of example 3 is significantly more blue than that of example 4. Thus, the method of preparing black antimicrobial nylon 6 fiber with enhanced jetness and blue phase in the present invention may be preferred as example 3.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related arts are included in the scope of the present invention.

Claims (10)

1. The preparation method is characterized in that spinning grade nylon 6 chips are added into a main feeding position of a double-screw extruder, carbon black powder, auxiliary agent powder and zinc oxide which are premixed in proper proportion are introduced into a side feeding position, the temperature of each section of the double-screw extruder is controlled, the main feeding and the side feeding are melted and plasticized, and the composite black antibacterial nylon 6 master batch is prepared through bracing, water tank cooling, granulating, vibration screening and vacuum constant temperature drying.
2. The method for preparing black antibacterial nylon 6 master batch for enhancing blackness and blue phase according to claim 1, wherein the ratio of the spinning grade nylon 6 chips is 56% -58% based on the total mass of the spinning grade nylon 6 chips, zinc oxide, auxiliary agent powder and carbon black powder.
3. The method for preparing black antibacterial nylon 6 master batch for enhancing blackness and blue phase according to claim 1, wherein the zinc oxide accounts for 9% -11% of the total mass of the spinning nylon 6 chips, the zinc oxide, the auxiliary agent powder and the carbon black powder.
4. The method for preparing black antibacterial nylon 6 master batch for enhancing blackness and blue phase according to claim 1, wherein the carbon black powder accounts for 30-32% based on the total mass of spinning grade nylon 6 chips, zinc oxide, auxiliary agent powder and carbon black powder.
5. The method for preparing black antibacterial nylon 6 master batch for enhancing blackness and blue phase according to claim 1, wherein the auxiliary agent powder is a dispersing agent JHX-100/HD65/330.
6. The method for preparing black antibacterial nylon 6 master batch for enhancing blackness and blue phase according to claim 1, wherein the auxiliary agent powder accounts for 1-3% of the total mass of the spinning grade nylon 6 chips, zinc oxide, the auxiliary agent powder and the carbon black powder.
7. The method for preparing the black antibacterial nylon 6 master batch for enhancing blackness and blue phase according to claim 1, wherein the temperatures of the temperature areas of each section are respectively as follows: the temperature of the first-stage temperature zone is 225 ℃; the temperature of the second section temperature zone is 225 ℃, the temperature of the third section temperature zone is 230 ℃, the temperature of the fourth section temperature zone is 230 ℃, the temperature of the fifth section temperature zone is 230 ℃, the temperature of the sixth section temperature zone is 225-230 ℃, the temperature of the seventh section temperature zone is 210-215 ℃, the temperature of the eighth section temperature zone is 200-205 ℃, the temperature of the ninth section temperature zone is 195-205 ℃, the temperature of the tenth section temperature zone is 185-195 ℃, the temperature of the eleventh section temperature zone is 180-190 ℃ and the temperature of the head temperature zone is 230-240 ℃.
8. The method for preparing black antimicrobial nylon 6 master batch for enhancing blackness and blue phase according to claim 1, wherein the melting temperature is 225-230 ℃.
9. The method for preparing black antibacterial nylon 6 master batch for enhancing blackness and blue phase according to claim 1, wherein the granulating vibration screening is to screen out a finished product with proper particle size by a vibrating screen with a screen with 1-3mm aperture after granulating by a granulator with the rotating speed of 890 rpm.
10. A black antimicrobial nylon 6 masterbatch having enhanced jetness and blue phase produced by the process of any one of claims 1-9.
CN202410409483.4A 2024-04-07 2024-04-07 Black antibacterial nylon 6 master batch for enhancing blackness and blue phase and preparation method thereof Pending CN118185079A (en)

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CN202410409483.4A CN118185079A (en) 2024-04-07 2024-04-07 Black antibacterial nylon 6 master batch for enhancing blackness and blue phase and preparation method thereof

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Application Number Priority Date Filing Date Title
CN202410409483.4A CN118185079A (en) 2024-04-07 2024-04-07 Black antibacterial nylon 6 master batch for enhancing blackness and blue phase and preparation method thereof

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CN118185079A true CN118185079A (en) 2024-06-14

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